Formulations for application to the skin, corrective body film or body modeling film formed from the

专利摘要:
skin compositions and methods of use thereof. Corrective cosmetic body formulations and methods of use thereof are provided.
公开号:BR112013004914B1
申请号:R112013004914-6
申请日:2011-08-31
公开日:2018-07-31
发明作者:Yu Betty；Lomakin Joseph；Kang Soo-Young；W. Adams Benjamin
申请人:Living Proof, Inc.；
IPC主号:

专利说明:

(54) Title: FORMULATIONS FOR SKIN APPLICATION, CORPORATE CORRECTIVE FILM OR BODY MODELING FILM FORMED FROM THE SAME AND METHODS OF USE OF THE SAME (51) Int.CI .: A61K 8/89; A61K 31/74; A61K 31/795; A61Q 19/00; A61P 17/00 (30) Unionist Priority: 06/03/2011 US 61 / 493,020, 04/07/2011 US 61 / 472,995, 11/11/2010 US 61 / 412,531, 01/13/2011 US 61 / 432,458, 6/13/2011 US 61 / 496,420, 5/16/2011 US 61 / 486,643, 6/20/2011 US 61 / 499,002, 5/23/2011 US 61 / 489,119, 6/23/2011 US 61 / 500,455, 2/24/2011 US 61 / 446,377, 8/31/2010 US 61 / 378,504 (73) Owner (s): LIVING PROOF, INC.
(72) Inventor (s): BETTY YU; JOSEPH LOMAKIN; SOO-YOUNG KANG; BENJAMIN W. ADAMS (85) National Phase Start Date: 28/02/2013
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Descriptive Report of the Invention Patent for FORMULATIONS FOR APPLICATION TO THE SKIN, CORPORATE CORRECTIVE FILM OR BODY MODELING FILM FORMED FROM THE SAME AND METHODS OF USE OF THE SAME. Related Orders [001] This application claims the benefit of US Provisional Patent Application 61/500455, filed on June 23, 2011; Provisional Patent Application US 61 / 499,002, filed on June 20, 2011; Provisional Patent Application US 61 / 496,420, filed on June 13, 2011; Provisional Patent Application US 61 / 493,020, filed on June 3, 2011; Provisional Patent Application US 61 / 489,119, filed on May 23, 2011; Provisional Patent Application US 61 / 486,643, filed on May 16, 2011; Provisional Patent Application US 61 / 472,995, filed on April 7, 2011; Provisional Patent Application US 61 / 446,337, filed on February 24, 2011; Provisional Patent Application US 61 / 432,458, filed on January 13, 2011; Provisional Patent Application US 61 / 412,531, filed on November 11, 2010 and Provisional Patent Application US 61 / 378,504, filed on August 31, 2010. The full content of the previous applications is incorporated herein by reference.
Background of the Invention [002] Current methods for reducing the appearance of skin imperfections, for example, wrinkles, fine lines, age spots, enlarged pores or scars, include invasive and non-invasive methods and formulations. Invasive techniques, such as surgery, fillers (for example, Restylane, Juvederm), laser re-epithelialization or Botox®, can provide longer-lasting effects and can treat prominent imperfections. However, many consumers cannot afford or want to undergo such drastic cosmetic treatments.
[003] Examples of non-invasive methods include imperfections
2/160 hidden by applying a make-up type foundation to the skin or by applying a cosmetic formulation that comprises an ingredient that can reduce the appearance of imperfections over time (for example, an anti-wrinkle cream). Unfortunately, applying makeup is not durable and cannot reduce the appearance of pronounced skin imperfections, such as deep wrinkles or scars, while cosmetic formulations containing ingredients that can reduce the appearance of an imperfection take time to produce an effect and may not yet reduce the appearance of a pronounced imperfection. In particular, many of today's cosmetic formulations do not have the mechanical properties necessary to reduce the appearance of pronounced imperfections.
[004] High molecular weight polymers, including proteins and polysaccharides, have been used in attempts to develop anti-aging formulations for cosmetic skin care (Jachowicz et al., Skin Res. And Tech., 2008, 14: 312-319). Although these polymers alter the physical properties (for example, elasticity and stiffness) of the skin upon application to the skin, they do not provide the durability to allow repeated natural facial movement for prolonged use. The commercially available polymer materials used in skin products today do not necessarily provide elasticity, environmental resistance and skin adhesion for long-lasting product performance, nor do they provide the aesthetic look and feel required by the consumer of cosmetic products.
Summary of the Invention [005] The present invention provides durable, natural-looking, non-invasive compositions that exhibit desirable aesthetic qualities and reduce the appearance of skin and body imperfections, while providing cosmetic effects that are typically achieved
3/160 through more invasive dermatological procedures administered, if as a whole.
[006] In one embodiment, the invention provides non-invasive body formulations that form a corrective body film on application to the subject, thereby improving the body's imperfections. The invention also provides methods of using such corrective body formulations. In another embodiment, the invention provides cleaners to remove the film.
[007] Thus, in one embodiment, the invention belongs, in part, to corrective body formulations for application to a subject's skin that comprise a) a reactive reinforcement component; and b) a cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a body corrective film is formed on the subject's skin and the film has a natural skin appearance.
[008] In one embodiment, the invention belongs, at least in part, to two corrective body part formulations for application to the skin of a subject comprising a) a reactive reinforcement component; and b) a cross-linking component; wherein the reactive reinforcement component and the crosslinking component are prevented from coming into contact before use; and wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a body corrective film is formed on the subject's skin.
[009] In one embodiment, the invention provides, at least in part, corrective body formulations for application to the skin of a subject comprising a) a reactive reinforcement component; and b) a cross-linking component; wherein the reactive reinforcement component has a viscosity between about 5,000 and about 1,000,000 cSt or cP at 25 ° C; and wherein the cross-linking component catalyzes an in situ re-linking of the reactive reinforcement component, so that a body corrective film is formed on the subject's skin.
[0010] In one embodiment, the invention belongs, at least in part, to corrective body formulations for application to the skin of a subject comprising a) a reactive reinforcement component; and b) a cross-linking component in which the reactive reinforcement component has a vinyl to hydride ratio between about 1:10 and about 1: 100; and wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a body corrective film is formed on the subject's skin.
[0011] In one embodiment, the invention belongs, at least in part, to body corrective films prepared by a process that comprises the steps of: a) applying a reactive reinforcement component to a subject's skin; and b) applying a crosslinking component to the reactive reinforcement component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a body corrective film is formed on the subject's skin.
[0012] In one embodiment, the invention belongs, at least in part, to body modeling films prepared by a process comprising the steps of a) applying a reactive reinforcement component to a subject's skin; and b) applying a crosslinking component to the reactive reinforcement component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that the body shaping film is formed on the subject's skin.
[0013] In one embodiment, the invention belongs, at least in part, to methods for correcting body imperfections in a subject comprising applying to the subject's skin a formulation comprising a) a first reactive reinforcement component; and b) one second
5/160 cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thus correcting body imperfections.
[0014] In one embodiment, the invention pertains, at least in part, to methods for protecting a subject's skin comprising applying to the subject's skin a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby protecting the skin.
[0015] In one embodiment, the invention belongs, at least in part, to methods for modeling a subject's body, comprising applying to a subject's body a formulation comprising
a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed in the body, thus shaping the body.
[0016] In one embodiment, the invention pertains, at least in part, to methods for delivering an agent to a subject, comprising applying to the subject's skin a formulation comprising a) a first reactive reinforcing component optionally comprising one or more agents; and b) a second cross-linking component optionally comprising one or more agents; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby releasing the agent to the subject.
[0017] In one embodiment, the invention belongs, at least in part, corrective body formulations for application to a subject's body, comprising at least one component of modulation of
6/160 pre-selected function, in which the composition forms a corrective body film when applied to the subject's body.
[0018] In one embodiment, the invention belongs, at least in part, to corrective body formulations for application to a subject's skin that targets a treatment area on a subject's body, comprising at least one specific pre-selected treatment component , in which the composition forms a corrective body film when applied to the target treatment area on the subject's body.
[0019] In one embodiment, the invention belongs, at least in part, to a cleaner that removes the film for use in removing a body corrective film, in which the film is prepared by a process comprising the steps of applying a component reactive reinforcement to the skin; and applying a crosslinking component to said reactive reinforcement component, and wherein said crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component.
[0020] In another embodiment, the invention belongs, at least in part, to a cleaner that removes the film comprising a wetting component of the film, a penetrating component, an intumescent film component and a film releasing component.
[0021] In some embodiments, the invention belongs to a formulation to repair a body corrective film applied to the skin, in which said formulation comprises a) a first reactive reinforcement component and b) a second cross-linking component, in which the cross-linking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin. [0022] In some embodiments, the invention belongs, at least in part, to a method for repairing a body corrective film applied to the skin comprising the steps of a) identifying an area of the film in need of repair; b) optionally smoothing the
7/160 edges of the film; and c) applying a formulation to repair the film, where the formulation comprises a first reactive reinforcement component and a second cross-linking component, wherein the cross-linking component catalyzes an in situ cross-linking of the reactive reinforcement component so that a film is formed on the skin, thus repairing the body corrective film.
[0023] In some embodiments, the invention belongs, at least in part, to a kit for repairing a body corrective film, the kit comprising a formulation comprising a) a first reactive reinforcement component and b) a second cross-linking component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin.
Brief Description of the Drawings [0024] Figure 1 is a graph illustrating the change in Young's Modulus of the skin after the application of a formulation of the invention. The change in Young's Module indicates that there is a reduction in skin stiffness when applying the formulation.
[0025] Figure 2 is a graph that illustrates the change in retraction time after applying a formulation of the invention. The change in the retraction time indicates that the skin is more elastic when applying the formulation.
[0026] Figure 3 is a graph illustrating the investigator's assessment of two formulations by attribute in a randomized double-blind clinical study. The formulations are provided in example 5. Classified attributes included reduced gloss reduction, pore reduction, deep crease reduction and fine crease reduction. For all attributes, the applications of these two films provided an improvement for the 22 subjects evaluated. These four attributes were further detailed by treatment location. These sites are forehead, crow's feet,
8/160 dark circles, and the nose channel ('number 11's'). Improvements were observed for each target treatment area.
[0027] Figure 4 is a graph that illustrates the assessor's assessment of two formulations described in example 5 by the attribute in a randomized double-blind clinical study. The assessor's assessments show an improvement in each of the beauty attributes classified after application of the formulations.
[0028] Figure 5 is a graph that illustrates the panel evaluation of two formulations described in example 5, by attribute, in a randomized double-blind clinical study. The attributes evaluated were youthful appearance, matification (or gloss reduction), pore size, uniform skin tone, stiffened skin appearance, and wrinkling. For each attribute, the panels, on average, experienced an improvement in each benefit after treatment with the formulations.
[0029] Figure 6 is a graph that illustrates the average age reduction of the panels as determined by the assessors. Age reductions in general of 8.7 years and 7.7 years of age were observed for formulation 60-140-LX2 and formulation 60-140-1, respectively.
[0030] Figure 7 is a graph that illustrates the average Griffith score resulting from blind assessment of the photographs of the panels. The Griffith score is a standardized qualitative measure of the extent of photodamage, where a score of 0 corresponds to no photodamage, and a score of 9 represents serious photodamage. For both examples, the Griffith score was reduced by 2.15 and 1.25 points, after applying the formula 60-140-LX2 and 60-140-1, respectively. This result is consistent with Figures 4 and 5, where the panels appeared younger after applying the formulation.
[0031] Detailed Description of the Invention [0032] In some embodiments, the invention belongs, at least in part, to body corrective formulations for application to the skin comprising a) a reactive reinforcement component; and b) a cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a body corrective film is formed on the skin.
[0033] The language corrective body formulation or formulation includes cosmetic compositions that, when applied to the body, form a film on the body that improves body imperfections. The language body imperfections includes those parts of a subject's body that the subject perceives as defective or flawed, or in which a specialist, for example, a dermatologist, a beautician or a plastic surgeon, could consider defective or failed. The language body imperfections includes skin imperfections, as well as sagging soft body tissues (for example, loose or flabby skin, sagging breasts, buttocks, abdomen, jowls, neck and the like). The language of skin imperfections includes those items on a subject's skin that the subject perceives as a defect or failure. Examples of skin imperfections include port-colored ax or nevus flammeus (eg nevus flammeus nuchae or nevus flammeus midline) melasma, wrinkles, blemishes, acne, warts, scars, tattoos, bruises, skin disfigurements, marks from birth, sun damage, age damage, uneven skin tone, sagging skin, skin roughness, hyperpigmentation, enlarged pores, telangiectasia, redness, shine, cellulite, stretch marks or loss of skin elasticity.
[0034] In one embodiment of the invention, the compositions, formulations or films of the invention result in visual and / or tactile improvement in the properties of the skin. In certain embodiments, the compositions, formulations or films of the invention mask, hide, or cover, but do not address the imperfection of the subject's skin or body.
10/160 [0035] In at least one modality, a skin or body imperfection does not include wounds or dermatological disorders.
[0036] The sore language includes skin lesions in which the skin is torn, cut or punctured. An injury is a breakdown of the skin. In one embodiment, the injury is caused by skin contact with a foreign object. The break in the skin can cause external bleeding. Injuries include open wounds, for example, abrasions, lacerations, incisions, perforations, avulsions or amputations. Injuries still include burn injuries. A burn is a type of injury caused by heat, electricity, chemicals, light, radiation or friction. [0037] The language dermatological disorder includes disorders that cause at least one symptom of a subject's skin that requires medical treatment. In one embodiment, dermatological disorders are caused by autoimmune disorders. In another modality, a dermatological disorder is caused by environmental factors, such as allergens or chemicals. Examples of symptoms of dermatological disorders requiring treatment are dermatitis, itchy skin, dry skin, scabs, blisters, or cracking of the skin, edema of the skin, or formation of skin lesions. Dermatological disorders include, but are not limited to, chronic lichen simplex, cutaneous lupus (for example, acute cutaneous lupus, subacute cutaneous lupus, chronic cutaneous lupus, chilean lupus erythematosus, discoid lupus erythematosus, lichen-lupus erythematosus overlap syndrome, paniculic lupus erythematosus, panicululus tumidous lupus erythematosus and warty lupus erythematosus), psoriasis (e.g., psoriasis vulgaris, psoriatic erythroderma, pustular psoriasis, drug-induced psoriasis, reverse psoriasis, seborrheic-type psoriasis and guttate psoriasis), eczema, eczema, eg, eczema contact dermatitis, xerotic eczema, seborrheic dermatitis, dehydrosis, discoid eczema, venous eczema, herpetiform dermatitis, neurodermatitis and auto-eczematization), or chronic dry skin.
11/160 [0038] In some modalities, the corrective body formulation is a corrective skin formulation. The corrective skin formulation language includes cosmetic compositions that, when applied to the skin, form a film on the skin that improves skin imperfections. In some modalities, the improvement is a complete improvement or partial improvement. A person skilled in the art might be able to determine the extent of improvement in one or more of the body imperfections using the methods described in example 6.
[0039] In some modalities, corrective body formulation is a formulation of body modeling. A body modeling formulation includes cosmetic compositions that, when applied to the skin, form a film that shapes the body on the subject's skin.
[0040] In some modalities, the corrective body formulation is a formulation that protects the skin. A protective skin formulation includes cosmetic compositions that, when applied to the skin, form a protective film on the subject's skin.
[0041] In some modalities, corrective body formulation can release cosmetic or therapeutic agents to a subject in need of it.
[0042] In some modalities, the body corrective formulation is used to repair a body corrective film.
[0043] In one embodiment, corrective body formulations include a reactive reinforcement component and a cross-linking component. The reactive reinforcement component language includes a component that, when applied to the skin as a first component, is the basis of the body corrective film that is formed when applying the crosslinking component to the reactive reinforcement component. In one embodiment, the reactive reinforcement component includes at least one reactive constituent and at least one reinforcement constituent.
[0044] The reactive constituent language includes one or more constituents of the reactive reinforcement component that provide the film forming elements of the formulation. In some embodiments, the reactive constituent includes at least one polysiloxane, polyethylene oxide, polypropylene oxide, polyurea, polyurethane, polyester (including polylactic-co-glycolic acid, polycaprolactone, polylactic acid, polyglycolic acid, and polyhydroxybutyrate, polyamide, or polysulfone. In another embodiment, the reactive constituent is a compound of formula I:
w-Fx-Hv + y — Z t (I) [0045] where [0046] W is R ¹ R ² R ³ SiO-, -OR ⁴ , -NR ⁵ R ⁶ , -CR ⁷ R ⁸ R ⁹ or C _5-10 aryl; [0047] X is -R ¹¹ R ¹² Si-O-, -OCONR ¹³ -, -NR ¹⁴ CONR ¹⁵ -, -CO-,
-NR ¹⁶ CO-, -SO2-, -O-, -S- or -NR ¹⁷ -;
[0048] V is absent, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, -O-, -NR ¹⁰ - or -S-;
[0049] Y is -R ¹⁸ R ¹⁹ Si-O-, -OCONR ²⁰ -, -NR ²¹ CONR ²² -, -CO-, -NR ²³ CO-, -SO2-, -O-, -S- or - NR ²⁴ ;
[0050] Z is -SiR ²⁵ R ²⁶ R ²⁷ , -OR ²⁸ , -NR ²⁹ R ³⁰ , -CR ³¹ R ³² R ³³ or C5-10 aryl;
[0051] R ¹ , R ² , R ³ , R ⁷ , R ⁸ , R ⁹ , R ¹¹ , R ¹² , R ¹⁸ R ¹⁹ , R ²⁵ , R ²⁶ , R ²⁷ , R ³¹ ,
R ³² and R ³³ are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy;
[0052] R ⁴ , R ⁵ , R ⁶ , R ¹³ , R ¹⁴ , R ¹⁵ , R ¹⁶ , R ¹⁷ , R ²⁰ , R ²¹ , R ²² , R ²³ , R ²⁴ , R ²⁸ ,
R ²⁹ and R ³⁰ are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl; and [0053] sets are each independently an integer from about 0 to about 6000.
[0054] X and Y of formula I represent an independent monomer unit. The number of X and Y monomer units present
13/160 in formula I is given by the value of s and t, respectively. Representative monomer unit includes:
RSi — o- HSi-O- J ““ ““ 2nd I ^E - _, or - I ISawI - R R IH R
[0055] where R is as defined for R ¹ , R ² , R ³ , etc., above.
[0056] It is understood that when more than one X (or Y) monomer unit is present (for example s (or t) is more than one), the values for R ¹¹ , R ¹² , R ¹³ , R ¹⁴ , R ¹⁵ , R ¹⁶ , R ¹⁷ , R ¹⁸ R ¹⁹ , R ²⁰ , R ²¹ , R ²² , R ²³ , and R ²⁴ are independently selected for each individual monomer unit described by - [X] s- (or - [Y] t -) - For example, if the value of the monomer unit X is -R ¹¹ R ¹² Si-O- and the value of s is 3, then - [X] s- is
- [R ¹¹ R ¹² Si-OR ¹¹ R ¹² Si-OR ¹¹ R ¹² Si-O] -.
[0057] In this example, it is understood that three R ¹¹ groups present may be the same or different from each other, for example, an R ¹¹ may be hydrogen, and the other two other R ¹¹ groups may be methyl.
[0058] W and Z of formula I represent independent end caps, one at each end. For example, terminal coverings include:
R
R
Si
R

H
OU - Si-R
14/160 [0059] where 5 denotes connection to a monomer unit and where R is as defined for R ¹ , R ² , R ³ , etc., above.
[0060] In one mode, [0061] W is R ¹ R ² R ³ SiO-, -OR ⁴ , -NR ⁵ R ⁶ , -CR ⁷ R ⁸ R ⁹ or C _5-10 aryl; [0062] X is -R ¹¹ R ¹² Si-O-, or -NR ¹⁴ CONR ¹⁵ -; [0063] -NR ¹⁰ - or V is absent, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, -O-, -S-; [0064] Y is -R ¹⁸ R ¹⁹ Si-O-, or -NR ²¹ CONR ²² -; [0065] Z is -SiR ²⁵ R ²⁶ R ²⁷ , -OR ²⁸ , -NR ²⁹ R ³⁰ , -CR ³¹ R ³² R ³³ or C5-10 ari- over there; [0066] 1 2 3 7 8 9 11 12 18 19 25 26 27 31R, R, R, R, R, R R, R, R R, R, R, R, R,
R ³² and R ³³ are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy;
[0067] R ⁴ , R ⁵ , R ⁶ , R ¹⁴ , R ¹⁵ , R ²¹ , R ²² , R ²⁸ , R ²⁹ and R ³⁰ are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl; and [0068] set are each independently an integer from about 0 to about 6000, where the sum of set is not 0.
[0069] In one mode, [0070] W is R ¹ R ² R ³ SiO-, -CR ⁷ R ⁸ R ⁹ or C _5-10 aryl; [0071] X is -R ¹¹ R ¹² Si-O-, or -NR ¹⁴ CONR ¹⁵ -; [0072] V is absent, C _1-20 alkyl, C _2-20 alkenyl, or C _5-10 aryl; [0073] Y is -R ¹⁸ R ¹⁹ Si-O-, or -NR ²¹ CONR ²² -; [0074] Z is -SiR ²⁵ R ²⁶ R ²⁷ , -CR ³¹ R ³² R ³³ or C5-10 aryl; [0075] 1 2 3 7 8 9 11 12 18 19 25 26 27 31R, R, R, R, R, R R, R, R R, R, R, R, R,
R ³² and R ³³ are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy;
[0076] R ¹⁴ , R ¹⁵ , R ²¹ , and R ²² are each independently hydrogen, C _1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl; and
15/160 [0077] s and t are each independently an integer from about 0 to about 6000, where the sum of s and t is not 0.
[0078] In one embodiment, V is absent, W is R ¹ R ² R ³ SiO-; X is -R ¹¹ R ¹² Si-O-; Y is -R ¹⁸ R ¹⁹ Si-O-; Z is -SiR ²⁵ R ²⁶ R ²⁷ ; and R ¹ , R ² , R ³ , R ¹¹ , R ¹² , R ¹⁸ , R ¹⁹ , R ²⁵ , R ²⁶ and R ²⁷ are each independently selected from C1-20 alkyl (e.g., C1 alkyl, as methyl) or C2-20 alkenyl (for example, C2 alkenyl, as vinyl). In one embodiment, at least one of R ¹ , R ² , R ³ , R ¹¹ , R ¹² , R ¹⁸ , R ¹⁹ , R ²⁵ , R ²⁶ and R ²⁷ is C2-20 alkenyl, for example, C2 alkenyl (for example example, vinyl). In another embodiment, at least two of R ¹ , R ² , R ³ , R ¹¹ , R ¹² , R ¹⁸ , R ¹⁹ , R ²⁵ , R ²⁶ and R ²⁷ are C2-20 alkenyl, for example, C2 alkenyl (eg example, vinyl). In some embodiments, at least one of R ¹ , R ² , R ³ , R ²⁵ , R ²⁶ and R ²⁷ are each C2-20 alkenyl, for example, C2 alkenyl (for example, vinyl).
[0079] In one embodiment, V is absent, W is R ¹ R ² R ³ SiO-; X is -R ¹¹ R ¹² Si-O-; Y is -R ¹⁸ R ¹⁹ Si-O-; Z is -SiR ²⁵ R ²⁶ R ²⁷ ; and R ¹ , R ² , R ³ , R ²⁵ , R ²⁶ and R ²⁷ are each independently selected from C1-20 alkyl (e.g., C1 alkyl, such as methyl) or C2-20 alkenyl (e.g., C2 alkenyl, like vinyl); and R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ are each independently selected from C 1-20 alkyl (e.g., C 1 alkyl, as methyl). In one embodiment, at least one of R ¹ , R ² , R ³ , and at least one of R ²⁵ , R ²⁶ and R ²⁷ is C2-20 alkenyl, for example, C2 alkenyl (for example, vinyl). In one embodiment, one of R ¹ , R ² , R ³ is C2 alkenyl (eg, vinyl) and the others are C1-20 alkyl (eg, C1 alkyl, such as methyl), and at least one of R ²⁵ , R ²⁶ and R ²⁷ is C2-20 alkenyl, for example, C2 alkenyl (for example, vinyl) and the others are C1-20 alkyl (for example, C1 alkyl, such as methyl). In one embodiment, at least one of R ¹¹ or R ¹² and at least one of R ¹⁸ or R ¹⁹ is C2-20 alkenyl, for example, C2 alkenyl (for example, vinyl) by at least one monomer unit. In one modality, one of
16/160
R ¹¹ or R ¹² is C2 alkenyl (eg vinyl) and the others are C1-20 alkyl (eg C1 alkyl, such as methyl), and at least one of R ¹⁸ or R ¹⁹ is C2-20 alkenyl, for example example, C ₂ alkenyl (eg, vinyl) and the others are C _1-20 alkyl (eg, C ₁ alkyl, such as methyl) for at least one monomer unit.
[0080] In some modalities, the organopolysiloxane includes fractions of vinyl only in the terminal covers of the polymer. In some embodiments, the organopolysiloxane includes fractions of vinyl only in the monomer unit, but not in the polymer end cap. In other embodiments, the organopolysiloxane includes fractions of vinyl in both end covers or in the polymer monomer unit. In one embodiment, the polymer includes two vinyl fractions located on the terminal cover, or within the monomer unit, or a combination thereof.
[0081] In one embodiment, on average at least two fractions of vinyl are present in the polymer. In a specific embodiment, at least two fractions of vinyl are present in the polymer and at least two fractions of vinyl are present in the two end caps of the polymer. In a specific embodiment, only two fractions of vinyl are present in the polymer. In a specific modality, only two fractions of vinyl are present in the polymer and are located in each of the terminal covers. In a specific embodiment, on average at least two fractions of vinyl are present in the polymer and at least two fractions of vinyl are present in one or more units of monomers of the polymer. In a specific embodiment, on average at least two fractions of vinyl are present anywhere in the polymer, but separated from another fraction of vinyl in about 2000 units of monomers, for example, 1500, 1600, 1700, 1800, 1900, 2000 , 2100, 2200, 2300, 2400, or 2500 units of monomers. In a modality
17/160 specific, on average at least two fractions of vinyl are present anywhere in the polymer, but separated from another fraction of vinyl in about 850 units of monomers, for example 350, 450, 550, 650, 750, 850 , 950, 1050, 1150, 1250, or 1350 units of monomers. In a specific embodiment, on average more than two fractions of vinyl are present anywhere in the polymer, but separated from another fraction of vinyl in about 40 units of monomers, for example, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, or 80 unit of monomers. In a specific modality, one or more Si-H units are present in addition to the vinyl fraction. Alternatively, in one embodiment, if a vinyl fraction is present then a Si-H is not present.
[0082] In one embodiment, V is absent, W is R ¹ R ² R ³ SiO-; X is -R ¹¹ R ¹² Si-O-; Y is -R ¹⁸ R ¹⁹ Si-O-; Z is -SiR ²⁵ R ²⁶ R ²⁷ ; R ¹ , R ² , R ³ , R ¹¹ , R ¹² ,
R ¹⁸ , R ¹⁹ , R ²⁵ , R ²⁶ and R ²⁷ are each independently are each independently selected from hydrogen or C 1-20 alkyl (for example, C 1 alkyl, as methyl). In one embodiment, R ¹ , R ² , R ³ , R ²⁵ , R ²⁶ and R ²⁷ are each independently selected from C 1-20 alkyl (for example, C ₁ alkyl, as methyl); and R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ are each independently selected from hydrogen or C 1-20 alkyl (for example, C 1 alkyl, as methyl), where at least one of e R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ are hydrogen for at least one monomer unit. In one embodiment, on average more than two Si-H units (for example one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen) are present in the polymer, for example 3- 15 Si-H units may be present. In a specific modality, 8 Si-H units are present. In one embodiment, one or more Si-H units (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen) are present in the polymer. In one embodiment, at least two monomer units include a -Si-H unit (for example, one or more
18/160 of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least three monomer units include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least three units of monomers include a Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least five monomer units include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least six units of monomers include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least seven monomer units include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least eight monomer units include a Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, a Si-H unit can be present in one or both end caps in addition to being present in a monomer unit as described above. In a specific embodiment, Si- (alkyl) or Si- (vinyl) units may be present in the polymer. In a specific modality, only Si-CH ₃ and Si-H units are present. In a specific embodiment, monomer units or end caps include C ₁ -C ₂₀ alkyl, specifically methyl groups, for the non-Si-H positions of the polymer.
[0083] In a specific modality, on average at least two Si-H units are present in the polymer. In a specific embodiment, on average at least two Si-H fractions are present anywhere in the polymer, but separated from another Si-H fraction in about 2000 units of monomers, for example, 1500, 1600, 1700, 1800, 1900 , 2000, 2100, 2200, 2300, 2400, or 2500 units of monomers. In a specific embodiment, on average at least two Si-H units are present anywhere in the polymer,
19/160 but separated from another Si-H fraction in about 850 units of monomers, for example, 350, 450, 550, 650, 750, 800, 850, 950, 1050, 1150, 1250, or 1350 units of monomers. In a specific embodiment, on average more than two Si-H units are present anywhere in the polymer, but separated from another Si-H fraction in about 40 units of monomers, for example, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, or 80 unit of monomers.
[0084] In one aspect of any of the above, the sum of s and t is an integer from about 1000 to about 8000; from about 1300 to about 2700; from about 1500 to about 2700;
from about 1600 to about 2600; from about 1600 to about 2500;
from about 1700 to about 2500; from about 1800 to about 2400;
from about 1800 to about 2300; from about 1900 to about 2300;
from about 2000 to about 2200; from about 2050 to about 2150;
of about 2100.
[0085] In one aspect of either mode, the sum of s and t is an integer from about 200 to about 1100; from about 600 to about 1100; from about 700 to about 1000; from about 800 to about 900; from about 825 to about 875; about 850; from about 200 to about 800; from about 225 to about 700; from about 250 to about 600; from about 275 to about 500; from about 300 to about 400; from about 350 to about 400; of about 375. In a specific embodiment, the sum of s and t is an integer of about 850.
[0086] In one aspect of either mode, the sum of s and t is an integer from about 5 to about 1300; from about 10 to about 1100; from about 10 to about 600; from about 15 to about 500; from about 15 to about 400; from about 20 to about 300; from about 20 to about 200; from about 25 to about 100;
20/160 of about 25 to about 75; from about 30 to about 50; about 40.
[0087] In some embodiments, the reactive constituent comprises at least one organopolysiloxane. The term organopolysiloxane includes compounds of formula II:
(II) [0088] where R ^1a , R ^2a , R ^3a , R ^4a , R ^5a , R ^6a , R ^7a , R ^8a , R ^9a and R ^10a are each independently selected from hydrogen, C1-20 alkyl, C _2-20 alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy epeq are each independently an integer between 10 and about 6000. [0089] In some embodiments, the organopolysiloxane is a compound of formula IIa:
^1a 'R ^10a ' /, ^{1 1 1 1} // 5í_q _Qi_nl — 1-Qi-nl— qí — J
R ^3a
Si-O
R ^4a '
R ^9a
Si-OR ^{5a J} q
R ^8a '
-SiR ^6a (IIa) [0090] where R ^1a , 'R ^3a ', R ^4a ', R ^5a ', R ^6a ', R ^8a ', R ^9a 'and R ^10a ' are each independently selected from hydrogen, C1-20 alkyl, C2-20 alkenyl, C5-10 aryl, hydroxyl or C1-20 alkoxy epeq are each independently an integer between 10 and about 6000. In one embodiment, R ^1a , 'R ^3a ', R ^4a ', R ^5a ', R ^6a ', R ^8a ', R ^9a 'and R ^10a ' are alkyl (for example, C1 alkyl, such as methyl).
[0091] The term alkyl includes both saturated branched or straight chain aliphatic hydrocarbon groups containing the specified number of carbon atoms. The term C _1-20 alkyl includes branched and straight chain aliphatic groups containing between 1 and 20 carbons. Examples of alkyl fractions include methyl, ethyl, n-propyl, ipropyl, n-butyl, s-butyl, t-butyl, n-pentyl, n-hexyl, isopropyl, isobuti21 / 160 la, sec-butyl, tert-butyl, isopentyl, and s-pentyl. In addition, the term alkyl includes both unsubstituted and substituted alkyl, the latter of which refers to alkyl moieties containing substituents (for example, F, Cl, Br, I, NO ₂ , CN, alkyl, aryl, hydroxyl, alkoxy, COCH ₃ and the like) replacing a hydrogen in one or more carbons of the hydrocarbon structure.
[0092] Alkenyl term includes the specific number of hydrocarbon atoms in linear or branched configuration with one or more unsaturated carbon-carbon bonds that can occur at any stable point along the chain, such as ethylene and propenyl. The C _2-20 alkenyl language includes straight and branched chain hydrocarbon groups of between 1 and 20 carbons with one or more unsaturated carbon-carbon bonds. In addition, the term alkenyl includes both unsubstituted alkenyl and substituted alkenyl, the latter of which refers to alkenyl fractions containing substituents (for example, F, Cl, Br, I, NO2, CN, alkyl, aryl, hydroxyl, alkoxy , COCH3 and the like) replacing a hydrogen in one or more carbons of the hydrocarbon structure.
[0093] Aryl term includes 5-10 membered monocyclic, bicyclic or tricyclic rings, in which at least one ring, if more than one is present, is aromatic. The term aryl further includes heteraryl fractions in which a hetero atom (for example, N, O or S) replaces one or more carbons in the monocyclic, bicyclic or tricyclic ring. The term aryl also includes both unsubstituted and substituted aryl, the latter of which refers to aryl fractions containing substituents (for example, F, Cl, Br, I, NO2, CN, alkyl, hydroxyl, alkoxy, COCH3 and the like) replacing a hydrogen in one or more aromatic carbon rings.
[0094] hydroxyl term includes -OH.
[0095] alkoxy term includes fractions where an O is
22/160 covalently attached to a C _1-20 alkyl group, as defined above. [0096] In some embodiments, the organopolysiloxane is finished vinyl. The vinyl terminated organopolysiloxane language includes organopolysiloxanes of formula II in which one or both of R ^2a and R ^7a are replaced with a C2 alkyl fraction, for example, a vinyl fraction (for example, -CH = CH2). In a specific embodiment, a finished vinyl organopolysiloxane includes organopolysiloxanes of formula II in which one or both of R ^2a and R ^7a are replaced with a C2 alkyl fraction, for example, a vinyl fraction (for example, CH = CH2), and R ^1a , R ^3a , R ^4a , R ^5a , R ^6a , R ^8a , R ^9a and R ^10a are independently selected from C _1-20 alkyl, for example, methyl.
[0097] In other modalities, the organopolysiloxane is selected from: finished vinyl polydimethylsiloxane; diphenylsiloxane finished vinyl-dimethylsiloxane copolymers; finished polyphenylmethylsiloxane vinyl, finished vinylphenylmethyl vinylphenylmethyl-phenylmethylsiloxane copolymer; vinyl terminated trifluoropropylmethylsiloxane -dimethylsiloxane copolymer; finished vinyl diethylsiloxane-copolymer dimethylsiloxane; vinylmethylsiloxane-dimethylsiloxane copolymer, finished trimethylsiloxy; vinylmethylsiloxane-dimethylsiloxanes copolymer, finished silanol; vinylmethylsiloxane-dimethylsiloxanes copolymer, finished vinyl; vinyl gums; vinylmethylsiloxane homopolymers; polymers of vinyl T structure; finished monovinyl polydimethylsiloxanes; vinylmethylsiloxane terpolymers; vinylmethoxysilane homopolymers and combinations thereof. [0098] In some embodiments, the organopolysiloxane is a high viscosity organopolysiloxane, a low viscosity organopolysiloxane or a combination thereof.
[0099] When organopolysiloxane is a combination of high and low viscosity organopolysiloxanes, the combination of a high viscosity and low viscosity organosiloxane vinyl provides a bimodal distribution of organosiloxane molecular weights. In
23/160 at least one modality, organopolysiloxane is a combination of vinyl-terminal organopolysiloxanes of high and low viscosity providing a bimodal distribution of the vinyl terminated organopolysiloxane. In one embodiment, the organopolysiloxane is a combination of formulas I, II, IIa, IIb, and IIc, specifically, of formula IIa, IIb and / or IIc, or more specifically, of formula IIb and IIc, providing a bimodal distribution of the organopolysiloxane vinyl-finished. In one embodiment, the bimodal polymer molecular weight distribution is represented by a molecular weight ratio (for example, the sum of s and t) of the high viscosity organopolysiloxanes to the low viscosity organopolysiloxane. In a modality, this ratio is 2 to 3. In a specific modality, this ratio is 2.5. [00100] The term viscosity refers to the measure of the resistance of a fluid that is being deformed by shear stress or tensile stress. A person skilled in the art without proper experimentation might be able to determine how to measure the viscosity of a fluid, for example, using a viscometer or a rheometer. Representative methods include the use of a capillary viscometer, rotational viscometer or rheometer to measure viscosity at a specific instrument voltage. Specific methods for determining the viscosity of a fluid are shown in example 8.
[00101] The high viscosity organopolysiloxane language includes organopolysiloxanes with a viscosity between about 100,000 and about 500,000 cSt or cP at 25 ° C, for example, and between about 110,000 and about 450,000 cSt or cP at 25 ° C, between about 120,000 and about 400,000 cSt or cP at 25 ° C, between about 125,000 and about 350,000 cSt or cP at 25 ° C, between about 130,000 and about 300,000 cSt or cP at 25 ° C, between about 135,000 and about 250,000 cSt or cP at 25 ° C, between about 140,000 and about 200,000 cSt or cP at 25 ° C, between about 145,000 and about 190,000 0 cSt or cP a
24/160
25 ° C, between about 150,000 and about 185,000 cSt or cP at 25 ° C, between about 155,000 and about 175,000 cSt or cP at 25 ° C, or between about 160,000 and about 170,000 cSt or cP at 25 ° C. In some embodiments, the viscosity of the high viscosity organopolysiloxane is between about 140,000 and about 200,000 cSt or cP at 25 ° C. In one embodiment, the high viscosity organopolysiloxane has a viscosity of about 165,000 cSt or cP at 25 ° C.
[00102] In one embodiment, the average molecular weight of the high viscosity organopolysiloxane is between about 100,000 and about 200,000 Da, for example, between about 115,000 and about 195,000 Da, between about 120,000 and about 190,000 Da, between about 125,000 and about 185,000 Da, between about 130,000 and about 180,000 Da, between about 135,000 and about 175,000 Da, between about 140,000 and about 170,000 Da, between about 145,000 and about 165,000 Da or between about 150,000 and about 160,000 Da. In one embodiment, the average molecular weight of the high viscosity organopolysiloxane is about 155,000 Da.
[00103] In some embodiments, the high viscosity organopolysiloxane is of formula II, where R ^2a and R ^7a are C2-20 alkenyl, for example, C2 alkenyl (for example, vinyl) and R ^1a , R ^3a , R ^4a , R ^5a , R ^6a , R ^8a , R ^9a and R ^10a are each C1-20 alkyl, for example, C ₁ alkyl (for example, methyl). In some embodiments, the high viscosity organopolysiloxane is finished vinyl. In other embodiments, the high viscosity organopolysiloxane is finished vinyl polydimethylsiloxane. [00104] In some embodiments, the high viscosity finished vinyl organopolysiloxane has a vinyl weight percentage between about 0.010 and about 0.100, for example, between about 0.015 and about 0.080, between about 0.020 and about 0.075 , between about 0.025 and about 0.060, or between about 0.030 and about 0.050. In one embodiment, the high viscosity organopolysiloxane has a
25/160 vinyl weight percentage between about 0.030 and about 0.040. [00105] In other embodiments, the high viscosity organopolysiloxane has a vinyl equivalent per kilogram between about 0.0100 and about 0.0200, for example, between about 0.0110 and about 0.0190, between about 0.0115 and about 0.0180, between about 0.0120 and about 0.0170, between about 0.0125 and about 0.0165 or between about 0.013 and about 0.016.
[00106] In one embodiment, the high viscosity organopolysiloxane has an average of at least two vinyl units per high viscosity organopolysiloxane. In one embodiment, the monomer unit including a vinyl fraction is spaced along the polymer. In one embodiment, the monomer unit containing vinyl is spaced about 2000 units of monomers from another monomer unit containing vinyl or a terminal cover containing vinyl. For example, the vinyl units in the high viscosity organopolysiloxanes are separated by 1500, 1600, 1700, 1800, 1900, 2000, 2100, 2200, 2300, 2400, or 2500 monomer units.
[00107] In some embodiments, the high viscosity organopolysiloxane is selected from: finished vinyl polydimethylsiloxane; finished vinyl diphenylsiloxane - dimethylsiloxane copolymers; polyphenylmethylsiloxane vinyl finished, vinylphenylmethyl finished vinylphenylsiloxane-phenylmethylsiloxane copolymer; vinyl terminated trifluoropropylmethylsiloxane dimethylsiloxane copolymer; finished vinyl diethylsiloxane - copolymer dimethylsiloxane; vinylmethylsiloxane-dimethylsiloxane copolymer, finished trimethylsiloxy; vinylmethylsiloxane-dimethylsiloxane copolymers, finished silanol; vinylmethylsiloxane-dimethylsiloxane copolymers, finished vinyl; vinyl gums; vinylmethylsiloxane homopolymers; polymers of vinyl T structure; finished monovinyl polydimethylsiloxanes; vinylmethylsiloxane terpolymers; vinylmethoxysilane homopolymers and combinations thereof.
26/160 [00108] The low viscosity organopolysiloxane language includes organopolysiloxanes with a viscosity between about 500 and about 50,000 cSt or cP at 25 ° C, for example, between about 1,000 and about 45,000 cSt or cP at 25 ° C, between about 1,500 and about 40,000 cSt or cP at 25 ° C, between about 2,000 and about 35,000 cSt or cP at 25 ° C, between about 2,500 and about 30,00 0 cSt or cP at 25 ° C , between about 3,000 and about 25,000 cSt or cP at 25 ° C, between about 3,500 and about 20,000 cSt or cP at 25 ° C, between about 4,000 and about 15,000 cSt or cP at 25 ° C, or between about 4,000 and about 12,000 cSt or cP at 25 ° C. In some embodiments, the low viscosity organopolysiloxane includes organopolysiloxanes with a viscosity between about 100 and about 5,000 cSt or cP at 25 ° C, for example, between about 200 and about 40 00 cSt or cP at 25 ° C , between about 300 and about 3000 cSt or cP at 25 ° C, between about 400 and about 2000 cSt or cP at 25 ° C or between about 750 and about 1500 cSt or cP at 25 ° C. In one embodiment, the low viscosity organopolysiloxane has a viscosity of about 10,000 cSt or cP at 25 ° C. In some embodiments, the low viscosity organopolysiloxane has a viscosity of about 1000 cSt or cP at 25 ° C.
[00109] In some embodiments, low viscosity organopolysiloxane has an average molecular weight between about 20,000 and about 80,000 Da, for example, between about 50,000 and about 75,000 Da, between about 55,000 and about 70,000 Da, between about 60,000 and about 65,000 Da or between 62,000 and about 63,000 Da. In one embodiment, the low viscosity organopolysiloxane has an average molecular weight of about 62,700 Da. In one embodiment, the low viscosity organopolysiloxane has a weight average molecular weight of about 28,000 Da.
[00110] In some modalities, low-level organopolysiloxane
27/160 viscosity is of formula II, where R ^2a and R ^7a are C2-20 alkenyl, for example, C2 alkenyl (eg, vinyl) and R ^1a , R ^3a , R ^4a , R ^5a , R ^6a , R ^8a , R ^9a and R ^10a are each C1-20 alkyl, for example, C ₁ alkyl (for example, methyl). In some embodiments, the low viscosity organopolysiloxane is finished vinyl. In other embodiments, the low viscosity organopolysiloxane is finished vinyl polydimethylsiloxane.
[00111] In some embodiments, low viscosity organopolysiloxane has a vinyl weight percentage between about 0.010 and about 0.30, for example, between about 0.020 and about 0.29, between about 0.030 and about between 0.28, between about 0.040 and about 0.27, between about 0.050 and about 0.26, between about 0.060 between about 0.25, between about 0.070 and about 0.24, between about 0.080 and about 0.23, or between about 0.090 and about 0.22. In some embodiments, low viscosity organopolysiloxane has a vinyl weight percentage between about 0.18 and about 0.26. [00112] In other embodiments, the low viscosity organopolysiloxane has a vinyl equivalent per kilogram between about 0.010 and about 0.100, for example, between about 0.015 and about 0.090, between about 0.020 and about 0.080, between about 0.025 and about 0.070, between about 0.030 and about 0.060 or between about 0.040 and about 0.050. In some embodiments, low viscosity organopolysiloxane has a vinyl equivalent per kilogram between about 0.030 and about 0.040.
[00113] In other modalities, low viscosity organopolysiloxane has on average at least two units of vinyl per low speed organpolysiloxane. In one embodiment, the monomer units including a vinyl fraction are spaced by the polymer. In one embodiment, the monomer unit containing vinyl is spaced about 800 units of monomers from the other unit of monomer containing vinyl or a terminal cover containing vinyl. For example, the vinyl units in the low viscosity organopolysiloxane are separated by 450, 550, 650, 750, 800, 850, 950, 1050, 1150, 1250, or 1350 monomer units.
[00114] In some embodiments, the low viscosity organopolysiloxane is selected from: finished vinyl polydimethylsiloxane; finished vinyl diphenylsiloxane - dimethylsiloxane copolymers; polyphenylmethylsiloxane vinyl finished, vinylphenylmethyl vinyl copolymer vinylphenylsiloxane-phenylmethylsiloxane; vinyl terminated trifluoropropylmethylsiloxane-dimethylsiloxane copolymer; diethylsiloxanodimethylsiloxane finished vinyl copolymer; vinylmethylsiloxane-dimethylsiloxane copolymer, finished trimethylsiloxy; vinylmethylsiloxane-dimethylsiloxane copolymers, finished silanol; vinylmethylsiloxane-dimethylsiloxane copolymers, finished vinyl; vinyl gums; vinylmethylsiloxane homopolymers; polymers of vinyl T structure; finished monovinyl polydimethylsiloxanes; vinylmethylsiloxane terpolymers; vinylmethoxysilane homopolymers and combinations thereof.
[00115] In some embodiments, organopolysiloxane is a compound of formula IIb:
[00116] where R ^1c , R ^3c , R ^4c , R ^5c , R ^6c , R ^8c , R ^9c and R ^10c are each independently selected from hydrogen, C1-20 alkyl, C2-20 alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy eeef are each independently an integer between 10 and about 6000. In one embodiment, R ^1c , R ^3c , R ^4c , R ^5c , R ^6c , R ^8c , R ^9c and R ^10c are alkyl (for example, C ₁ alkyl, such as methyl). In some embodiments, the sum of eef is an integer from about 1000 to about 8000; from about 1300 to about 2700; from about 1500 to about 2700; from about 1600 to about 2600; from about 1600 to about 2500; from about 1700 to about 2500; from about 1800 to about 2400; from about 1800 to about 2300; from about 1900 to about 2300; from about 2000 to about 2200; from about 2050 to about 2150; of about 2100.
[00117] In some embodiments, organopolysiloxane is a compound of formula IIc:
> (IIc), [00118] where R ^1d , R ^3d , R ^4d , R ^5d , R ^6d , R ^8d , R ^9d and R ^10d are each independently selected from hydrogen, C _1-20 alkyl, C _{2- 20} alkenyl, C _5-10 aryl, hydroxyl or C _1-20 alkoxy egej are each independently an integer between 10 and about 6000. In one embodiment, R ^1d , R ^3d , R ^4d , R ^5d , R ^6d , R ^8d , R ^9d and R ^10d are alkyl (for example, C1 alkyl, as methyl). In some embodiments, the sum of gej is an integer from about 200 to about 1100; from about 600 to about 1100; from about 700 to about 1000; from about 800 to about 900; from about 825 to about 875; about 850; from about 200 to about 800; from about 225 to about 700; from about 250 to about 600; from about 275 to about 500; from about 300 to about 400; from about 350 to about 400; of about 375. In some embodiments, the sum of gej is an integer of about 850.
30/160 [00119] In some embodiments, the reactive constituent comprises at least one polysiloxane functionalized with hydride. The hydride functionalized polysiloxane language includes compounds of formula III:
R ^1b
R ^2b -Si-O □ 3b ₅ 10b
9b
R '
8b
-n - Qi_n- - o; _D7b
Si-O j4b
Si-O
I j5b
-τη
-Si-R ^z
I
36b (III) [00120] where R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are each independently selected from hydrogen, C1-20 alkyl , C2-20 alkenyl, C5-10 aryl, hydroxyl or C1-20 alkoxy emen are each independently an integer between 10 and about 6000, provided that at least one of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are hydrogen. In some embodiments, at least one of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b is hydrogen and the others are C1-20 alkyl. In some embodiments, at least two of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are hydrogen (for example, two Si-H units per molecule hydride functionalized polysiloxane). In other embodiments, at least three of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are hydrogen (for example, three Si-H units per molecule hydride functionalized polysiloxane). In some embodiments, at least two of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are hydrogen (for example, two Si-H units per molecule of polysiloxane functionalized with hydride) and the others are C1-20 alkyl. In other embodiments, at least three of R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b , R ^9b and R ^10b are hydrogen (for example, three Si-H units per molecule of polysiloxane functionalized with hydride) and the others are C1-20 alkyl. In some embodiments, at least two of R ^4b , R ^5b , R ^9b and R ^10b are hydrogen (for example, two Si-H units per hydride-functionalized polysiloxane molecule) and the rest are C _1-20 alkyl. In other modalida31 / 160 de, at least three of R ^4b , R ^5b , R ^9b and R ^10b are hydrogen (for example, three Si-H units per hydride-functionalized polysiloxane molecule) and the rest are C _1-20 alkyl .
[00121] In one embodiment, at least more than two monomers of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). For example, on average 2 to 15 units of formula III monomers include a Si-H unit. In one embodiment, at least two monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least three monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least four monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least five monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least six monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least seven monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In one embodiment, at least eight monomer units of formula III include a -Si-H unit (for example, one or more of R ¹¹ , R ¹² , R ¹⁸ , and R ¹⁹ is hydrogen). In a specific embodiment, non-Si-H positions can include a Si- (alkyl) or Si- (vinyl) unit. In a specific embodiment, the non-Si-H positions are Si-CH3. In one embodiment, the Si-H units in the organopolysiloxane functionalized hydride are separated by 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 60, 65, 70, 75, 80, 85, 90, 100, 125, 150, or 200 unit of monomers.
32/160 [00122] In one aspect of either embodiment, the sum of m and n is an integer from about 10 to about 1300; from about 10 to about 1100; from about 10 to about 600; from about 15 to about 500; from about 15 to about 400; from about 20 to about 300; from about 20 to about 200; from about 25 to about 100; from about 25 to about 75; from about 30 to about 50; about 40.
[00123] In some embodiments, the hydride-functionalized polysiloxane includes Si-H units only the polymer end caps. In some embodiments, the polysiloxane includes SiH units only in the monomer unit, but not in the polymer end cap. In other embodiments, the polysiloxane includes Si-H units in both end caps or in the polymer monomer unit. In one embodiment, the polysiloxane includes two to twelve Si-H units located on the terminal cover, or within the monomer unit, or a combination thereof. In one embodiment, the polysiloxane includes four to fifteen Si-H units located on the terminal cover, or within the monomer unit, or a combination thereof. In one embodiment, the polysiloxane includes eight Si-H units located on the terminal cover, or inside the monomer unit, or a combination thereof.
[00124] In some embodiments, the hydride-functionalized polysiloxane has a viscosity between about 5 and about 11,000 cSt or cP at 25 ° C, for example, between about 10 and about 10,000 cSt or cP at 25 ° C, between about 15 and about 5.00 0 cSt or cP at 25 ° C, between about 20 and about 1,000 cSt or cP at 25 ° C, between about 25 and about 500 cSt or cP at 25 ° C, between about 30 and about 100 cSt or cP at 25 ° C, and between about 40 and about 50 cSt or cP at 25 ° C. In one embodiment, the polysiloxane functionalized with hydride has a viscosity of about 45 cSt or cP at 25 ° C.
33/160 [00125] In some embodiments, hydride-functionalized polysiloxane has an average molecular weight between about 900 and about 60,000 Da, for example, between about 1000 and about 50,000 Da, between about 1200 and about 25,000 Da, between about 1400 and about 20,000 Da, between about 1600 and about 15,000 Da, between about 1800 and about 10,000 Da, between about 2000 and about 5000 Da, between about 2200 and about 4000 Da, and between 2300 and about 2500 Da. In one embodiment, the average molecular weight of the hydride functionalized polysiloxane is about 2400 Da.
[00126] In some embodiments, the hydride-functionalized polysiloxane has a percentage content of SiH between about 3 and about 45%, for example, between about 5 and about 40%, between about 10 and about 35% , between about 20 and about 30%, or between about 26 and 27%. In some embodiments, the hydride-functionalized polysiloxane has a percentage content of about 26% SiH.
[00127] In some embodiments, the hydride-functionalized polysiloxane has a SiH content between about 0.500 mmol / g and about 10.00 mmol / g, for example, between about 1.00 mmol / g and about 9.00 mmol / g, between about 2.00 and about 8.00 mmol / g, between about 3.00 mmol / g and about 7.00 mmol / g, and about 4.00 mmol / g and about 6 .00 mmol / g. In one embodiment, the hydride-functionalized polysiloxane has a SiH content between about 4.00 and about 5.00 mmol / g, for example, 4.35 mmol / g.
[00128] In other embodiments, the polysiloxane functionalized with hydride is finished alkyl. The finished alkyl language includes functionalized polysiloxane hydrides of formula III in which one or both of R ^2b and R ^7b are C1-20 alkyl. In some embodiments, finished alkyl includes polysiloxane functionalized with hydrides of formula III in which one, two, three, four, five or six of R ^1b , R ^2b , R ^3b , R ^6b , R ^7b and R ^8b are C _1-20 alkyl. In one embodiment, R ^1b , R ^2b , R ^3b , R ^4b , R ^5b ,
34/160
R ^6b , R ^7b , R ^8b and R ^10b are each C1-20 alkyl, for example, C1 alkyl (for example, methyl) and R ^9b is hydrogen. In one embodiment, R ^1b , R ^2b , R ^3b , R ^4b , R ^5b , R ^6b , R ^7b , R ^8b and R ^9b are each C1-20 alkyl, for example, C ₁ alkyl (for example, methyl) and R ^10b is hydrogen.
[00129] In some embodiments, the hydride-functionalized polysiloxane is selected from the group consisting of finished polydimethylsiloxane hydride; polyphenyl- (dimethylhydrosiloxy) siloxane, finished hydride; methylhydrosiloxane-phenylmethylsiloxane copolymer, finished hydride; methylhydrosiloxane-dimethylsiloxane copolymers, finished trimethylsiloxy; polymethylhydrosiloxanes, finished trimethylsiloxy; polyethylhydrosiloxane, triethylsiloxane, methylhydrosiloxanophenyloctylmethylsiloxane copolymer; methylhydrosyloxanophenyloctylmethylsiloxane terpolymer and combinations thereof.
[00130] In some embodiments, the reactive constituent comprises combinations of polymers of formulas I, II, IIa, IIb, IIc, IId, and / or III. In a specific embodiment, the reactive constituent comprises a combination of polymers of formulas IIa, IIb, IIc and / or III. In a specific embodiment, the reactive constituent comprises a combination of polymers of formulas IIb, IIc and III.
[00131] In some embodiments, the reactive constituent comprises a combination of high molecular weight organopolysiloxanes vinyl, low molecular weight organopolysiloxanes vinyl, and / or organopolysiloxane functional hydrides. In one embodiment, each of the high and low molecular weight organopolysiloxanes includes on average at least two fractions of vinyl per polymer. In a specific embodiment, each organopolysiloxane vinyl includes exactly two fractions of vinyl. In one embodiment, the ratio of high molecular weight organopolysiloxane to low molecular weight organopolysiloxane is 2 to 3, for example 2, 2.5 or 3. The ratio can be selected to adjust the chemical and physical properties of the film to suit one
35/160 specific method or body part. In one embodiment, the functionalized hydride organopolymer includes on average more than two Si-H units in the polymer. In a specific modality, there are 8 Si-H units per functionalized organopolysiloxane hydride.
[00132] In some embodiments, the reactive constituent comprises high molecular weight organopolysiloxane functionalized hydrides, low molecular weight organopolysiloxane functionalized hydride, and / or organopolysiloxane vinyl. In one embodiment, each of the high and low molecular weight organopolysiloxanes includes on average at least two Si-H units per polymer. In a specific embodiment, each functionalized organopolysiloxane hydride includes exactly two Si-H fractions. In one embodiment, the ratio of high molecular weight organopolysiloxane to low molecular weight organopolysiloxane is 2 to 3, for example 2, 2.5 or 3. The ratio can be selected to adjust the chemical and physical properties of the film to suit a specific method or body part. In one embodiment, the vinyl organopolymer includes on average greater than at least two vinyl units in the polymer. In a specific embodiment, there are 8 vinyl units per organopolysiloxane vinyl.
[00133] The reinforcement constituent language includes one or more constituents of the reactive reinforcement component that provides the required physical properties of the film that result from in situ reaction between the reactive reinforcement component and the crosslinking component. Such physical properties include, for example, mechanical elements (for example, elasticity, durability, fracture deformation, tensile strength, etc.), biocompatibility (for example, selective breathability, adhesion, etc.), optical effects (for example, reflectance, color, etc.) and surface modulation (eg texture, chemistry, etc.). Examples of reinforcing constituents include clays, (for example, Al2O3,
36/160
SiO ₂ ), chalk, talc, calcite (eg CaCO ₃ ), mica, barium sulfate, zirconium dioxide, zinc sulfide, zinc oxide, titanium dioxide, aluminum oxide, silica aluminates, calcium silicates , or optionally surface-treated silica (for example, fumed silica, hydrated silica or anhydrous silica). In some embodiments, the reinforcing constituent is silica, for example, surface-treated silica, such as hexamethyldisilazane-treated silica.
[00134] In some embodiments, the reinforcing constituent has a surface area between about 100 and about 300 m ² / g, for example, between about 110 and about 250 m ² / g, between about 120 and about 225 m ² / g, between about 130 and about 200 m ² / g, between about 135 and about 185 m ² / g, between about 160 and about 170 m ² / g, and between about 164 and about 166 m ² / g. In one embodiment, the reinforcing constituent has a surface area of about 160 ± 25 m ² / g.
[00135] In some embodiments, the reinforcing constituent has an average particle size between about 1 and about 20 pm.
[00136] In some embodiments, the reinforcing constituent is composed of a low viscosity organopolysiloxane and / or a high viscosity.
[00137] In some embodiments, reactive constituent and reinforcement constituent comprise between about 20 and about 90% of the reactive reinforcement component, for example, between about 40% and about 60% of the reactive reinforcement component. In some embodiments, the reactive constituent and reinforcement constituent comprise between about 45.0 and about 61.0% of the reactive reinforcement component, for example, about 45.0%, about 45.5%, about 46.0%, about
46.5%, about 47.0%, about 47.5%, about 48.5%, about
49.0%, about 49.5%, about 50.0%, about 50.5%, about
51.0%, about 51.5%, about 52.0%, about 52.5%, about
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53.0%, about 53.5%, about 54.0%, about 54.5%, about
55.0%, about 55.5%, about 56.0%, about 56.5%, about
57.0%, about 58.0%, about 58.5%, about 59.0%, about
59.5%, about 60.0%, or about 60.5%. In some embodiments, the reactive constituent and the reinforcement constituent comprise about 45% of the reactive reinforcement component. In one embodiment, the reactive constituent and reinforcement constituent comprise about 48.0% of the reactive reinforcement component. In some embodiments, the reactive constituent and the reinforcement constituent comprise about 50.0% of the reactive reinforcement component. In another embodiment, the reactive constituent and the reinforcement constituent comprise about 51.0% of the reactive reinforcement component. In some embodiments, the reactive constituent and the reinforcement constituent comprise about 51.5% of the reactive reinforcement component. In another embodiment, the reactive constituent and the reinforcement constituent comprise about 54.5% of the reactive reinforcement component. In another embodiment, the reactive constituent and the reinforcement constituent comprise about 55.0% of the reactive reinforcement component. In some embodiments, the reactive constituent and the reinforcement constituent comprise about 59.5% of the reactive reinforcement component. In another embodiment, the reactive constituent and the reinforcement constituent comprise about 60.5% of the reactive reinforcement component. In some embodiments, the reactive constituent and reinforcement constituent comprise between about 30.0 and about 40.0% of the reactive reinforcement component, for example, about 30.0%, about 30.5%, about 31.0%, about 31.5%, about 32.0%, about 32.5%, about 33.0, about
33.5%, about 34.0%, about 34.5%, about 35.0%, about
35.5%, about 36.0%, about 36.5%, about 37.0%, about
37.5%, about 38.0%, about 38.5%, about 39.0%, about
39.5%, about 40.0%. In some embodiments, the reactive constituent and reinforcement constituent comprise between about 33.0 and about 40.0% of the reactive reinforcement component.
[00138] In one embodiment, the reinforcement constituent comprises between about 8.0 and about 13.0% of the reactive reinforcement component, for example, about 8.5%, about 9.0%, about 9.5%, about 10.0%, about 10.5%, about 11.0%, about 11.5%, about 12.0% or about 12.5%. In some embodiments, the reinforcement constituent comprises about 8.5% of the reactive reinforcement component. In one embodiment, the reinforcement constituent comprises about 9.0% of the reactive reinforcement component. In another embodiment, the reinforcement constituent comprises about 9.5% of the reactive reinforcement component. In some embodiments, the reinforcement constituent comprises about 10.0% of the reactive reinforcement component. In some embodiments, the reinforcement constituent comprises about 10.5% of the reactive reinforcement component. In another embodiment, the reinforcement constituent comprises about 11.0% of the reactive reinforcement component. In another embodiment, the reinforcement constituent comprises about 12.0% of the reactive reinforcement component. In another embodiment, the reinforcement constituent comprises about 13.0% of the reactive reinforcement component.
[00139] In another embodiment, the reactive constituent comprises between about 30.0 and about 60.0% of the reactive reinforcement component, for example, about 30.5%, about 31.0%, about 32 , 0%, about 33.0%, about 34%, about 35.0%, about 36.0%, about 37.0%, about 38.0%, about 39.0% , about 40.0%, about 41.0%, about 42.0%, about 43.0%, about 44.0%, about
45.0%, about 46.0%, about 47.0%, about 48.0%, about
49.0%, about 50.0%, about 51.0%, about 52.0%, about
53.0%, about 54.0%, about 55.0%, about 56.0%, about
57.0%, about 58.0% or about 59.0%.
39/160 [00140] In some embodiments, the reactive reinforcement component has a viscosity between about 5,000 and 1,000,000 cSt or cP at 25 ° C. In some embodiments, the reactive reinforcement component has a viscosity between about 10,000 and 10,000,000 cSt or cP at 25 ° C., For example, about 10,000,000, about 9,000,000, about 8,000,000, about 7,000,000, about 6,000,000, about 5,000,000, about 4,000,000, about 3,000,000 or about 2,000,000, about 1,000,000, about 900,000, about 800,000, about 700,000, about 600,000, about 500,000, about 400,000, about 300,000, about 200,000, about 100,000, about 90,000, about 80,000, about 70,000, about 60,000, about 50,000, about 40,000, about 30,000, about 20,000, about 10,000 cSt. In one embodiment, the reactive reinforcement component has a viscosity of about 1,000,000 cSt.
[00141] In some embodiments, the reactive reinforcement component has a vinyl to functional hydride ratio (for example, -CH = CH ₂ of one or more organopolysiloxanes to Si-H of the hydride functionalized polysiloxane) between about 1:10 and about 1: 100, for example, between about 1:15 and about 1:90, between about 1:20 and about 1:80, between about 1:25 and about 1:70, between about 1:30 and about 1:60, between about 1:35 and about 1:50. In one embodiment, the reactive reinforcement component has a vinyl to hydride ratio of about 1:40. In another embodiment, the reactive reinforcement component has a vinyl to hydride ratio of about 1:20. In some embodiments, the reactive reinforcement component has a vinyl to hydride ratio of about 1:15. [00142] The cross-linking component language includes a component that, when applied to the reactive reinforcement component, catalyzes the in situ formation of the body corrective film.
[00143] The term catalyzes the in situ formation of the corrective film cor40 / 160 poral includes causing a reaction to occur between the reactive constituents of the reactive reinforcement component, so that a corrective body film is formed on the skin. Without wishing to be bound by theory, the crosslinking component induces a reaction between the one or more organopolysiloxanes and the hydride functionalized polysiloxane of the reactive reinforcement component causing the condensation of these constituents, so that a film is formed on the skin.
[00144] In some embodiments, the crosslinking component comprises a metal catalyst, for example, a platinum catalyst, a rhodium catalyst or a tin catalyst. Examples of platinum catalysts include, for example, platinum carbonyl cyclovinylmethylsiloxane complex, platinum divinyl tetramethyldisiloxane complex, platinum cyclovinylmethylsiloxane complexes, octanaldehyde / octanol platinum complexes and combinations thereof. An example of a rhodium catalyst includes Tris (dibutyl sulfide) Rhodium trichloride. Examples of tin catalysts include tin octoate II, tin neodecanoate II, dibutyltin diisooctylmaleate, Di-n-butylbis (2,4 pentanedionate) tin, di-n-butylbutoxychlorotin, dibutyltin dilaurate, dimethyltin dineodecanate (dimethyltin) and dimethyl tin tin oleate II.
[00145] In some embodiments, the crosslinking component further comprises a finished vinyl organopolysiloxane (for example, a compound of formula I, II IIa, IIb or IIc). In some embodiments, the amount of vinyl-terminated polysiloxane is a stabilizing amount of vinyl-terminated polysiloxane. The stabilizing quantity language includes an amount that prevents degradation of the catalyst and / or the cross-linking component and / or the body corrective film. In some embodiments, the stabilizing amount of vinyl-terminated polysiloxane is less than about 50%, less than about 40%, less than about 30%, less than
41/160 than about 20%, less than about 10%, less than about 5% or less than about 2%. In some embodiments, the stabilizing amount of the vinyl-terminated polysiloxane is about 1%.
[00146] In some embodiments, the crosslinking component has a viscosity between about 1,000 and about 50,000 cSt or cP at 25 ° C.
[00147] In some embodiments, the catalyst is added as a solution and the solution comprises between about 1.0 and about 5.0% of the cross-linking component, for example, about 1.5%, about 2, 0%, about 2.5%, about 3.0%, about 3.5%, about 4.0% or about 4.5%. In one embodiment, the catalyst is about 2.0% of the cross-linking component.
[00148] In some embodiments, the catalyst comprises between about 0.005 and about 0.04% of the cross-linking component, for example, about 0.005%, about 0.010%, about 0.015%, about 0.020%, about 0.025%, about 0.030% or about 0.035% or about 0.040%. In one embodiment, the catalyst is about 0.02% of the cross-linking component.
[00149] In some embodiments, the catalyst is present in the cross-linking component in an amount between about 100 ppm and about 500 ppm.
[00150] In some modalities, the reactive reinforcement component and the cross-linking component are prevented from coming into contact before use. The reactive reinforcement component and the crosslinking component can be kept from contacting before use by usual means known to a person skilled in the art. In one embodiment, the corrective skin formulation is a two-part formulation in which the reactive reinforcement component and said cross-linking component are packaged in separate containers and mixed before
42/160 of use. In another embodiment, the reactive reinforcement component is applied to the skin first, and the cross-linking component is applied to the surface of the reactive reinforcement component. In yet another embodiment, the crosslinking component is applied to the skin first and the reactive reinforcement component is applied to the surface of the crosslinking component. In another embodiment, the reactive reinforcement component and the crosslinking component are packaged together in the same container with a barrier between the two components, and are mixed when the components are extracted from the container.
[00151] The term body includes any part of the subject's body that can benefit from the formulations disclosed here. Examples of the subject's body include the skin, neck, forehead, jowls, eyes, hands, feet, face, cheeks, breasts, abdomen, buttocks, thighs, back, legs , ankles, cellulite, fat deposits, and the like.
[00152] The term skin includes the subject's skin epidermis, which is the outer layer of the skin and includes the stratified squamous epithelium composed of proliferating basal keratinocytes and differentiated suprabasals.
[00153] The term subject includes subjects in which the formulations disclosed here could be appropriate for use. In one example, the subject is a mammal, for example, a human. In another modality, the subject suffers from skin imperfections, body imperfections, or has recently undergone a cosmetic procedure. In another modality, the subject wants to look younger or wants to improve his body.
[00154] In one embodiment, the corrective body formulation further comprises one or more of sensation modifiers, adhesion modifiers, spreadability enhancers, diluents, adhesion modifiers, optical modifiers, particles, volatile siloxanes,
43/160 emulsifiers, emollients, surfactants, thickeners, solvents, film-forming agents, humectants, preservatives, pigments, cosmetic agents or therapeutic agents. In other embodiments, the reactive reinforcement component and / or the crosslinking component further comprises one or more of sensation modifiers, adhesion modifiers, spreadability enhancers, diluents, adhesion modifiers, optical modifiers, particles, volatile siloxanes, emulsifiers, emollients, surfactants, thickeners, solvents, film-forming agents, humectants, preservatives, pigments, cosmetic agents or therapeutic agents. A person skilled in the art could readily determine appropriate additives based on the INCI dictionary, which is incorporated herein by reference in its entirety. [00155] Examples of cosmetic or therapeutic agents include sunscreens (for example, UV protective agents) anti-aging agents, anti-acne agents, anti-wrinkle agents, stain reducers, emollients, antioxidants, vitamins.
[00156] In some embodiments, the emulsifier is SIMULGEL ^TM 400.
[00157] In some embodiments, the composition or film is administered first followed by administration of one or more cosmetic or therapeutic agents. In some embodiments, the composition or film is administered after one or more cosmetic or therapeutic agents. In some embodiments, the film and the one or more cosmetic or therapeutic agents are administered at substantially the same time. In some embodiments, the composition or film is used to release one or more cosmetic or therapeutic agents. [00158] In some modalities, a finishing formulation can be applied to a corrective body formulation during or after the formation of the film in the body. The term finishing formulation includes a composition comprising components that provide a desired tactile sensation or a desired aesthetic appearance to the film after formation. For example, the finishing formulation can provide a silky, smooth and / or soft tactile sensation or a refreshing, fresh, matte, glossy, or luminescent aesthetic appearance after application to the film.
[00159] In some embodiments, the finishing formulation comprises one or more of oils, esters or ethers, for example, triglycerides, PPG-3 benzyl ether myristate, Schercemol DISD ester, or particles, for example, nylon, silica and beads of silicone elastomer. In some embodiments, the one or more of these components comprises from about 0.5% to about 100% of the finishing formulation.
[00160] In some modalities, the finishing formulation is a creamy spray, foam, ointment, serum, gel or powder.
[00161] In some modalities, the finishing formulation still comprises one or more of sensation modifiers, adhesion modifiers, spreadability improvers, diluents, adhesion modifiers, optical modifiers, particles, volatile siloxanes, emulsifiers, emollients, surfactants, thickeners , solvents, film-forming, humectants, preservatives, pigments, dyes (for example, fluorescent dyes), cosmetic agents or therapeutic agents.
[00162] In some embodiments, the films and formulations described here comprise one or more pigments. This includes natural and unnatural coloring agents or dyes. In one embodiment, the pigments are fluorescent dyes.
[00163] In some embodiments, the films and formulations further comprise a pigment dispersion formulation. The pigment dispersion formulation language includes formulations that are capable of delivering one or more pigments to films or formulas as a separate component of the formulation or film. In some embodiments, the pigment dispersion formulation allows for uniform distribution of the pigment in the films and formulations. In some embodiments, the pigment dispersion formulation comprises at least one reactive constituent. In some embodiments, the pigment dispersion formulation comprises at least one reinforcing constituent. In some embodiments, the pigment dispersion formulation comprises one or more of sensation modifiers, adhesion modifiers, spreadability enhancers, diluents, adhesion modifiers, optical modifiers, particles, volatile siloxanes, emulsifiers, emollients, surfactants, thickeners, solvents , film-forming, humectants, preservatives, pigments, cosmetic agents or therapeutic agents. In other embodiments, the reactive reinforcement component and / or the crosslinking component further comprises one or more of sensation modifiers, adhesion modifiers, spreadability enhancers, diluents, adhesion modifiers, optical modifiers, particles, volatile siloxanes, emulsifiers, emollients, surfactants, thickeners, solvents, film-forming agents, humectants, preservatives, pigments, cosmetic agents or therapeutic agents.
[00164] In some embodiments, the pigment dispersion formulation is applied before or after application of the reactive reinforcement component to the skin. In some embodiments, the pigment dispersion formulation is applied before or after applying the crosslinking component to the skin. In some embodiments, the pigment dispersion formulation is applied between the application of the reactive reinforcement component and the cross-linking component to the skin.
[00165] In some embodiments, the pigment dispersion formulation can be applied to skin that has not been subjected to the application of corrective body formulation or film. For example, a subject can apply a pigment dispersion formulation to the skin in the area around the body correction film or formulation, or the subject can apply the pigment formulation to the skin instead of applying the body correction film or formulation. .
[00166] The terms apply, applied and application include methods for administering the formulations disclosed here to a subject's body, such as application by fingers, brush, cotton ball, pad, spray, sponge, cotton swab, roll-on and the like . One skilled in the art can readily determine appropriate methods for applying the formulations disclosed here.
[00167] In some embodiments, the invention belongs, at least in part, to a kit comprising the corrective body formulation comprising a reactive reinforcement component and a cross-linking component. In some embodiments, the p kit is a multi-compartment kit comprising at least two compartments in which one compartment comprises the reactive reinforcement component and the second compartment comprises the cross-linking component. In some embodiments, the kit also includes instructions for using the kit, one or more brushes, one or more cotton swabs, a cleaner to remove the film or a mirror. In some embodiments, the kit also comprises one or more finishing formulations.
[00168] In some embodiments, the invention belongs, at least in part, to a body corrective film prepared by a process that comprises the steps of applying a reactive reinforcement component to the body; and applying a crosslinking component to the reactive reinforcement component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component.
[00169] In some embodiments, the invention belongs, at least in part, to a body correction film prepared by a process that comprises the steps of applying a crosslinking component
47/160 to the body; and applying a reactive reinforcement component to the crosslinking component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component.
[00170] The language corrective body film includes films that are formed in the reaction of the reactive reinforcement component and the cross-linking component and that, in formation, improves one or more body imperfections. In some modalities, the body corrective film is a skin corrective film (for example, a film that improves one or more skin imperfections).
[00171] In some modalities, the body corrective film has a natural skin appearance when applied to the skin. The natural skin appearance language includes the perception that the body corrective film, when applied to the skin, has the look, feel and texture of real skin and that the treated film has the physical properties (for example, elasticity and stiffness) of real skin (for example, live). A trained observer and / or technician might be able to determine whether the film on application to the body looks like natural skin. For example, a trained observer might be able to determine if the film, when applied to the body, appears excessively shiny, as described in example 3, or if the film appears not to move with the underlying musculature of the skin by, for example, breaking , deform or flicker, in response to the skin's natural movement.
[00172] A technician might be able to determine if the film looks like natural skin when applied to the body. For example, skin elasticity and stiffness, with or without the body corrective film applied to it, can be assessed by a variety of methods (Agache et al., Arch. Dermatol. Rev., 269 (1980) 221, the teachings of which are incorporated by reference). For example, the DermaLab suction cup instrument provides a common method for assessing the mechanical properties of the skin, and previously 48/160 showed younger skin to be less rigid and more elastic than skin of age (Grahame et al. Clinicai Science 39 (1970) 223-238, the teachings of which are hereby incorporated by reference). With this method, the skin's stiffness is indicated by the Young's Module, a medicine calculated by the instrument based on the pressure required on the skin over a predetermined distance.
[00173] In some modalities, the Young Module of the skin treated with the corrective body formulation is reduced by between about 5% to about 70%, for example, between about 30% and about 60%, or between about 40% and about 50% compared to untreated skin. In some modalities, the Young's Module of the skin treated with the corrective body formulation is reduced by between about 5% and about 25% compared to untreated skin.
[00174] Skin elasticity is determined by the skin's retraction time. The retraction time is obtained by measuring the time it takes for the skin to fall a predetermined distance in the direction of its natural position, after the suction pressure is removed. In some modalities, the retraction time of the skin treated with the corrective body formulation is reduced by between about 5% and about 75%, for example, between about 30% and about 60%, or about 50% and about 65% when compared to untreated skin. In some modalities, the retraction time of the skin treated with the corrective body formulation is reduced by between about 5% and about 10% compared to untreated skin. In some embodiments, the shrinkage time of the skin treated with the film is close to the shrinkage time of the film alone.
[00175] The biceps and hand skin were evaluated before and after corrective body treatment was applied, as shown in Figures 1 and 2. The DermaLab results confirmed that the skin was more rigid (Figure 1) and more elastic (Figure 2 ) after application of the product.
49/160
The observed reduction in stiffness and the increase in skin elasticity are consistent with the skin being younger.
[00176] In some modalities, the body corrective film, when applied to the skin, has the appearance and physical properties of natural young skin, not defective. Young skin language includes skin that has little or no damage, as measured by the Griffith score. The Griffith score (GS), as shown below, is a quantitative measure of the amount of skin damage the subject has.
[00177] 0-1: No damage [00178] 2-3: Slight damage [00179] 4-5: Moderate damage [00180] 6-7: Moderate to severe damage [00181] 8-9: Serious damage [00182] In some modalities, young skin includes skin that has the
Griffith score between about 0 and about 3.
[00183] In some modalities, the subject has a negative change in the Griffith score (AGS) of about 1, about 2, about 3, about 4, about 5, about 6, about 7 or about 8 after applying a corrective body formulation. In some modalities, the subject has an AGS between about -0.5 and about -3.0 when applying corrective body formulation. In one modality, the subject has an AGS between about -1 and about -1.5, between about -1.2 and about -1.3 (for example, about -1.25) when applying the corrective body formulation. In another embodiment, the subject has an AGS between about -2.0 and about -3.0, for example, between about -2.0 and about -2.5, or between about -2.1 and about -2.2 (for example, about -2.15) in applying the corrective body formulation.
[00184] A person skilled in the art might be able to determine whether the film, when applied to the body, looks like young, natural skin, not defective by the methods revealed in example 6.
50/160 [00185] In other modalities, the film, when applied to the skin, provides rigidity and elasticity so that the skin treated with the film looks substantially more similar to young skin than untreated skin. The term elasticity includes the tendency of the skin to return to its original shape once it has been deformed. The elasticity language substantially similar to young skin includes the skin's ability to return to its original shape once it has been deformed in a manner similar to that of a young skin. The term stiffness includes the skin's resistance to deformation. The stiffness language substantially similar to youthful skin includes the skin's ability to resist deformation in a manner similar to that of youthful skin. A technician could also be able to determine whether the film, when applied to the body, has the aforementioned physical properties of youth, without stain, natural by the techniques described above (for example, using the Dermalab suction cup instrument). [00186] In some modalities, the subject and / or subject observers perceive a reduction in age in the application of the body correction formulation. In some modalities, the perceived age reduction is about 1 year, about 2 years, about 3 years, about 4 years, about 5 years, about 6 years, about 7 years, about 8 years, about 9 years, about 10 years, about 11 years, about 12 years, about 13 years, about 14 years or about 15 years less than the real age of the subject. In some modalities, the perceived age reduction is about 7.5 years less than the subject's real age when applying corrective body formulation. In other modalities, the perceived age reduction is about 8.5 years less than the subject's real age when applying corrective body formulation.
[00187] The language the film is formed in and film formation includes the results of the polymerization reaction that occurs in the interaction of the
51/160 reactive reinforcement component and the crosslinking component. Without wishing to be bound by theory, film formation is characterized by a phase transition from the viscous sol state of a mixture to that state of continuous interconnected polymer film.
[00188] A technician could determine when the film is formed on the body using routine methods. For example, rheological measurements using small amplitude oscillatory shear can determine the continuous evolution of viscoelastic properties, such as elastic modulus (G '), viscous modulus (G) and loss of tangent (tan δ) of the reaction mixture continuously through the film formation process. In some embodiments, the rheometer can be used to determine the crossing over time between G 'and G and the time when tan δ becomes an independent frequency, which is a measure of film formation. In some embodiments, the film is formed within at least about five minutes, for example, within about a minute, about two minutes, about three minutes or about four minutes. In some embodiments, the film is formed within at least about 10 seconds and about 3 minutes.
[00189] In some modalities, the skin or body corrective film has a Young's Modulus (for example, tensile strength) between about 0.01 and about 1 MPa, as illustrated in example 1.
[00190] In some embodiments, the fracture deformation of the skin or body corrective film has a fracture deformation of at least about 150%, as measured by Example 1.
[00191] In some modalities, the skin or body corrective film has a strength of adhesion to the leather of more than about 20 N / mm, for example, more than about 25 N / mm, more than about 30
N / mm, more than about 35 N / mm, more than about 40
N / mm, more than about 45 N / mm, more than about 50
N / mm, more than about 55 N / mm, more than about 60
52/160
N / mm, more than about 65 N / mm, more than about 70 N / mm, more than about 75 N / mm, or more than about 80 N / mm, as determined by the adhesion to the leather illustrated in example 2. In one embodiment, the adhesion strength to the leather is between about 50 and about 80 N / mm, as determined by the leather adhesion test illustrated in example 2.
[00192] In some embodiments, the skin or body corrective film has a hysteresis of less than about 10% for example, less than about 9%, less than about 8%, less than about 7% less than about 6%, less than about 5%, less than about 4%, less than about 3%, less than about 2%, less than 1% or about 0 %.
[00193] In some embodiments, the skin or body corrective film is between about 10 pm and about 1500 pm thick, for example, between about 50 pm and about 500 pm thick. In some embodiments, the film is less than about 100 pm thick. The thickness of the film can be measured by methods known to a person skilled in the art, for example, by combining calipers and a calibrated microscope. The thickness of the film can also be digitally measured using a micrograph of the film's cross section. The calibration of the microscope allows the conversion of pixel distance measured in units of metric distance.
[00194] In some modalities, the skin or body corrective film shrinks by less than between about 1 and 30%, for example, between about 1 to about 15%. The amount of shrinkage can be determined by methods known to a person skilled in the art, for example, by the Croll method (Croll, S.G. J. Coatings Tech. 52 (1980) 35, the teachings of which are incorporated herein by reference). In this method the film is used to coat one side of a thin flexible substrate. The amount of curve developed in the substrate due to
53/160 to the shrinkage of the coating is used to calculate the magnitude of shrinkage of the coating (Francis et al., J Mater Sci 2002; 37: 4717-31, the teachings of which are incorporated here by reference.) [00195] In some modalities, body corrective films are physiologically stable. Physiologically stable language includes the durability of the film when exposed to normal skin conditions, for example, moisture, tears, sweat or sebum. Physiological stability can be determined by methods typically used by a person skilled in the art, such as an absorption test, which measures the change in weight of the film after exposure to a physiological factor. For example, the absorption test can employ a simulated sweat formulation (eg 1X phosphate buffered saline) or simulated tallow (eg 25% wax monoesters, 41% triglycerides, 16% free fatty acids and 12% squalene ). In some embodiments, the weight of the film increases by less than about 10%, for example, less than about 9%, less than about 8%, less than about 7%, less than about 6%, less than about 5%, less than 4%, less than 3%, less than 2%, less than 1% or has no increased exposure to moisture, tears, sweat or tallow.
[00196] In some embodiments, the invention belongs, at least in part, to methods for correcting body imperfections in a subject comprising applying to the subject a formulation comprising a) a first reactive reinforcement component; and a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thereby correcting body imperfections. The language to correct body imperfections includes improving (for example, partially or completely) one or more body imperfections54 / 160 raises, permanently or temporarily (for example, for the duration that the film is left on the skin). A person skilled in the art might be able to determine whether body imperfections are corrected, partially or completely, in applying the corrective body formulation to the body by the techniques described in example 6.
[00197] In some modalities, the language correcting body imperfections includes reducing the appearance of body imperfections in a subject comprising applying to the subject a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thereby reducing the appearance of skin or body imperfections. The language to reduce the appearance of body imperfections includes the reduction of one or more external aspects of one or more body imperfections. In some modalities, the appearance of body imperfections in the application of corrective body formulation to the subject are reduced by about 100%, by about 95%, by about 90%, by about 85%, by about 80%, in about 75%, about 70%, about 65%, about 60%, about 55%, about 50%, about 50%, about 45%, about 40%, about 35%, about 30%, about 25%, about 20%, about 10% or about 5% compared to the untreated subject.
[00198] In some modalities, the language to correct body imperfections includes masking body imperfections in a subject comprising applying to that subject a formulation comprising
a) a first reactive reinforcement component; and b) a second cross-linking component; wherein said crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thus masking the appearance of
55/160 body imperfections. The language of masking body imperfections includes hiding or obscuring, partially or completely, one or more body imperfections. In some modalities, the method provides to mask body imperfections in a subject after a cosmetic procedure, comprising applying to the skin where the cosmetic procedure was carried out a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein said crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thereby masking the appearance of body imperfections. Examples of cosmetic procedures include, for example, cosmetic surgery (for example, eye lift, face lift, tummy tuck and the like) or Botox® injections. In some modalities, skin imperfections are masked. In some modalities, body imperfections after applying body correction formulation are masked in about 5%, in about 10%, in about 15%, in about 20%, in about 25%, in about 30 %, about 35%, about 40%, about 45%, about 50%, about 55%, about 60%, about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about 90%, about 95%, or about 100% compared to untreated body imperfections.
[00199] In some modalities, the language to correct body imperfections includes improving the appearance of a subject's body, comprising applying to said subject a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein said crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thereby improving the appearance of the body. Language improves the appearance of a subject's body in56 / 160 and improves the external aspects of the body. Examples of improved body appearance include reducing or masking the appearance of port wine stain or nevus flammeus (eg nevus flammeus nuchae or nevus flammeus midline) melasma, wrinkles, scars, warts, acne, skin disfigurements, birthmarks, burn wounds, blemishes or pores, nocturnal skin tone, reduce or mask brightness, elevated sagging skin, or reduce or mask the appearance of cellulite or stretch marks. In some embodiments, the appearance of the subject's skin is improved.
[00200] In some modalities, the language to correct body imperfections includes improving the body of a subject, comprising applying to the body of a subject a formulation comprising a) a first reactive reinforcement compound; and b) a second crosslinking component, wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin, thereby improving the subject's body. The language improving the body includes increasing or elevating the characteristics of a subject's body so that the subject's appearance is more attractive. For example, a subject's body can be improved by adding dyes, gliter and the like. In some embodiments, the appearance of the subject's skin is improved.
[00201] In some embodiments, the invention pertains, at least in part, to methods for reducing the subject's age appearance comprising applying to the subject a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby reducing a subject's age appearance. The language reducing the appearance of a subject agent includes the perception by the subject or those who visualize the subject of
57/160 that the subject is younger when applying the body corrective film to the subject. In some modalities, the subject seems about 1 year, about 2 years, about 3 years, about 4 years, about 5 years, about 6 years, about 7 years, about 8 years, about 9 years, about 10 years, about 11 years, about 12 years, about 13 years, about 14 years, about 15 years, about 16 years, about 17 years, about 18 years, about 19 years or about 20 years younger when applying body corrective film.
[00202] In some embodiments, the invention pertains, at least in part, to methods of protecting a subject's body comprising applying to the subject a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby protecting the body. The language protecting a subject's body includes preserving or shielding a subject's skin or body from elements of environmental damage, for example, damage by the sun, wind, rain or environmental toxins. In some modalities, the subject's skin is protected.
[00203] In some embodiments, the invention belongs, at least in part, to methods for shaping a subject's body, comprising applying to the subject a formulation comprising: a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thus shaping the body. The language modeling the subject's body includes altering a subject's body, for example, providing support for soft body tissues and preventing sagging soft body tissues. Examples of soft body tissues include the abdomen, buttocks, thighs, neck, forehead, jowls, breasts, skin under
58/160 the arms, and the skin around the eyes. In some modalities, the subject's skin is modeled.
[00204] In some modalities, language modeling a subject's body includes structurally altering, for example, redistribution of a part of the subject's body, comprising applying to the subject a formulation comprising a) a first reactive reinforcement component; and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thus shaping the body. In some embodiments, a part of the subject's body is elevated, for example, the breasts, the skin, the buttocks, and the like. The language raising the subject's body includes raising the subject's body, for example, in a similar way to a surgical cosmetic procedure (for example, face elevation, eye elevation, sinus elevation and the like). In some modalities, the subject's skin is raised. In some embodiments, the skin is the facial skin (for example, the skin around the eyes, the skin on the forehead or the skin around the lips) or skin on the neck. In some modalities, when applying corrective body formulation, the body is elevated by about 5%, about 10%, about 15%, about 20%, about 25%, about 30%, about 35% , about 40% or about 50% compared to the body of the untreated subject. In some embodiments, the body is raised by about 1 mm, about 2 mm, about 3 mm, about 4 mm, about 5 mm, about 6 mm, about 7 mm, about 8 mm, about 9 mm, about 1 cm, about 1.5 cm, about
2.0 cm, about 2.5 cm, about 3.0 cm, about 3.5 cm, about
4.0 cm, about 4.5 cm, about 5.0 cm, about 5.5 cm, about
6.0 cm, about 6.5 cm, about 7.0 cm, about 7.5 cm, about
8.0 cm, about 8.5 cm, about 9.0 cm, about 9.5 cm or about 10 cm when applying the body correction film.
In some embodiments, the invention pertains, at least in part, to a method for releasing an agent to a subject, comprising applying to the subject's skin a formulation comprising a) a first reactive reinforcement component optionally comprising a or more agents; and b) a second cross-linking component optionally comprising one or more agents; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby releasing the agent to the subject. The language of releasing an agent includes releasing an agent (for example, a cosmetic agent or therapeutic agent) to the subject's skin in the formation of the film on the subject's skin. In some embodiments, the agent is released in one portion or the agent is formulated to be released in a release mode over time. Examples of agents include cosmetic agents and therapeutic agents.
[00206] In some embodiments, the invention belongs, at least in part, to a corrective body formulation for application to the subject's body, comprising at least one pre-selected function modulation component, in which said composition forms a body corrective film in application to the subject's body.
[00207] The pre-selected term includes components that are chosen before preparing the formulation. For example, components can be chosen during the manufacturing process to create a specific formulation. Alternatively, the components can be chosen by the subject before applying the formulation. [00208] The modeling function component language includes components that allow corrective body formulations to be selectively stiffened for a particular use of the film (for example, reducing the appearance of wrinkles, minimizing glare, masking pores, etc.). The modulation function component or components
60/160 can be selected based on the physical properties of the film that are needed to be effectively applied for a particular use of the film. For example, if the formulation will be used to minimize glare, the modules must be low in relation to the values of other physical properties of the resulting film.
[00209] In some embodiments, the invention belongs, at least in part, to a corrective body formulation that targets a treatment area in a subject's body, comprising at least one specific pre-selected treatment component, in which said composition forms a body corrective film on application to the target treatment area on the subject's body.
[00210] The target treatment area language includes an area of the body where the formulation is intended to be applied.
[00211] The specific treatment component language includes components that allow corrective body formulations to be selectively stiffened for a targeted treatment area on the body (for example, under the eyes, forehead, lips, buttocks, neck, etc ...). The specific treatment component or components can be selected based on the physical properties of the film that results from formulations that are necessary to be effectively applied to a target treatment area, as shown in Table 1. For example, if the treatment area target treatment is under the eyes, the modulus must be low in relation to the values of the other physical properties of the resulting film.
Table 1
Target treatment area Mo-idle Elasti-City Stretchedment Accession Matte finish Tex-ture Under the eyes Low High Medium High High High Forehead High High Medium High High High Lips Medium High High High Low Low
[00212] Examples of modulation function components and
61/160 specific treatment components include a stiffness component, an elasticity component, an elongation component, an adhesive component, a matte component and a texture component.
[00213] The stiffness component language includes components that modulate the flexibility of the resulting film, which is determined by measuring the Young's Module of the film (see Example 2). Examples of stiffness components include the reactive constituent (e.g., organopolysiloxane and / or hydride functionalized polysiloxane) and the reinforcing constituent.
[00214] The elasticity component language includes components that modulate the indentation of the resulting film, which is determined by measuring hysteresis, and includes, for example, the reinforcing constituent.
[00215] The component stretching language includes components that modulate the stretching of the resulting film, which is determined by measuring the percentage elongation to produce. Examples of elongation components include the reactive constituent (e.g., organopolysiloxane and / or hydride functionalized polysiloxane) and the reinforcing constituent.
[00216] The component adhesion language includes components that modulate the adhesion of the resulting film to the skin, as measured by the leather adhesion test (see Example 2). Examples of adhesion components include the reactive constituent (e.g., organopolysiloxane and / or hydride functionalized polysiloxane) and the reinforcing constituent.
[00217] The matte component language includes components that modulate the gloss of the resulting film, as measured by determining the gloss of the resulting film (see Example 3). Examples of matte components include the reinforcing constituent and light scattering particles.
[00218] The texture component language includes components
62/160 that modulate the texture of the film so that the resulting film has the appearance and feel of natural skin, and is measured by determining the friction of the film. A person skilled in the art can readily determine methods for measuring the friction of the film, for example, by pressing and dragging a cantilever across the surface and recording the resistance force. The greater friction corresponds to the greater force registered and more wrinkled surfaces tend to have greater friction.
[00219] In some embodiments, the invention belongs, at least in part, to a cleaner that removes the film for use in removing a corrective body film, in which said film is prepared by a process comprising the steps of a) applying a reactive reinforcement component to the skin; and b) applying a crosslinking component to said reactive reinforcement component, wherein said crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component. [00220] In other embodiments, the invention belongs, at least in part, to a cleaner that removes the film comprising a wetting component of the film, a penetrating component, an intumescent film component and a film releasing component.
[00221] The film removal cleaner language includes a cosmetic formulation that, when applied to a body correction film, breaks the film components so that the film can be removed from the body. In some embodiments, the film cleaner removes the film by wetting the film, penetrating the film, swelling the film and releasing the film from the skin.
[00222] The film wetting component language includes those components of the cleaner that allow the film to absorb liquid. In some embodiments, the film wetting component comprises a caprylyl methicone, ethyl trisiloxane or a combination thereof.
63/160 [00223] The penetration component language includes those components of the cleaner that allow the cleaner to permeate the film. Examples of penetrating components include siloxane, caprylyl methicone, ethyl trisiloxane emulsifiers or a combination thereof.
[00224] The intumescent film component language includes components of the cleaner that cause the film to expand. Examples of swollen components of the film include caprylyl methicone, ethyl trisiloxane, isododecane or a combination thereof. [00225] The film release component language includes components of the cleaner that prevent the film from adhering to the skin or body of the subject to which the film is applied. Examples of film release components include glycols, water or a combination thereof.
[00226] In some embodiments, the cleaner breaks the mechanical integrity of the film. Language disrupts the mechanical integrity of the film includes disturbing the mechanical characteristics that provide the film with its unique properties (for example, stiffness, elasticity, elongation, adhesion and the like).
[00227] In some embodiments, the cleaner comprises a siloxane phase, an emulsifying phase and an aqueous phase. The siloxane phase language includes a cleaner component that comprises one or more siloxanes, for example, caprylyl methicone and ethyl trisiloxane. In some embodiments, the siloxane phase still includes isododecane and Airgel VM2270 (Dow Corning). The emulsifying phase language includes a cleaner component that comprises one or more emulsifiers, for example, siloxane emulsifiers like PEG-9 polydiethylsiloxyethyl dimethicone, PEG-35 Castor oil, or isododecane and cross-polymer lauryl dimethicone / polyglycerin 3. The aqueous phase language includes a cleaner component that is soluble in water,
64/160 eg water, propylene glycol, butylenes diglycol, glycerol or combinations thereof. In some embodiments, the aqueous phase includes MPdiol glycol, preservatives (eg, neolone PE), optical particles (eg, silica and DMPA / isophthalic acid / SMDI copolymer & Green 5) and structural particles (eg, nylon-12) .
[00228] In some embodiments, the siloxane phase is about 50% of the cleaner, the emulsifying phase is about 8% of the cleaner and the aqueous phase is about 42% of the cleaner.
[00229] In some embodiments, the invention belongs, at least in part, to a method of cleaning a body surface containing a corrective body film, comprising applying an effective amount of a film that dissolves the cleaner to the film, so that said film dissolves. In some modalities, the body surface is the skin.
[00230] In some embodiments, the invention belongs, at least in part, to a formulation for repairing a corrective body skin applied to the skin in which the formulation comprises a) a first reactive reinforcement component and b) a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin.
[00231] The terms repair and repair include improving imperfections in the body corrective film after the film forms on the skin. In some embodiments, the term repair includes repairing or mending cuts, gaps or breaks in the film. In some embodiments, the term repair includes replacing a part of the film that may have been removed from the skin. In some embodiments, the term repair includes re-joining or assembling the part of the film that may have become loose on the skin (for example, delaminated skin). In some embodiments, the term repair includes swelling of the edges of the tear, gap or break in the
65/160 film to make the film more malleable, so that the film may be able to be remodeled.
[00232] In some embodiments, the invention belongs, at least in part, to a method for repairing a body corrective film applied to the skin by a) identifying an area of the film in need of repair; b) optionally smoothing the edges of the film; and c) applying a formulation to repair the film, wherein the formulation comprises a first reactive reinforcement component and a second cross-linking component; wherein the crosslinking component catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin, thereby repairing the body corrective film.
[00233] The language to smooth the edges of the film includes removing, brushing, swelling, brushing or polishing the edges of the film in the area in need of repair to remove notched or uneven parts of the film.
[00234] In some embodiments, the invention belongs to a kit comprising a first reactive reinforcement component, and a second cross-linking component, wherein the cross-linking component catalyzes an in situ cross-linking of the reactive reinforcement component so that a film is formed on the skin. In some embodiments, the invention belongs, at least in part, to a kit for repairing a body corrective film in which the kit comprises a formulation comprising a) a first reactive reinforcement component and b) a second cross-linking component in which the crosslinking catalyzes an in situ crosslinking of the reactive reinforcement component so that a film is formed on the skin.
[00235] In some embodiments, the kit is a multi-compartment kit comprising at least two compartments. In some modalities, the reactive reinforcement component is at a
66/160 compartment and the crosslinking component is in a second compartment. In some embodiments, the kit also includes one or more brushes, one or more cotton swabs, a film that removes the cleaner, instructions for use or a mirror. In some embodiments, the kit also comprises a pigment dispersion formulation.
Examples
Example I. Cyclic Traction Test and Extension [00236] Sample preparation: For the purpose of determining coarse mechanical properties, target materials were dropped into dumbbell-shaped molds. The dimensions of the mold neck were 20 mm long, 5 mm wide and 1.5 mm thick. The mold handles were 20 mm by 15 mm and provided an adequate area to ensure good safe adhesion during the test. The dimensions of the mold are in accordance with the guidelines ASTM D638.
[00237] Once the spilled samples were fully cured and dried, the formed samples were extracted from the individual molds, using a spatula and the geometry of the finished parts was measured with digital calipers to determine the exact dimensions.
[00238] Mechanical Tests: The mechanical characterization of species was performed in Instron 3342 (Instron, Norwood MA) equipped with a 100N load cell (Instron # 2519-103). Dumbbell samples were mounted on the instrument using modified Instron 2710-101 handles which ensured that the sample did not slip or fall into the handles during the test. Two types of tests were performed sequentially on each sample, first the cyclic test followed by the cyclic traction test. Note that the first test (for example, the cyclic test) had a negligible effect on the result of the second test (for example, the extension traction test). Each test was pre-programmed in Bluehill Lite Software used to operate the instrument. The analysis of the data and parameters associated with each of the two tests is described below.
[00239] Cyclic test: To determine the elasticity of materials, a cyclic test was designed. The cyclic test was used to determine the most elastic material (for example, spring type) and an instantaneous residual stress (IRS) was obtained from this test, as described below. Generally, the more elastic the material, the faster it returns to its original shape after deformation. For perfectly elastic materials, the IRS and cyclic area test approach zero, and therefore the lower the value, the better.
[00240] Before starting the test, a sample was mounted on the device in such a way that the rectangular handle portions of the specimen and none of the specimens were fixed inside the instrument handles. The distance from the instrument handle was stiffened so that the sample was in neutral extension, as indicated by the instrument strength being close to zero (± 0.01 N). Subsequently, the cyclic extension was performed at 1 mm / s for a maximum extension of 15% of the initial sample length. A total of 15 cycles are performed and recorded. The stress data recorded by the instrument was exported to Excel, where the reported mechanical properties were calculated.
[00241] An Excel model was used to automatically extract a number of parameters. Cyclic Young's Modulus as calculated as the slope of the straight line of the first cycle stress-strain curve between 1% to 4%. The R-squared value of the linear adjustment was above 0.99 or Young's modulus was discarded. The instantaneous residual voltage (IRS) was calculated for each cycle according to the difference in voltage between the loading and unloading curves68 / 160 to half the maximum voltage obtained during the first cycle. The IRS for the first cycle, as well as the average IRS for the fourth through 14 cycles were recorded. The area bounded by the loading and unloading curves of each cycle was also calculated. Good agreement was observed between IRS and the calculated cycle area. [00242] Most of the evaluated materials were elastic and sufficiently flexible so that the cyclic test can be repeated on the same sample, without a significant change in the calculated properties. This suggests this test does not result in long-term changes to the material tested.
[00243] Extension Tensile Test: The extension tensile test was used to determine the rigidity and elasticity of a material, measuring Young's Modulus and Final Tension. Young's modulus was used as a measure of the material's stiffness, while the final stress was used as a measure of the material's flexibility. In order to develop a film with a skin appearance, Young's Module must fall within a target range (for example, 0.1-1.0 MPa), while fracture deformation (as measured by the final stress) ) must be high enough (for example, more than about 150%) so that the film does not break when it is being deformed by a movement of the skin.
[00244] The sample was mounted on the apparatus in such a way that the rectangular handle portions of the specimen and none of the specimens were fixed inside the instrument handles. The distance from the instrument handle was stiffened so that the sample was in neutral extension, as indicated by the instrument strength being close to zero (± 0.01 N). Subsequently, the extension to rupture of the sample was performed at 10 mm / s. The stress data recorded by the instrument were exported to Excel, where the reported mechanical properties were calculated.
69/160 [00245] An Excel model was used to automatically extract a number of parameters from the data generated by the instrument. The Young's Modulus (YM) of extension as calculated as the slope of the straight line of the stress-strain curve between 6% to 11%. The R-squared value of the linear adjustment was above 0.99 or the Young's Modulus was calculated from a 5% more linear stress range on the tension traction curve. The shear modulus (G) was determined from the same stress range as YM. G was calculated as the slope of the best adjustment line between recorded voltage and α-α-2, where α is 1 plus the instantaneous voltage. The yield voltage was determined as the voltage at which the measured voltage differed by more than 10% from the Neo-Hookean voltage; the multiple of G e (α-α2). The final stress was calculated as the maximum stress recorded during the test. The mechanical properties calculations presented here are consistent with the ASTM D412 standard.
[00246] Example 2: T-Peel adherence test: To determine the adherence of the target materials, the materials were spread on a sheet of flexible soft leather 25.4 mm wide and 76.2 mm long. The leather used as a test substrate was lightweight upholstery leather (AD1100 Leather Unlimited, Belgium WI). Immediately after spreading the material over the first piece of leather, a second equivalent piece of leather was placed on top of a thin layer sandwich of material between the two pieces. The two pieces of leather were pressed together to leave a thin homogeneous layer of material at the interface between the two leather substrates. The edges were annihilated to remove the access materials and the material was allowed to cure and dry to form a test specimen.
[00247] The adhesion test sample was partially peeled off at one end by hand to separate enough of the two
70/160 leather substrates for effective clamping by Instron 3342 claws. Each leather substrate was attached to its own instrument and an extension adhesion test was performed at a speed of 10 mm / s to peel the two substrates from each other. The force data vs. Time was recorded by the instrument during the extension and exported to Excel where the reported adhesive strength was calculated. [00248] An Excel model was used to automatically extract the adhesive parameters from the data generated by the instrument. The average adhesive force of the sample was calculated by weighting the instantaneous force measured by the instrument during the experiment normalized by the sample width (25.4 mm). This test method was developed in accordance with the ASTM D1876 standard. The minimum acceptable adhesion, which depends on the stiffness of the material and the area on which the film is placed, was approximately more than 25 N / mm.
Example 3. Image Analysis Measures [00249] Brightness: To measure brightness, in vitro or in vivo, a clear box with a light source placed at a relative angle of 45 ° to the location being measured was used to create brightness, and a camera, positioned so that the angle formed by a line drawn from the lenses to the area being measured is 45 °, was used to photograph the place. The camera's white balance, F-stop and ISO were manually set to adjusted values to give adequate exposure and color temperature. A photo was taken without any diffusion element between the light source and the location to capture the glow. Then, a diffusion surface was placed between the light source and location and another photograph was taken (changing the shutter speed so that the exposure is similar or equal to the first photograph). This photograph captured on the surface, without the presence of any glare while the first photograph captured the maximum amount of glare
71/160 as a result of specular reflectance. These photographs were overlaid and cut to the relevant sample area, then the diffused photograph was subtracted from the maximum brightness photograph to create a photograph with only the brightness highlights present. The entire photograph subtracted was then summarized by finding the average gray value, along with the standard deviation. This average gray value was indicated as the brightness value and was used to compare the present amount of specular reflectance for each sample. For each sample, the chamber settings for each situation (with and without the diffuser) were identical.
[00250] Adjustment of photo capture: To ensure maximum repeatability in the placement of panels for each photograph taken to evaluate the product's performance, a head positioning system (HPS) was created. This HPS had two configurations: assessments only of the forehead and assessment of the entire face. In both configurations, an 819 series model of fixed chinrest table from Applied Science Laboratories (ASL) was used as a base to mount the two different configurations to a table. Two cameras were used to capture the subject from two different angles. The first camera (normal shooting) was positioned with the face so that the lens line through the camera was positioned in relation to the plane of the subject's face at an angle of approximately 90 °. The second camera (45 ° shot) was positioned to the left of the subject so that the lens line through the camera was positioned in relation to the plane of the subject's face at an angle of approximately 45 ° capturing mainly the left side of the face of the subject. The position of the chambers in relation to the chin rest remained fixed.
[00251] In the first configuration, an ASL cheek rest (819-2155) was mounted on the chin rest ASL. In this configuration, the head of the panel member was positioned so that the line formed from the center of the camera lens to the evaluation area is normal for the evaluation area on the forehead. In the second configuration, a forehead rest ASL (819-2150) was attached to the chin rest. In this configuration, the chin rest was positioned in such a way that the horizontal bar on the forehead rest was located on the horizontal line of the panel member, maximizing the evaluation area of each photograph.
[00252] Lighting for the photograph consisted of two Calumet Quattro fluorescent lamps (CF0003) with four Calumet 35 Watt 5500K of daylight color temperature fluorescent lights (OL2003) placed in front and on both sides of the panel member, in angle to point directly at the panel member. A glow stop polarization filter from Visual Pursuits, Inc. was also placed on the front of each lamp. The lights were allowed to warm up for at least 10 minutes before taking any pictures. In addition to lighting, a circular polarization filter was used on each of the camera's lenses to control the type of light in each photograph.
[00253] For each evaluation, two sets of photos were taken for the camera in normal shooting. In the first set, the circular polarization filter of the chamber was configured so that its polarization was parallel to the polarization of fluorescent lamps, giving an image that highlighted the brightness, as well as the fine wrinkles, pores and skin texture. In the second set, the circular polarization filter was configured so that the polarization was perpendicular (or crossed) for the polarization of the fluorescent lights producing a result that eliminated all glare showing the underlying skin tone, discoloration, and deep wrinkles. The camera's 45 ° firing was configured for each assessment so that its circular polarization filter was
73/160 configured so that this polarization was parallel to the polarization of fluorescent lamps, giving an image that highlighted the brightness, as well as the fine wrinkles, pores and skin texture.
[00254] Measuring the forehead elevation photo: To measure the height of the forehead of a photograph, a photograph was obtained using the photo capture method previously described above. A corner line was then drawn over the photograph from the medial to the lateral corner in each eye. This corner line was used as a base from which the height of the forehead was measured. The eyebrow was isolated from the image through the application of valley detection, border detection and graphic threshold operations in the image. Within an experiment, the parameters for valley and border detection were constant, so that the same eyebrow portions of each image in the series were the same. In order to accurately isolate the eyebrow, these parameters were changed to explain the differences in photographic exposure between the experiments and skin colors of the forehead between panel members. From these methods, a binary mask was created that was further manipulated in order to ensure that only the eyebrows were isolated in the image. For measurements of total height change, the center of mass of each eyebrow was then determined from its binary mask. The parameters for binary operations and center of mass determination have always been kept constant. The height of each eyebrow was normal from its center of mass to its corresponding corner line. This method measured change in overall height, but did not capture the magnitude of the change to severe bowing or angulation in which parts were raised and parts were lowered. For such cases, instead of measuring the center of mass of the eyebrow, the height of the eyebrow normal to the corner line and its right and left edges and in its center were determined from the binary mask.
74/160 [00255] Redness measurement by photoreduction: Photographs are obtained from the panel using the photographic configuration described above. Redness comparisons are made only on photographs taken within the same experiment, due to exposure, and light and face placement are only constant within a single experiment. After the series of photographs in the experiment are taken, the crossed polarization images are superimposed so that the area to be evaluated for redness reduction remains fixed as possible between each image. Using graphics manipulation software, the channels L * a * b * in CIELAB colorspace are created for each image in the series. The L * value represents the degree of illumination, while a * and b * define the chromaticity. Specifically, a * represents the degree of redness (+ values) or greenness (- values). The intensity of the red color square on the color card in the a * channel of the basal photograph is then used to normalize the subsequent images, adjusting the intensity of the image of the subsequent a * channel until the a * values within the red color square in the color cards in those images are equal to the baseline value. The evaluation area is then cut out of the photographs. The redness reduction is then determined by subtracting the a * values for the area in the 'before' photographs from the a * values in the 'after' photographs. A negative value of this subtraction indicates a reduction in redness, while a positive value indicates an increase.
Example 4: Tension testing methods [00256] The mechanical durability of the materials was assessed by creating an artificial forehead lift by applying one of the following skin pre-tensioning methods during product application. These pre-tensioning methods were used to tension the skin surface and pull the eyebrow in an elevated position:
75/160 [00257] push the orthogonal eyebrow, in which a tension was applied that originated in the eyebrow and is previously vectored from the eyebrow at an angle that was between 80 ° and 100 ° in relation to the eyebrow line, [00258] diagonal pull of the corner hairline, in which a tension was applied that originated at the most anterior and lateral point of the panel hairline and was previously vectored outward and at an angle between 10 ° and 80 ° in relation to the eyebrow line, [00259] pull orthogonal the corner thin line, in which a tension was applied that originated at the most anterior and lateral point of the panel's thin line and was previously vectored outward and at an angle between 80 ° and 100 ° in relation to the line of the eyebrow, [00260] orthogonal push the lateral hairline on which a tension was applied that originated the most lateral point of the hairline that was at or above eye level and was previously vectored out at an angle between 80 ° and 100 ° in relation to the eyebrow. [00261] While the forehead was kept elevated by one of these tensions, the product was applied to the area of the skin over which the tension was being applied. Once the film was cured, the tension was removed and the mechanical durability of the film's ability to maintain skin tensions was assessed. This assessment was achieved by measuring the degree of forehead elevation using the methods described before and after applying the product. The durability of the effect was measured by the time allowed, normal and exaggerated facial expressions and environmental tensions such as water, sweat, heat, sebum production and surface contact to interact with the film. The amount of elevation was plotted at regular intervals to determine how quickly the film's ability to maintain the mechanical benefit lasted. A film was determined to be mechanically durable if it could withstand the aforementioned stresses and maintain the forehead elevation at the level 76/160 originally reached immediately after application.
Example 5. Formulations [00262] Examples of formulations that illustrate the two-step application method are provided below. The first step of the reactive reinforcement component (eg treatment) includes formulations 60-140-1, 60-140-1B, 60-140-HP2, SK 87/2, 60-140-LX2, SK 87/1 , 48-196, 48-199, 60-211, 60-200-1N, 60-208, 66-166-F, 66-167-E, 66-166-C, 66-169-3, 66-170 , 79-23, 79-24b, 79-45, 79-46, 79-41, 8830-1, 83-16, 79-55a, 79-55b, 79-55c, 79-55d, 79-55e, 79 -55f, 79-55g, 83-54, 79-55h, 81-18, 81-19, 81-20, 81-21, 79-74, 80-23, 79-88, 79-883A, 79-74 -RD, 79-90-B, 88-70, 88-72, 88-75-2, 88-75-3, 88-80, 88-851,88-85-2, 88-83-V2, 88 -83-V3 and 83-54 shown below.
Formulation components are commercially available. The following table provides the generic name for any brand name used throughout this order.
Brand name Name of Cosmetic Ingredient inInternational Nomenclature (INCI) Airgel VM2270 Silica silicate Aerosil 8200 ™ or AerosilR8200 ™ Hexogenated modified fumed silicatildisilazane Andisil C1000 ™ Silicon dioxide + Dimethylpolysiloxane Andisil C1300 ™ Silicon dioxide + Dimethylpolysiloxane Andisil CE-4 ™ ¹ Dimethicone vinyl Andisil MV 2,000 ™ orMV2000 Dimethicone vinyl Andisil VS 1,000 ™ Dimethicone vinyl Andisil VS 10,000 ™ Dimethicone vinyl Andisil VS 165,000 ™ or Andisil VS165K Dimethicone vinyl Andisil VS 20,000 ™ Dimethicone vinyl
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Name of Cosmetic Ingredient in Brand name International Nomenclature (INCI) Andisil VS 250 ™ Dimethicone vinyl Andisil VS 500 ™ or VS500 Dimethicone vinyl Andisil VS 65,000 ™ or VS65,000 Dimethicone vinyl Andisil XL-11 ™ Hydrogen Dimethicone, Functional SiH Andisil XL-1B ™ or XL-1B Hydrogen Dimethicone, Functional SiH Aquadis titanium dioxidePersistent Rutile ™ Titanium dioxide Barium sulfate HL Barium sulphate Beaver UV / Pigment Fluo- rescuer AROMATIC HETEROCYCLECAB-O-SPERSE® 1030K is an aqueous dispersion of CAB-O-SIL® L-90, a fumed silica with a very low surface area. It is electrostatically stabilized Cabosperse 1030K with potassium hydroxide and has an alkaline pH. Carbopol Ultrez 21 Acrylates / C10- alkyl acrylate Crospolymer30 Cetiol OE Ether Dicaprila Optical Chrono-sphere Brite or Optical Chrono-sphere / Optical Brite Silica and polyurethane-40 / silica and polyurethane- tico 40 and green 5 cremaphor EL PEG-35 Castor Oil Crodamol STS PPG 3 Benzyl ether myristate DC 200 Fluid (1cSt) Dimethicone DC 2-1184 fluid (DOW CORNING® 2-1184 FLUID) Trisiloxane (e) Dimethicone DC 556 Phenyl Trimethicone
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Name of Cosmetic Ingredient in Brand name International Nomenclature (INCI) DMF5 CS dimethicone DMS-V41 Poly (Dimethylsiloxane), Finished Vinyl Dow 245 Fluid (Dow CORNING 245 Fluid) Cyclopentasiloxane Dow 246 Fluid (Dow CORNING 246 Fluid) Cyclohexasiloxane Dow 9011 Elastomer Blend (Dow Corning 9011 Elastomer Blend) Cyclopentassiloxane (e) PEG-12 Dimethicone Crospolymer Dow Corning 9011 SiliconeElastomer Blend ™ or Dow Cyclopentassiloxane (e) PEG-12 Dimethyl- Elastomer Blend 9011 in Crospolymer Dow 9045 Elastomer Blend or Dow Corning 9045 Silicone Elastomer Blend ™ Cyclopentassiloxane (e) Dimethicone Crospolymer Dow Corning 200 Fluid 0.65cSt ™ Hexamethyldisiloxane Dow Corning 245 Fluid ™ Decamethylcyclopentassiloxane Dow Corning 5329 PEG-12 Dimethicone Dow Elastomer Blend 9041 or DOW CORNING ^® 9041 ELASTOMER SILICONE BLEND Dimethicone (e) Dimethicone Crospolymer dowanol DPM Dipropylene glycol Methyl ether Dri-Flow Elite BN or DRY- Aluminum starch Octenyl succinate (e) FLO Elite BN boron nitride Flo-Beads SE-3207B ™ Ethylene-methyl methacrylate copolymer Dow Corning FZ-3196 Caprilil Meticona Ganzpearl GMP-0830 ™ Crospolymer Acrylates
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Name of Cosmetic Ingredient in Brand name International Nomenclature (INCI) Granhydrogel O ™ Water (e) Glyceryl Polyacrylate (e) 1,3Butylene Glycol (e) PVM / MA (e) Propylparaben (e) Methylparaben Granpowder Nylon ™ Nylon-12 Gransil EP-LS ™ Polysilicone-11 (e) Laureth-12 Gransurf 90 Cetyl PEG / PPG-10/1 Dimethicone Iris C12-17 alkanes Iron oxide shade or mixture of iron oxide Iron oxides Isododecane Mixture of branched C12 isoparaffins, mainly the 2,2,4,6,6 pentamethylheptane isomer (typically 85% a.a.). Jeechem BUGL ™ or Jeen BUGL Butylene Glycol Jeecide chap 5 Phenoxyethanol, Caprylyl Glycol, Potassium sorbate, Aqua, Hexylene Glycol Jeensilc CPS-312 ™ Cyclomethicone Kaolin USP BC2747 Kaolin KF6013 PEG-9 Dimethicone KTZ Xian Vistas ™ Titanium dioxide (e) Mica (e) iron oxide (C.I. 77491); chemical name: Mica (e) Titanium dioxide (e) Ferrous oxide Labrafac CC ™ Caprylic / capric triglyceride LILAC ™ (Sonneborn) C14 - 22 Alkane MPDiol Methyl Propanediol Neolone PE ™ Phenoxyethanol, Methylisothiazolinone Nylon Nylon 12 Nylon 10-I2 ™ Nylon 12 (e) Isopropyl Titanium trioesterate
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Brand name Name of Cosmetic Ingredient inInternational Nomenclature (INCI) PC 075.3 Hydrogen Dimethicone Pink paint mix Iron oxides Plantacare 818 UP ™ Coco-Glucoside; Chemical description is C8-16 fatty alcohol glycoside Platinum divinyl complex (forexample, PT-50175F) Name UPAC 1,3-Dietenyl-1,1,3,3-tetramethyldisiloxane - platinum (1: 1); Namebrand: Platinum complex-diviniltetramethyldisiloxane; synonyms:Platinum complex solution (0) -1,3-divinyl-1, 1,3,3-tetramethyldisiloxane; pt (0) -1.3- divinyl-tetramedisiloxane compl 0.100;1.3- Divinyl-1,1,3,3-tetramethyl-disiloxane-platinum (0) PMX-1184 or XIAMETER®PMX-1184 Silicone Fluid Dimethicone and trisiloxane Polyglycol P425 PPG-9 Prestige pearly beige Mixture of titanium and iron oxides from abeige color PS123-KG Hydrogen Dimethicone RM 2051 or RM 2051 Agentthickener Sodium polyacrylate (e) Dimethicone (e)Cyclopentassiloxane (e) Trideceth-6 (e)PEG / PPG 18/18 Schercemol ™ 318 Ester Isopropyl Isostearate Sepiplus 400 ™ Polyacrylate 13 (e) Polyisobutene (e)sorbate 20 Shin Etsu KF 6038 Lauril PEG-9 Polymethylsiloxyethyl Dimethicone Shin Etsu KSG 820 Lauril Dimethicone / Polyglycerin-3 Crospolí-mere Silsoft 034 Caprilil Meticona
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Brand name Name of Cosmetic Ingredient inInternational Nomenclature (INCI) silsoft ETS ethyl trisiloxane Simulgel EG ™ Sodium acrylate / acryloyldimethyl taurate co-Polymer & Isohexadecane & Polysorbate80 SIMULGEL NS Hydroxyethylacrylate / acryloyldimethyl tauratecopolymer sodium & squalane & polysorbate 60 Soft Bead B or Soft Beads B Ethylene / Methacrylate Copolymer Solagum AX Senegal acacia gum and xanthan gum SR 1000 resin Trimethylsiloxysilicate Hue Iron oxides TMF 1.5 Methyl Trimethicone Tween 20 Polysorbate 20 UCT-PS448,5 Polydimethylsiloxane, Finished Vinildimethyl USG 102 Dimethicone / Vinyl Dimethicone Crospolymer Veegum Pro Magnesium and aluminum trometamine silicate Veegum Ultra Granules Magnesium and aluminum silicate Velvesil 125 ™ Cyclopentassiloxane (e) C30-45 Alkyl Ce-loom Dimethicone Crospolymer Velvet Veil 310 ™ Mica (e) Silica Vitamin-A Complex retinol Vitamin-C Complex Ascorbic acid Vitamin-E Complex Tocopherol Blue Xirona caribbean Mica, Titanium dioxide, Silica, oxidetin
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Formulation 60-140-1
No. of the component Component Formulation Percentage (%) 1 DMS-V41 23.80 2 Aerosil 8200 9.45 3 PS123-KG 12.00 4 UCT-PS448.5 5.55 5 Velvesil 125 3.60 6 Gransil EP-LS ™ 3.60 7 Soft Beads B 1.20 8 Sepiplus 400 1.20 9 Water 27.00 10 Granhydrogel O 6.70 11 Granpowder Nylon 5.90
Procedure:
[00263] Components 1 to 4 were mixed by hand in a graded mixture of 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 5-8 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate pot, components 9 and 10 were mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, so component 11 was added at mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
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Formulation 60-140-1B
No. of the component Component Formulation Percentage (%) 1 DMS-V41 22.60 2 Aerosil 8200 8.94 3 PS123-KG 11.30 4 UCT-PS448.5 5.30 5 Velvesil 125 3.42 6 Gransil EP-LS ™ 3.42 7 Soft Beads B 1.20 8 Sepiplus 400 1.20 9 Water 25.66 10 Granhydrogel O 6.36 11 Granpowder Nylon 5.60 12 Cetiol OE 5.00 Procedure:
[00264] Components 1 to 4 were mixed by hand in a graded mixture of 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 5-8 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate pot, components 9 and 10 were mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, then components 11 and 12 were added and the mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
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Formulation 60-140-HP2
No. of the component Component Formulation Percentage (%) 1 UCT-PS448.5 32.97 2 Aerosil 8200 12.82 3 PS123-KG 14.65 4 Velvesil 125 4.40 5 Gransil EP-LS ™ 4.40 6 Soft Beads B 1.47 7 Sepiplus 400 1.47 8 Granhydrogel O 20.63 9 Granpowder Nylon 7.20
Procedure:
[00265] Components 1-3 were mixed by hand in a graded mixture of * 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 4-7 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate vessel, component 8 was mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, so component 9 was added at mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
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SK 87/2 formulation
No. of the component Component Formulation Percentage (%) 1 DMS V41 35.00 2 Aerosil 8200 11.60 3 PS123-KG 5.20 4 Velvesil 125 11.20 5 Gransil EP-LS ™ 8.70 6 Water 6.70 7 Polyvinyl alcohol 2.00 8 Granhydrogel O 8.70 9 Granpowder Nylon 6.10 10 Silsoft 034 4.80
Procedure:
[00267] Components 1-3 were mixed by hand in a graded mixture of 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 4 and 5 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate pot, components 6 and 7 were mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, then components 8-10 were added and the mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
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Formulation 60-140-LX2
No. of the component Component Percentdog (%) of Formula- 1 DMS V41 27.51 2 Aerosil 8200 10.87 3 PS123-KG 3.47 4 UCT-PS448.5 13.41 5 Velvesil 125 4.16 6 Gransil EP-LS ™ 4.16 7 Soft Bead B 1.39 8 Sepiplus 400 1.39 9 Water 21.45 10 Granhydrogel O 5.38 11 Granpowder Nylon 6.82
Procedure:
[00268] Components 1 to 4 were mixed by hand in a graded mixture of 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 5-8 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate pot, components 9 and 10 were mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, so component 11 was added at mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
87/160
SK 87/1 formulation
No. of the component Component Formulation Percentage(%) 1 DMS V41 36.90 2 Aerosil 8200 12.30 3 PS123-KG 5.50 4 Velvesil 125 11.60 5 Gransil EP-LS ™ 9.10 6 Water 7.10 7 Polyvinyl alcohol 2.00 8 Granhydrogel O 9.10 9 Granpowder Nylon 6.40 Procedure:
[00269] Components 1-3 were mixed by hand in a graded mixture of 113g (4 ounces) until the mixture was free of white particles. Subsequently, components 4 and 5 were added to and the mixture was confirmed to be homogeneous (Mixture A). In a separate pot, components 6 and 7 were mixed by hand until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation, supplied by a 4-blade propellant, 40 mm at 550 rpm, then components 8 and 9 were added and the mixing speed was at 1000 rpm and mixed for 5 minutes. The mixture was confirmed to be homogeneous.
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Formulation 48-196
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 24.46 2 Andisil VS165K 3.66 3 Aerosil 8200 9.72 4 Andisil XL-11 12.33 5 Velvesil 125 3.70 6 Gransil EP-LS ™ 3.70 7 Soft Beads B 1.23 8 Sepiplus 400 1.23 9 Water 27.75 10 Granhydrogel O 6.87 11 Neolone PE 0.21 12 Granpowder Nylon 4.11 13 Hue 1.03
Procedure:
[00270] Components 1-3 were mixed in a 113g (4 ounce) graduated with a 4 blade propellant at 1000 RPM until homogeneous (Mixture A) and the mixture was confirmed as homogeneous. In a separate container, components 4-8 were mixed with a 4-blade propellant at 750 RPM until homogeneous (Mixture B). In another container, components 9-11 were mixed with a 4-blade propellant at 750 RPM until homogeneous (Mixture C). Mixture B was added to mixture C under strong agitation, supplied by a 4-blade propellant, 40 mm at 750 rpm, then mixture A was added to the combined mixtures B and C dropwise. Finally, components 12
89/160 and 13 were added and the mixing speed increased to 1000 RPM and mixing for 10 minutes. The mixture was confirmed to be homogeneous.
Formulation 48-199
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 22.11 2 Andisil VS165K 3.31 3 Aerosil 8200 8.79 4 Andisil XL-11 11.15 5 Velvesil 125 3.35 6 Gransil EP-LS ™ 3.35 7 Soft Beads B 1.12 8 Sepiplus 400 1.12 9 Water 25.09 10 Granhydrogel O 6.21 11 Neolone PE 0.19 12 Granpowder Nylon 4.94 13 Silsoft 034 9.29
Procedure:
[00271] Components 1-3 were mixed in a 113g (4 ounce) graduated with a 4 blade propellant at 1000 RPM until homogeneous (Mixture A). In a separate container, components 4-8 were mixed with a 4-blade propellant at 750 RPM until homogeneous (Mixture B). In another container, components 9-11 were mixed with a 4-blade propellant at 750 RPM until homogeneous (Mixture C). Mixture B to Mixture C was added under strong agitation90 / 160 tion, supplied by a 4-blade propellant, 40 mm at 750 rpm, then mixture A was added to the combined mixtures B and C dropwise. Finally, components 12 and 13 were added and the mixing speed was added at 1000 RPM and mixed for 10 minutes. The mixture was confirmed to be homogeneous.
Formulation 60-211
No. of the component Component Formulation Percentage (%) 1 Andisil C1000 33.66 2 Andisil C1300 6.73 3 Andisil XL-11 9.62 4 Velvesil 125 3.46 5 Gransil EP-LS ™ 3.46 6 Soft Beads B 1.15 7 Sepiplus 400 1.15 8 Water 25.97 9 Granhydrogel O 6.42 10 Jeechem BUGL 3.85 11 Neolone PE 0.19 12 Granpowder Nylon 3.85 13 Hue 0.49
Procedure:
[00273] Components 1-7 were mixed in a 113g (4oz) graduated with a 4 blade propellant at 2000 RPM until homogeneous (Mixture A). In a separate container, components 8-11 were mixed with a 4-blade propellant at 750 RPM until ho91 / 160 mogenous (Mixture B). Mixture B was slowly added to Mixture A under strong agitation provided by a 4-blade propellant at 2000 RPM. Components 12 and 13 were added and the mixing speed was increased to 2000 RPM for 5 minutes. The mixture was confirmed to be homogeneous.
Formulation 60-200-1N
No. of the component Component Formulation Percentage (%) 1 Andisil C1000 33.88 2 Andisil C1300 7.65 3 Andisil XL-11 18.03 4 SR 1000 resin 10.93 5 Iris 2.19 6 Dri-Flow Elite BN 10.93 7 Barium sulfate HL 4.37 8 Gransil EP-LS ™ 8.74 9 Sepiplus 400 2.19 10 Neolone PE 0.55 11 Hue 0.54
Procedure:
[00275] Components 1-5 were mixed in a 113g (4 ounce) graduated with a 4 blade propellant at 2000 RPM until homogeneous (Mixture A). Components 6-9 were then added and mixed with a 4-blade propellant at 2000 RPM until homogeneous. Components 10 and 11 were added and the mixing speed was mixed at 2000 RPM until homogeneous.
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Formulation 60-208
No. of the component Component Formulation Percentage (%) 1 Andisil C1000 30.05 2 Andisil C1300 6.56 3 Andisil XL-11 22.95 4 SR 1000 resin 10.93 5 Iris 2.19 6 Dri-Flow Elite BN 10.93 7 Barium sulfate HL 4.37 8 Gransil EP-LS ™ 8.74 9 Sepiplus 400 2.19 10 Neolone PE 0.55 11 Hue 0.54 Procedure:
[00277] Components 1-5 were mixed in a 113g (4oz) graduated with a 4-blade propellant at 2000 RPM until homogeneous (Mixture A). Components 6-9 were then added and mixed with a 4-blade propellant at 2000 RPM until homogeneous. Components 10 and 11 were added and the mixing speed was mixed at 2000 RPM until homogeneous.
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Formulation 66-166-F
No. of the component Component Formulation Percentage (%) 1 Aerosil 8200 ™ 8.43% 2 Andisil VS 10,000 ™ 21.22% 3 Andisil VS 165,000 ™ 3.17% 4 Andisil XL11 ™ 10.34% 5 Velvesil 125 ™ 3.10% 6 Gransil EP-LS ™ 3.10% 7 Flo-Beads SE-3207B ™ 1.03% 8 Sepiplus 400 ™ 1.03% 9 Water 23.28% 10 Granhydrogel O ™ 5.75% 11 Neolone PE ™ 0.17% 12 Granpowder Nylon ™ 4.23% 13 Ganzpearl GMP-0830 ™ 0.31% 14 Velvet Veil 310 ™ 0.21% 15 Aquadispersable Rutile Titanium dioxide ™ 0.21% 16 Yellow iron oxide 0.09% 17 Red iron oxide 0.04% 18 Black iron oxide 0.01% 19 Dow Corning 200 Fluid0.65 cSt ™ 14.29%
Procedure:
[00278] Components 1-3 were mixed as the siloxane phase A. In phase B siloxane, components 4-8 were mixed. Compo94 / 160 nents 9-11 were combined as the aqueous phase. The aqueous phase was slowly added to the siloxane B phase and mixed until homogeneous. In this new phase, phase A was added very slowly drop by drop. Once all of the phase A siloxane was added, components 12-19 were added to the formula and mixed until homogeneous.
Formulation 66-167-E
No. of the component Component Formulation percentage (%) 1 Aerosil 8200 ™ 8.36% 2 Andisil VS 10,000 ™ 21.05% 3 Andisil VS 165,000 ™ 3.15% 4 Andisil XL11 ™ 10.25% 5 Velvesil 125 ™ 3.08% 6 Gransil EP-LS ™ 3.08% 7 Flo-Beads SE-3207B ™ 1.02% 8 Sepiplus 400 ™ 1.02% 9 Water 23.09% 10 Granhydrogel O ™ 5.70% 11 Neolone PE ™ 0.17% 12 Granpowder Nylon ™ 4.20% 13 Ganzpearl GMP-0830 ™ 0.31% 14 Velvet Veil 310 ™ 0.20% 15 Aquadispersable Rutile Titanium dioxide ™ 0.20% 16 Yellow iron oxide 0.09% 17 Red iron oxide 0.04% 18 Black iron oxide 0.01% 19 LILAC ™ (Sonneborn) 2% 20 Cetyl Dimethicone 5% 21 Granhydrogel O ™ 8%
Procedure:
[00279] Components 1-3 were mixed as phase A siloxane. In phase B siloxane components 4-8 were added. Components 9-11 were combined as the aqueous phase. The aqueous phase was slowly95 / 160 added to the siloxane B phase and mixed until homogeneous. In this new phase, phase A was added very slowly drop by drop. Once all of the phase A siloxane was added, components 12-21 were added to the formula and mixed until homogeneous.
Formulation 66-166-C
No. of the component Component Percent(%) Formulation 1 Aerosil 8200 ™ 8.43% 2 Andisil VS 10,000 ™ 21.22% 3 Andisil VS 165,000 ™ 3.17% 4 Andisil XL11 ™ 10.34% 5 Velvesil 125 ™ 3.10% 6 Gransil EP-LS ™ 3.10% 7 Flo-Beads SE-3207B ™ 1.03% 8 Sepiplus 400 ™ 1.03% 9 Water 23.28% 10 Granhydrogel O ™ 5.75% 11 Neolone PE ™ 0.17% 12 Granpowder Nylon ™ 4.23% 13 Ganzpearl GMP-0830 ™ 0.31% 14 Velvet Veil 310 ™ 0.21% 15 Aquadispersable Rutile Titanium dioxide ™ 0.21% 16 Yellow iron oxide 0.09% 17 Red iron oxide 0.04% 18 Black iron oxide 0.01% 19 Granhydrogel O ™ 14.29%
96/160
Procedure:
[00281] Components 1-3 were mixed as phase A siloxane. In phase B siloxane components 4-8 were added. Components 9-11 were combined as the aqueous phase. The aqueous phase was slowly added to the siloxane B phase and mixed until homogeneous. In this new phase, phase A was added very slowly drop by drop. Once all of the phase A siloxane was added, components 12-19 were added to the formula and mixed until homogeneous.
Formulation 66-169-3
No. of the component Component Formulation Percentage (%) 1 Ganzpearl GMP-0830 ™ 0.16% 2 Velvet Veil 310 ™ 0.10% 3 Aquadispersable Ruti-le ™ Titanium dioxide 0.10% 4 Yellow iron oxide 0.04% 5 Red iron oxide 0.02% 6 Black iron oxide 0.01% 7 Gransil EP-LS ™ 0.76% 8 Andisil XL-11 ™ 8.61% 9 Gransil EP-LS ™ 2.34% 10 Andisil C1000 ™ 33.51% 11 Andisil C1300 ™ 6.67% 12 Andisil XL-11 ™ 1.59% 13 Velvesil 125 ™ 3.48% 14 Flo-Beads SE-3207B ™ 1.15% 15 Sepiplus 400 ™ 1.27% 16 Water 25.18% 17 Granhydrogel O ™ 6.22% 18 Jeechem BUGL ™ 3.75% 19 Neolone PE ™ 0.21% 20 Granpowder Nylon ™ 3.83% 21 KTZ Xian Vistas ™ 1.00%
97/160
Procedure:
[00283] Components 1-8 were mixed and homogenized at 26,000 RPM for 10 minutes. After 10 minutes, component 9 was added and homogenized again for 10 minutes at 26,000 RPM. To this homogenized mixture, 10-15 components were added and mixed with an overhead stirrer at 2,000 RPM until homogeneous in appearance (this is the siloxane phase). In a separate container, components 16-19 were mixed until homogeneous to form the aqueous phase. The aqueous phase was added to the siloxane phase very slowly, with continuous stirring at 2,000 RPM. Once the aqueous phase was completely mixed in, components 20 and 21 were added to the formula and mixed at 2,000 RPM until homogeneous.
Formulation 66-170
No. of the component Component Percent ofFormulation (%) 1 Andisil C1300 ™ 8.92% 2 Andisil C1000 ™ 44.21% 3 Andisil XL-11 ™ 12.67% 4 Sepiplus 400 ™ 1.30% 5 Ganzpearl GMP-0830 ™ 0.18% 6 Velvet Veil 310 ™ 0.12% 7 Aquadispersable Rutile ™ Titanium dioxide 0.12% 8 Yellow iron oxide 0.05% 9 Red iron oxide 0.02%
98/160
No. of the component Component Percent ofFormulation (%) 10 Black iron oxide 0.01% 11 Dow Corning 9011 Silicone Elastomer Blend ™ 3.25% 12 Dow Corning 9045 Silicone Elastomer Blend ™ 3.25% 13 Dow Corning 245Fluid ™ 2.62% 14 Jeensilc CPS-312 ™ 0.65% 15 Water 9.49% 16 Plantacare 818 UP ™ 0.16% 17 Propylene glycol 6.60% 18 Glycerin 1.29% 19 Jeechem BUGL ™ 3.22% 20 Sodium chloride 0.32% 21 Nylon 10-I2 ™ 1.53%
Procedure:
[00284] Components 1-10 were mixed together to create siloxane phase A. Then components 11-14 were mixed to create siloxane phase B. An aqueous phase was created by mixing components 15-20. The aqueous phase was slowly added to the siloxane phase B while mixing at 2,000 RPM to create phase C. Finally, phase C was mixed in siloxane phase A until homogeneous.
99/160
Formulation 79-23
No. of the component Component Formulation Percentage (%) 1 Andisil VS 500 ™ 0.72 2 Andisil MV 2000 ™ 1.02 3 Andisil VS 65,000 ™ 17.20 4 Andisil XL-1B ™ 22.52 5 Aerosil R8200 ™ 11.77 6 Ganzpearl GMP-0830 ™ 0.19 7 Velvet Veil 310 ™ 0.13 8 Aquadispersable Rutile ™Titanium dioxide 0.13 9 Yellow iron oxide 0.05 10 Red iron oxide 0.03 11 Black iron oxide 0.01 12 Gransil EP-LS ™ 3.59 13 Velvesil 125 ™ 3.58 14 Flo-Beads SE-3207B ™ 1.02 15 Sepiplus 400 ™ 1.10 16 Water 23.72 17 Granhydrogel O ™ 6.99 18 Jeechem BUGL ™ 3.50 19 Sodium chloride 0.35 20 Neolone PE ™ 0.35 21 Granpowder Nylon ™ 2.05
Procedure:
[00286] Components 1-5 were combined and mixed (Mixture A) in an asymmetric dual centrifugal mixer at 2500 RPM while confirming that the mixture was free of white particles. Components 6-15 were mixed in Mixture A and mixed in an asymmetric dual centrifugal mixer. Mixture A was confirmed as homogeneous. In a separate vessel, components 16 and 20 were mixed with a 100 blade propeller, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under dripping while mixing with a 4-blade propellant, 40 mm at 2000 rpm and the mixture was confirmed to be homogeneous. Component 21 was added to the product of Mixture A and Mixture B and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-24b
No. of the component Component Percent ofFormulation (%) 1 Andisil VS 500 ™ 0.72 2 Andisil MV 2000 ™ 1.07 3 Andisil VS 65,000 ™ 17.91 4 Andisil XL-1B ™ 23.15 5 Aerosil R8200 ™ 12.12 6 Ganzpearl GMP-0830 ™ 0.19 7 Velvet Veil 310 ™ 0.13 8 Oxide shade ofiron 0.22 9 Gransil EP-LS ™ 3.70 10 Velvesil 125 ™ 3.70 11 Flo-Beads SE-3207B ™ 1.06 12 Sepiplus 400 ™ 1.11 13 Water 22.31 14 Granhydrogel O ™ 6.56 15 Jeechem BUGL ™ 3.28 16 Sodium chloride 0.33 17 Neolone PE ™ 0.33 18 Granpowder Nylon ™ 2.12
101/160
Procedure:
[00287] Components 4, 8 and 9 were combined and homogenized at 20000 RPM. Components 1-3, 6-7, 10-12 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture A). In a separate vessel, components 13-17 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under dripping while mixing with a 4-blade propellant, 40 mm at 2000 rpm and the mixture was confirmed to be homogeneous. Component 18 was added to the product of Mixture A and Mixture B and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-45 [00288] A 2: 1 mixture of formulations 60-211 and 79-24b was mixed together with a 4-blade propellant, 40 mm at 2000 rpm for 2 minutes.
Formulation 79-46 [00289] A 1: 2 mixture of formulations 60-211 and 79-24b was mixed together with a 4-blade propellant, 40 mm at 2000 rpm for 2 minutes.
Formulation 79-41 [00290] A 1: 5 mixture of formulations 60-211 and 79-24b was mixed together with a 4-blade propellant, 40 mm at 2000 rpm for 2 minutes.
102/160
Formulation 88-30-1
No. of the component Component Formulation Percentage (%) 1 VS500 0.68 2 MV2000 1.02 3 VS65,000 17.00 4 XL-1B 21.96 5 Aerosil R 8200 11.51 6 Dow 246 Fluid 10.43 7 Crodamol STS 1.15 8 83-49 12.00 9 83-50 3.39 10 Cabosperse 1030K 20.87
Procedure:
[00291] Ingredients 1 to 7 were mixed using a 275 RPM blade propellant to prepare phase A. In a separate vessel components 8 to 10 were mixed using a 275 RPM blade propellant to prepare phase B. Phase B was mixed in phase A at 275 RPM until the emulsion is uniform. An amount of 0.01% iron oxides was added to the final formulation to impart color. Formulation 83-49 and 83-50 are emulsions of VS 165,000 vinyl siloxane and XL-11 functionalized siloxane hydride, respectively, containing 65% siloxanes, 8% oleth-10 surfactant, and water balance.
103/160
Formulation 83-16
No. of the component Component Formulation Percentage (%) 1 Gransil EP-LS ™ 3.5 2 Andisil XL-11 ™ 9.76 3 Andisil VS 1,000 ™ 25.53 4 Andisil VS 165.000 ™ 5.12 5 Aerosil R8200 ™ 10.23 6 Velvesil 125 ™ 3.51 7 Flo-Beads SE-3207B ™ 1.17 8 Sepiplus 400 ™ 1.22 9 Granpowder Nylon ™ 3.9 10 Water 25.47 11 Granhydrogel O ™ 6.32 12 Jeechem BUGL ™ 3.97 13 Neolone PE ™ 0.22 14 Shade mix ofiron oxide 0.08
Procedure:
[00292] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 9 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 10 to 13 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 14 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
104/160
Formulation 79-55a
No. of the component Component Formulation Percentage (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-11 ™ 8.17 3 Andisil VS 1,000 ™ 32.59 4 Andisil VS 165.000 ™ 6.52 5 Andisil XL-11 ™ 3.04 6 Aerosil R8200 ™ 13.04 7 Sepiplus 400 ™ 1.14 8 Water 21.76 9 Granhydrogel O ™ 6.40 10 Jeechem BUGL ™ 3.20 11 Sodium chloride 0.32 12 Neolone PE ™ 0.32 13 Mixing of oxide shadeof iron 0.01
Procedure:
[00293] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 7 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 8 to 12 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 13 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
105/160
Formulation 79-55b
No. of the component Component Formulation Percentage (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-11 ™ 8.17 3 Andisil VS 10,000 ™ 30.33 4 Andisil VS 165.000 ™ 7.10 5 Andisil XL-11 ™ 5.49 6 Aerosil R8200 ™ 12.26 7 Sepiplus 400 ™ 1.14 8 Water 21.76 9 Granhydrogel O ™ 6.40 10 Jeechem BUGL ™ 3.20 11 Sodium chloride 0.32 12 Neolone PE ™ 0.32 13 Mixing of oxide shadeiron 0.01
Procedure:
[00294] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 7 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 8 to 12 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 13 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
106/160
Formulation 79-55c
No. of the component Component Percent ofFormulation (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.17 3 Andisil VS 500 ™ 0.84 4 Andisil MV 2.000 ™ 1.29 5 Andisil VS 65.000 ™ 21.04 6 Andisil XL-1B ™ 17.82 7 Aerosil R8200 ™ 14.20 8 Sepiplus 400 ™ 1.14 9 Water 21.76 10 Granhydrogel O ™ 6.40 11 Jeechem BUGL ™ 3.20 12 Sodium chloride 0.32 13 Neolone PE ™ 0.32 14 Iron oxide shade mix 0.01
Procedure:
[00295] Components 1 and 2 were combined and homogenized until uniform at 20000RPM (Mixture A). Components 3 to 8 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 9 to 13 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 14 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
107/160
Formulation 79-55d
No. of the component Component Percent ofFormulation (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.17 3 Andisil VS 250 ™ 1.29 4 Andisil MV 2.000 ™ 1.94 5 Andisil VS 20,000 ™ 24.52 6 Andisil CE-4 ™ 1.94 7 Andisil XL-1B ™ 0.33 8 Andisil XL-11 ™ 10.97 9 Aerosil R8200 ™ 14.20 10 Sepiplus 400 ™ 1.14 11 Water 21.76 12 Granhydrogel O ™ 6.40 13 Jeechem BUGL ™ 3.20 14 Sodium chloride 0.32 15 Neolone PE ™ 0.32 16 Mixing of oxide shadeiron 0.01
Procedure:
[00296] Components 1 and 2 were combined and homogenized until uniform at 20000RPM (Mixture A). Components 3 to 10 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 11 to 15 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture
108/160 was confirmed as homogeneous. Component 16 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-55e
No. of the component Component Percent ofFormulation (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.17 3 Andisil VS 250 ™ 1.29 4 Andisil MV 2.000 ™ 1.94 5 Andisil VS 65.000 ™ 22.91 6 Andisil XL-1B ™ 6.78 7 Andisil XL-11 ™ 8.07 8 Aerosil R8200 ™ 14.20 9 Sepiplus 400 ™ 1.14 10 Water 21.76 11 Granhydrogel O ™ 6.40 12 Jeechem BUGL ™ 3.20 13 Sodium chloride 0.32 14 Neolone PE ™ 0.32 15 Hue mixof iron oxide 0.01 Procedure:
[00297] Components 1 and 2 were combined and homogenized until uniform at 20000RPM (Mixture A). Components 3 to 9 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 10 to 14 were mixed with a 4-blade pro109 / 160, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 15 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-55f
No. of the component Component Percent ofFormulation (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.17 3 Andisil VS 250 ™ 1.34 4 Andisil VS 65.000 ™ 23.74 5 Andisil XL-1B ™ 7.03 6 Andisil XL-11 ™ 8.36 7 Aerosil R8200 ™ 14.71 8 Sepiplus 400 ™ 1.14 9 Water 21.76 10 Granhydrogel O ™ 6.40 11 Jeechem BUGL ™ 3.20 12 Sodium chloride 0.32 13 Neolone PE ™ 0.32 14 Mixing of oxide shadeof iron 0.01
Procedure:
[00298] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 8 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles are no longer
110/160 visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 9 to 13 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 14 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-55g
No. of the component Component Formulation Percentage (%) 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.17 3 Andisil VS 250 ™ 1.29 4 Andisil MV 2.000 ™ 1.94 5 Andisil VS 20,000 ™ 22.91 6 Andisil XL-1B ™ 6.78 7 Andisil XL-11 ™ 8.07 8 Aerosil R8200 ™ 14.20 9 Sepiplus 400 ™ 1.14 10 Water 21.76 11 Granhydrogel O ™ 6.40 12 Jeechem BUGL ™ 3.20 13 Sodium chloride 0.32 14 Neolone PE ™ 0.32 15 Hue mixof iron oxide 0.01
111/160
Procedure:
[00299] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 9 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 10 to 14 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 15 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 83-54
No. of the component Component Formulation Percentage (%) 1 Andisil VS 10,000 ™ 27.58 2 Andisil VS 165.000 ™ 6.46 5 Andisil XL-11 ™ 13.50 6 Aerosil R8200 ™ 17.50 7 Labrafac CC ™ 3.00 7 Sepiplus 400 ™ 1.44 8 Water 29.29 9 Plantacare 818UP ™ 0.50 11 Sodium chloride 0.36 12 Neolone PE ™ 0.36 13 Hue mixof iron oxide 0.01
112/160
Procedure:
[00300] Components 1 to 7 were added and mixed with a dual asymmetric centrifugal mixer at 2500 RPM for 6 minutes until particles are no longer visible (Mixture A). In a separate vessel, components 8 to 12 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under drip while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 13 was added to the product of Mixture A and Mixture B and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 79-55h
No. of the component Component Percentdog (%) of Formula- 1 Gransil EP-LS ™ 3.50 2 Andisil XL-1B ™ 8.15 3 Andisil VS 250 ™ 1.25 4 Andisil MV 2.000 ™ 1.85 5 Andisil VS 20,000 ™ 24.40 6 Andisil CE-4 ™ 1.85 7 Andisil XL-1B ™ 0.30 8 Andisil XL-11 ™ 10.80 9 Aerosil R8200 ™ 14.20 10 Sepiplus 400 ™ 1.14 11 Water 21.50 12 Granhydrogel O ™ 6.30 13 Jeechem BUGL ™ 3.15 14 Sodium chloride 0.30 15 Neolone PE ™ 0.30 16 UV Beaver / Fluorescent Pigment 1.00
113/160
Procedure:
[00301] Components 1 and 2 were combined and homogenized until uniform at 20000 RPM (Mixture A). Components 3 to 10 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture B). Mixture A and Mixture B were combined and mixed in a centrifuge for 6 minutes at 2500 RPM (Mixture A + B). In a separate vessel, components 11 to 15 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture C). Mixture C was added to mixture A + B under dripping while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 15 was added to the product of Mixture A + B and Mixture C and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
Formulation 81-18
No. of the component Component Formulation Percentage (%) 1 Dow 9011 Elastomer Blend 10.45 2 Dow 9045 Elastomer Blend 10.45 3 Dow 245 Fluid 8.4 4 Jeensilc CPS-312 2.09 5 PT-50175F 1.00 6 Water 30.33 7 Plantacare 818 UP 0.55 8 Neolone PE 0.21 9 Propylene glycol 20.87 10 Glycerin 4.16 11 Jeechem BUGL 10.44 12 Sodium chloride 1.05
114/160
Procedure:
[00302] Components 1-5 were mixed in a glass beaker at 2000 rpm with a propeller of 4 blades, 40 mm for 2 minutes until the mixture was homogeneous (Mixture A). Separately, components 6-12 were mixed until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation provided by a 4-blade propellant, 40 mm at 2000 rpm until homogeneous. The final formulation was further homogenized for 2 minutes.
Formulation 81-19
No. of the component Component Formulation Percentage (%) 1 Dow 9011 ElastomerBlend 10.45 2 Dow 9045 ElastomerBlend 10.45 3 Dow 245 Fluid 8.4 4 Jeensilc CPS-312 2.09 5 PT-50175F 1.00 6 Water 29.83 7 Plantacare 818 UP 0.55 8 Neolone PE 0.21 9 Propylene glycol 20.87 10 Glycerin 4.16 11 Jeechem BUGL 10.44 12 Sodium chloride 1.05 13 Nylon 10-12 0.5
115/160
Procedure:
[00303] Components 1-5 were mixed in a glass beaker at 2000 rpm with a propeller of 4 blades, 40 mm for 2 minutes until the mixture was homogeneous (Mixture A). Separately, 612 components were mixed until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation provided by a 4-blade propellant, 40 mm at 2000 rpm until homogeneous. Component 13 was then added and the resulting mixture was homogenized for 2 minutes.
Formulation 81-20
No. of the component Component Formulation Percentage (%) 1 Dow 9011 ElastomerBlend 10.45 2 Dow 9045 ElastomerBlend 10.45 3 Dow 245 Fluid 8.4 4 Jeensilc CPS-312 2.09 5 PT-50175F 1.00 6 Water 29.33 7 Plantacare 818 UP 0.55 8 Neolone PE 0.21 9 Propylene glycol 20.87 10 Glycerin 4.16 11 Jeechem BUGL 10.44 12 Sodium chloride 1.05 13 Nylon 10-12 1.0
116/160
Procedure:
[00305] Components 1-5 were mixed in a glass beaker at 2000 rpm with a propeller of 4 blades, 40 mm for 2 minutes until the mixture was homogeneous (Mixture A). Separately, 612 components were mixed until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation provided by a 4-blade propellant, 40 mm at 2000 rpm until homogeneous. Component 13 was then added and the resulting mixture was homogenized for 2 minutes.
Formulation 81-21
No. of the component Component Formulation Percentage(%) 1 Dow 9011 ElastomerBlend 10.45 2 Dow 9045 ElastomerBlend 10.45 3 Dow 245 Fluid 8.4 4 Jeensilc CPS-312 2.09 5 PT-50175F 1.00 6 Water 27.33 7 Plantacare 818 UP 0.55 8 Neolone PE 0.21 9 Propylene glycol 20.87 10 Glycerin 4.16 11 Jeechem BUGL 10.44 12 Sodium chloride 1.05 13 Nylon 10-12 3.0 Procedure:
[00307] Components 1-5 were mixed in a glass beaker at 2000 rpm with a propeller of 4 blades, 40 mm for 2 minutes until the mixture was homogeneous (Mixture A). Separately, 612 components were mixed until homogeneous (Mixture B). Mixture B was added to mixture A under strong agitation provided by a 4-blade propellant, 40 mm at 2000 rpm until homogeneous. Component 13 was then added and the resulting mixture was homogenized for 2 minutes.
117/160
Formulation 79-74
No. of the component Component Percent ofFormulation (%) 1 Andisil VS 10,000 ™ 27.58 2 Andisil VS 165,000 ™ 6.46 5 Andisil XL-11 ™ 13.50 6 Aerosil R8200 ™ 17.50 7 Schercemol ™ 318 Ester 3.00 7 Sepiplus 400 ™ 1.44 8 Water 29.29 9 Plantacare 818UP ™ 0.50 11 Sodium chloride 0.36 12 Neolone PE ™ 0.36 13 Mixing of oxide shadeiron 0.01
Procedure:
[00308] Components 1 to 7 were added and mixed with an asymmetric dual centrifugal mixer at 2500 RPM for 6 minutes until particles were no longer visible (Mixture A). In a separate vessel, components 8 to 12 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under drip while mixing with a 4-blade propellant, 40 mm at 400 rpm and the mixture was confirmed to be homogeneous. Component 13 was added to the product of Mixture A and Mixture B and mixed with a propeller of 4 blades, 40 mm at 1000 rpm until homogeneous.
118/160
Pigment dispersion formulation 80-23
No. of the component Component Percent ofFormulation (%) 1 Dow 9011 Elastomer Blend 10 2 Dow 9045 Elastomer Blend 10 3 Dow 245 Fluid 10 4 Water 27 5 Plantacare 818 UP 0.5 6 Neolone PE 0.5 7 Propylene glycol 20 8 Glycerin 4 9 Jeechem BUGL 10 10 Sodium chloride 1 11 Nylon 4.5 12 Hue 2.5 Procedure:
[00309] Components 1-3 were mixed in a glass beaker at 2000 rpm with a propeller of 4 blades, 40 mm for 2 minutes until homogeneous (Mixture A). Separately, components 5-10 were mixed until homogeneous (Mixture B). Mixture B was added to Mixture A under strong agitation, supplied by a propeller of 4 blades, 40 mm at 2000 rpm until homogeneous. Components 11 and 12 were then added and mixed at 200 rpm and even homogeneous. The final mixture was then homogenized for 2 minutes.
119/160
Formulation 79-88
No. of the component Component Percent ofFormulation (%) 1 Andisil VS 10,000 ™ 27.59 2 Andisil VS 165.000 ™ 6.46 3 Andisil XL-11 ™ 13.50 4 Aerosil R8200 ™ 17.50 5 Labrafac CC ™ 3.00 6 Sepiplus 400 ™ 1.44 7 Water 29.29 8 Plantacare 818UP ™ 0.50 9 Sodium chloride 0.36 10 Neolone PE ™ 0.36 Procedure:
[00310] Components 1 to 4 were combined and mixed with KitchenAid mixer for 5 hours. Subsequently the mixture was vacuumed overnight. Components 5 and 6 were then added and the mixture was homogenized in a 2500RPM asymmetric dual centrifugal mixer. In a separate vessel, components 7 to 10 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under drip while mixing with a 4-blade propellant, 40 mm at 500 rpm and the mixture was confirmed to be homogeneous.
120/160
Formulation 79-88-3A
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 ™ 27.59 2 Andisil VS165,000 ™ 6.46 3 Andisil XL-11 ™ 13.50 4 Aerosil R8200 ™ 17.50 5 Labrafac CC ™ 3.00 6 Simulgel EG ™ 1.44 7 Water 29.29 8 Plantacare818UP ™ 0.50 9 Sodium chloride 0.36 10 Neolone PE ™ 0.36
Procedure:
[00311] Components 1 to 4 were combined and mixed with KitchenAid mixer for 5 hours. Subsequently the mixture was vacuumed overnight. Components 5 and 6 were then added and the mixture was homogenized in a 2500RPM asymmetric dual centrifugal mixer. In a separate vessel, components 7 to 10 were mixed with a 4-blade propellant, 40 mm at 550 rpm until homogeneous (Mixture B). Mixture B was added to mixture A under drip while mixing with a 4-blade propellant, 40 mm at 500 rpm and the mixture was confirmed to be homogeneous.
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Formulation 79-74-RD
No. of the component Component Formulation Percentage (%) 1 Andisil VS 500 ™ 0.52 2 Andisil MV2000 ™ 0.80 3 Andisil VS65,000 ™ 13.04 4 Andisil XL-1B ™ 16.84 5 Aerosil R8200 ™ 8.80 6 Water 50.00 7 Veegum Pro 4.00 8 Solagum AX 1.00 9 Dow Corning5329 5.00
Procedure:
[00312] Components 1 to 5 were combined and mixed under vacuum (Mixture A). In a separate vessel, components 6 to 7 were mixed with a 4-blade propellant, 40 mm at 550 rpm until the mixture was homogeneous and the particles were thoroughly wetted (Mixture B). Component 8 was added to mixture B and mixed with a 4-blade propellant, 40 mm at 500 rpm until the mixture thickened and became homogeneous. Component 9 was added to mixture B and mixed with a 4-blade propellant, 40 mm at 500 rpm for 10 minutes. Mixture A was added slowly to Mixture B in a continuous mixture at 500 rpm. The product was homogenized for 5 minutes at 10,000 rpm.
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Formulation 79-90-B
No. of the component Component Formulation Percentage (%) 1 Andisil VS 500 ™ 0.68 2 Andisil MV 2000 ™ 1.04 3 Andisil VS 65.000 ™ 16.95 4 Andisil XL-1B ™ 21.89 5 Aerosil R8200 ™ 11.44 6 Water 40.00 7 Veegum Pro 4.00 8 Solagum AX 1.00 9 Dow Corning 5329 3.00
Procedure:
[00313] Components 1 to 5 were combined and mixed under vacuum (Mixture A). In a separate vessel, components 6 to 7 were mixed with a 4-blade propellant, 40 mm at 550 rpm until the mixture was homogeneous and the particles were thoroughly wetted (Mixture B). Component 8 was added to mixture B and mixed with a 4-blade propellant, 40 mm at 500 rpm until the mixture thickened and became homogeneous. Component 9 was added to mixture B and mixed with a 4-blade propellant, 40 mm at 500 rpm for 10 minutes. Mixture A was added slowly to Mixture B in a continuous mixture at 500 rpm. The product was homogenized for 5 minutes at 10,000 rpm.
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Formulation 88-70
No. of the component Component Percent ofFormulation (%) 1 Andisil VS10,000 28.7% 2 Andisil VS165,000 6.7% 3 Andisil XL-11 14.0% 5 Aerosil R8200 18.2% 6 KF6013 2.1% 7 TMF 1.5 2.3% 8 USG 102 2.3% 9 DI water 22.3% 10 Glycerin 1.1% 11 Jeen BUGL 1.2% 12 Jeecide Cap-5 1.0%
Procedure:
[00314] Components 1-8 (part A) and components 9-11 (part B). Part B was introduced to part A while mixing part A with a flat blade propellant at 500 RPM. The resulting solution was mixed until a uniform emulsion was formed. Component 12 was subsequently added to the emulsion.
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Formulation 88-72
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 28.60% 2 Andisil VS165,000 6.69% 3 Andisil XL-11 13.99% 5 Aerosil R8200 18.16% 6 KF6013 2.08% 7 TMF 1.5 2.25% 8 USG 102 2.35% 9 Pink paint mix 0.02% 10 DI water 22.25% 11 Glycerin 1.16% 12 Jeen BUGL 1.24% 13 Veegum Ultra Granules 0.11% 14 Kaolin USP BC2747 0.10% 15 Jeecide Cap-5 1.00%
Procedure:
[00315] Components 1-9 (Phase A) were mixed separately from components 10-14 (Phase B). Phase B was added to Phase A while mixing at 500 RPM using a 4-blade blade mixer, followed by homogenization using a Silverson homogenizer for one hour at 3000 to 5000 RPM. Subsequently, component 15 was added using a 200 rpm blade mixer.
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Formulation 88-75-2
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 21.39% 2 Andisil VS165,000 5.00% 3 Andisil XL-11 10.47% 4 Aerosil R8200 13.58% 5 RM2051 1.95% 6 DC 556 3.12% 7 FZ3196 3.11% 8 Squalane 1.85% 9 USG 102 6.90% 10 Jeechem BUGL 1.85% 11 DI water 29.03% 12 Polyglycol P425 1.22% 13 Jeecide Cap-5 0.52% Procedure:
[00316] Components 1 to 4 (Phase A) were mixed. Separately, components 5-9 were further mixed (Phase B) until a uniform dispersion was formed. Components 10-12 (Phase C) were further mixed separately. Phase C was slowly introduced into Phase B, mixing at 700 RPM with a 4-blade stem propellant to create a uniform emulsion (Phase D). Phase D was slowly introduced into Phase A at 700 RPM until uniform, and the resulting formulation was mixed for 5 minutes. Component 13 was added and mixed for 2 minutes.
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Formulation 88-75-3
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 18.64% 2 AndisilVS165,000 4.36% 3 Andisil XL-11 9.12% 4 Aerosil R8200 11.84% 5 RM2051 2.21% 6 DC 556 3.53% 7 FZ3196 3.52% 8 Squalane 2.10% 9 USG 102 7.81% 10 Jeechem BUGL 2.10% 11 DI water 32.85% 12 Polyglycol P425 1.38% 13 Jeecide Cap-5 0.54%
Procedure:
[00318] Components 1 to 4 (Phase A) were mixed. Components 5-9 (Phase B) were mixed separately from Phase A until a uniform dispersion was formed. Components 10-12 (Phase C) were further mixed separately from Phase A and Phase B. Phase C was slowly introduced into Phase B, while mixing at 700 RPM with a 4-blade stem propellant to create a uniform emulsion (Phase D) . Phase D was slowly introduced to Phase A at 700 RPM until uniform, and mixed for 5 minutes. Component 13 was then introduced to the resulting formulation and mixed for 2 minutes, followed by homogenization at 5000 RPM for 15 minutes.
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Formulation 88-80
No. of the component Component Formulation Percentage (%) 1 Andisil VS10,000 12.72% 2 Andisil VS165,000 2.98% 3 Andisil XL-11 6.23% 4 Aerosil R8200 8.08% 5 RM2051 2.79% 6 DC 556 4.45% 7 FZ3196 4.44% 8 Squalane 2.64% 9 USG 102 9.85% 10 Jeechem BUGL 2.64% 11 DI water 41.44% 12 Polyglycol P425 1.74% 13 Jeecide Cap-5 0.005%
Procedure:
[00320] Components 1 to 4 (Phase A) were mixed. Components 5-9 (Phase B) were mixed separately from Phase A until a uniform dispersion was formed. Components 10-12 (Phase C) were further mixed separately from Phase A and Phase B. Phase C was slowly introduced into Phase B, while mixing at 700 RPM with a 4-blade stem propellant to create a uniform emulsion (Phase D) . Component 13 was added to Phase D and mixed for 2 minutes. The resulting emulsion was slowly introduced into Phase A at 700 RPM until uniform, and mixed for 5 minutes, followed by homogenization at 9000 RPM for 7 minutes.
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Formulation 88-85-1
No. of the component Component Formulation Percentage (%) 1 RM 2051 3.28% 2 FZ 3196 4.92% 3 USG 102 12.11% 4 Water 48.83% 5 Jeecide Cap-5 0.87% 6 Andisil VS10,000 12.72% 7 Andisil VS165,000 2.98% 8 Andisil XL-11 6.23% 9 Aerosil R8200 8.08%
Procedure:
[00322] Components 1-3 (Phase A) were mixed. Component 4 was added while mixing Phase A, until a white emulsion was formed. Components 6-9 (Phase B) were mixed and Phase B was subsequently added to the emulsion and mixed for 5 minutes at 1300 RPM. The resulting formulation was homogenized (Silverson) for 5 minutes and component 5 was added, followed by mixing for 2 minutes at 700 RPM with a blade propellant.
Formulation 88-85-2
No. of the component Component Formulation Percentage (%) 1 RM 2051 2.62% 2 FZ 3196 3.93% 3 USG 102 9.68% 4 Water 39.03% 5 Jeecide Cap-5 0.78% 6 Andisil VS10,000 18.6% 7 Andisil VS165,000 4.4% 8 Andisil XL-11 9.1% 9 Aerosil R8200 11.8%
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Procedure:
[00323] Components 1-3 (Phase A) were mixed. Component 4 was added while mixing phase A until a white emulsion was formed. Components, 6-9 (Phase B) were mixed separately and subsequently added to the emulsion while mixing at 1300 RPM for 5 minutes. The mixture was homogenized (Silverson) for 5 minutes. Component 5 was added and the resulting formulation was mixed for 2 minutes at 700 RPM with a blade propellant.
Formulation 88-83-V2
No. of the component Component Formulation Percentage (%) 1 RM 2051 3.3% 2 FZ 3196 3.3% 3 DC 2-1184 fluid 10.0% 4 USG 102 3.3% 5 Water 46.3% 6 Jeecide Cap-5 0.3% 7 Andisil VS10,000 14.1% 8 Andisil VS165,000 3.3% 9 Andisil XL-11 6.9% 10 Aerosil R8200 9.0%
Procedure:
[00324] Components 1 to 4 were mixed (Phase A), followed by addition of component 5, until a white emulsion was formed. Component 6 was added to the emulsion and mixed for 5 minutes (base emulsion). Components 7-10 (Phase B) were mixed separately and added to the base emulsion at 1300 RPM, followed by mixing for 5 minutes and homogenization (Silverson) for 10 minutes.
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Formulation 88-83-V3
No. of the component Component Formulation Percentage (%) 1 RM 2051 3.3% 2 DC 2-1184 fluid 13.3% 3 Water 49.7% 4 Jeecide Cap-5 0.3% 5 Andisil VS10,000 14.1% 6 Andisil VS165,000 3.3% 7 Andisil XL-11 6.9% 8 Aerosil R8200 9.0%
Procedure:
[00326] Components 1 and 2 were mixed (Phase A), followed by addition of component 3, until a white emulsion was formed. Component 4 was added to the emulsion and mixed for 5 minutes (base emulsion). Components 5-8 (Phase B) were mixed separately and added to the base emulsion at 1300 RPM, followed by mixing for 5 minutes and homogenization (Silverson) for 10 minutes.
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Formulation 83-54
Composition of reactive constituent and reinforcing constituent (vinyl, hydride, fumed silica)
Tracks Brand name description Percent inWeight bottom higher Andisil VS10,000 0.05 mmol / g vinyl,10,000 cSt 42.40% 30 50 Andisil VS165,000 0.015 mmol / g vinyl,165,000 cSt 9.92% 5 15 Andisil XL-11 4.35 mmol / g, 45 cSt 20.75% 10 30 Aerosil R8200 Silica silicate 26.93% 20 34 total 100.00% Reinforcement componentreactive RM 2051 thickening agentyou Sodium polyacrylate (e)Dimethicone (e) cyclo-pentassiloxane (e) Tri-deceth-6 (e) PEG / PPG-18/18 Dimethicone 3.63% 3.00% 5.00% Gransurf 90 Cetyl PEG / PPG-10/1Dimethicone 0.50% 0.20% 2.00% PMX-1184 Dimethicone and trisiloxaneat the 13.63% 10.00% 40.00% Water AT 46.00% 20.00% 60.00% Vitamin-C Complex Ascorbic acid 0.08% 0.05% 0.50% Jeecide Cap-5 Phenoxyethanol, CaprililGlycol, Potassium sorbate, Aqua, HexyleneGlycol 0.33% 1.00% Tween 20 Polysorbate 20 0.33% 5.00% Vitamin-A Complex Vitamin A Palmitate 1.7MIU / g 0.40% 5.00% Vitamin-E Complex Vitamin E Acetate 0.10% 5.00% Constituent Compositionreactive and constituent ofreinforcement (vinyl, hydride, silicafumed) above AT 35.00% 30.00% 60.00% total 100.00%
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Procedure:
[00328] Formulation 83-54 was prepared by a procedure similar to 88-83-V3.
[00329] Andisil VS10.000, Andisil VS165.000, Andisil XL-11 were obtained from Anderson and Associates, Aerosil R8200 was obtained from Evonik, and the four components were mixed by Crisil. RM 2051 Thickening agent and PMX-1184 were obtained from Dow. Gransurf 90 was obtained from Grant. Vitamin-C complex and Vitamin A were obtained from DSM. Jeecide CAP-5 was obtained from Jeen. Tween 20 was obtained from Croda. Vitamin-E complex was obtained from TRI-K.
[00330] The second cross-linking component step includes formulations 60-148-99, 60-144-San 86-114, and 86-141c shown below.
Formulation 60-148-99
No. of the component Component Percent ofFormulation (%) 1 Water 28.60 2 Plantacare 818UP 0.49 3 Propylene glycol 19.72 4 Glycerin 3.94 5 Jeechem BUGL 9.86 6 Sodium chloride 0.99 7 Dow Elastomer Blend 9011 9.86 8 Dow Elastomer Blend 9041 9.86 9 Dow 245 Fluid 7.89 10 Jeensilc CPS-312 1.97 11 Nylon 10-12 4.64 12 Optical Brite Chrono-Sphere 0.18 13 Divinil Platinum Complex PC 075.3 1.00
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Procedure:
[00331] Components 1-6 were combined and mixed at 750 RPM for two minutes with a propeller of 4 blades, 40 mm until homogeneous to create an aqueous phase. In a separate container 7-10 components were mixed at 750 RPM for two minutes with a 4-blade propeller, 40 mm until homogeneous to create a Silicon A Mixture. In the aqueous phase, components 11 and 12 were added and mixed at 750 RPM with a propeller with 4 blades, 40 mm. The mixing speed was increased to 1000 RPM and the mixture was mixed until homogeneous and thickened. Component 13 was added and stirred at 1000 RPM for 1 minute, then homogenized at 25,000 RPM for 5 minutes.
Formulation 60-144-San
No. of the component Component Percent ofFormulation (%) 1 Water 67.47 2 Carbopol Ultrez 21 1.01 3 Denatured Ethanol 190 Proof 29.35 4 Glycerin 2.02 5 2% sodium hydroxide 0.20 6 Divinil Platinum Complex 3% PC075.3 1.99
Procedure:
[00332] Components 1 and 2 were gently mixed with a 4-blade propellant, 40 mm at 250 RPM until the Carbopol was completely wet and the mixture was free of white particles. Components 3 and 4 were added in moderate agitation provided by a 4-blade propellant, 40 mm at 500 RPM. Component 5 was added under a drip under moderate agitation provided by a
134/160 propeller with 4 blades, 40 mm at 550 RPM until the mixture is homogeneous and thickened. Component 6 was added under moderate agitation provided by a 4-blade propellant, 40 mm at 550 RPM, followed by mixing at 1000 RPM for 5 minutes until the mixture was homogeneous.
Formulation 86-114 and 86-141c
Brand name description Percentby weight Provides-ache bottom higher Divinil PlatinumComplex 2%PT-50175F(CAS # 68478-922, 2627-95-4,68083-19-2) CatalystKarstedt on vinyl-stabilized dimethiconezante 1.00% Umicore 0.50% 2.50% 1.00% total 86-114 Crosslinking component # 1 bottom higher Dow 9011 Elas-tomer Blend Cyclopentassiloxane (e) PEG-12 Dimethicone Crospolymer 10.00% DowCorning 5.00% 20.00% Dow 9045 Elas-tomer Blend Cyclopentasiloxaneand Crospolymer Dimethicone 10.00% DowCorning 5.00% 20.00% PMX -0245 Cyclopentasiloxane 10.00% DowCorning 5.00% 25.00% Water 28.50% AT - 90.00% Sodium chloride Sodium chloride 1.00% Spectrum - 5.00% Plantacare 818UP Coco-Glucosideo 0.50% Cognis 4.00% Tween 20 Polysorbate 20 0.00% Cognis - 2.00% Propylene glycol Propylene glycol 20.00% RugerChemicalCo 40.00% Lipo Polyglycol® 200 PEG-4 0.00% Lipo Chemicals Inc 40.00% Glycerin Glycerin 4.00% RugerChemicalCo 10.00% Jeechem BUGL 1,3-Butylene Glycol 10.00% Jeen - 50.00% Nylon 10-12 Nylon 12 and Isopropyl Triisostearate oftitanium 4.50% KOBO 15.00%
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Brand name description Percentby weight Provides-ache bottom higher Jeecide Cap-5 Phenoxyethanol, Caprylyl Glycol, Potassium sorbate, Aqua,Hexylene Glycol 0.50% Jeen 2.00% PT-50175F Divinildissi- Platinumloxane 1.00% Umicore 0.50% 2.50% total 100.00% total 86-141c Cross-linking component # 2 bottom higher KSG-240 Dimethicone / PEG-10/15 Crospolymer 10.00% Shin Etsu 3.00% 20.00% DC 9045 Cyclopentasiloxaneand Crospolymer Dimethicone 7.50% Dow Corning 25.00% KF-995 Cyclopentasiloxane 11.50% Shin Etsu 25.00% KF-6028 PEG-9 Polydimethyl-loxietil dimethicone 1.00% Shin Etsu 4.00% Water 28.25% AT 90.00% Sodium chloride Sodium chloride 1.00% Spectrum 5.00% Plantacare 818UP Coco-Glucosideo 0.50% Cognis 4.00% Tween 20 Polysorbate 20 0.00% Cognis 2.00% Propylene glycol Propylene glycol 20.00% RugerChemicalCo 40.00% Lipo Polyglycol® 200 PEG-4 0.00% Lipo Chemicals Inc 40.00% Glycerin Glycerin 4.00% RugerChemicalCo 10.00% Jeechem BUGL 1,3-Butylene Glycol 10.00% Jeen 50.00% Nylon 10-12 Nylon 12 and Isopropyl Triisostearate oftitanium 4.50% KOBO 15.00% Jeecide Cap-5 Phenoxyethanol, Caprylyl Glycol, Potassium sorbate, Aqua,Hexylene Glycol 0.50% Jeen 2.00% PT-50175F Divinildissi- Platinumloxane 1.25% Umicore 2.50% 100.00% total
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Procedure for 86-114:
[00333] Components 1-3 were combined and mixed at 750 RPM for two minutes until homogeneous to create a silicone phase. In a separate container, components 4-11 and 13 were mixed at 750 RPM for 15 minutes until homogeneous to create an aqueous phase. The aqueous phase was added slowly to the silicone phase and mixed at 750 RPM. The mixing speed was increased to 2000 RPM and the mixture was mixed until homogeneous and thickened. Component was added and stirred at 1000 RPM for 5 minutes. Component was added and stirred at 1000 RPM for 5 minutes.
Procedure for 86-141c:
[00334] Components 1 to 4 were combined and mixed at 750 RPM for two minutes until homogeneous to create a silicone phase. In a separate container, components 5-12 and 14 were mixed at 750 RPM for 15 minutes until homogeneous to create an aqueous phase. The aqueous phase was added slowly to the silicone phase and mixed at 750 RPM. The mixing speed was increased to 2000 RPM and the mixture was mixed until homogeneous and thickened. Component was added and stirred at 1000 RPM for 5 minutes. Component was added and stirred at 1000 RPM for 5 minutes.
Example 6: a 2-day double-blind study evaluating 2 different formulations to obtain a cosmetic benefit on aged skin [00335] Purpose: The objective of the study was to identify the leading candidates, from 2 different candidate formulations, to advance to a clinical study subsequent confirmatory. The selection criteria were based on the improvements immediately visible in the appearance of fine lines, uniformity of skin tone, skin texture and pores, as well as the duration of the effect for a period of six hours. An additional objective was to determine the ease of application of each formulation for a typical user when self-applying.
137/160 [00336] Background: This study was an early stage development project focused on bringing reactive systems based on polysiloxane for studies of topical human use. Currently, performance evaluation studies have been restricted to supervised, limited-use applications. The evaluated systems consisted of finished vinyl polysiloxanes, functionalized silicon polysiloxane hydride, fumed silica particles, and a platinum catalyst. In these studies, the polysiloxane systems were applied to the surface of the skin and cured by adding the platinum catalyst.
[00337] Composition of Test Material: The compositions of the formulation under consideration generally consisted of the following ingredients:
[00338] finished vinyl polysiloxane, [00339] polysiloxane functional hydride, [00340] fumed silica particles, [00341] platinum catalyst, and [00342] commercially available cosmetic ingredients. [00343] The polysiloxanes under consideration all exceeded a molecular weight of 600 Daltons. The percentage compositions of the polysiloxanes evaluated are summarized in the table below. These represent the upper concentration ranges of the siloxane and fumed silica materials present in the total formulation. For example, adding cosmetic ingredients at a level of 50% could lead to a dilution of each ingredient by a factor of 2, so composition number 1 was 35% finished vinyl polysiloxane, 15% polysiloxane functional hydride, 0% fumed silica, and 50% commercially available cosmetic ingredients. The platinum catalyst in the final formulation was always present in concentrations less than 500 ppm. The two treatments tested were formulations 60-140-1 and 60140-LX2 and the crosslinking component used was 60-148-99.
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Inclusion of the subject:
[00344] Number of subjects: Approximately 25 subjects were screened to include a total of 20 subjects to ensure that at least 15 subjects completed the study.
[00345] Informed Consent Form: Two copies of an informed consent form were given to each subject before the study started. The subject was given the opportunity to have his questions answered to his satisfaction. However, if doubts existed, the subject received sufficient time on the first visit to clarify open questions and concerns about the study and / or informed consent with the investigator before signing.
[00346] Subject identification: The subjects were assigned a three-digit number, which, when used in conjunction with the clinical study number, uniquely identified each subject in the study. This number remained with the subject throughout the study.
[00347] Eligibility criteria: The Fitzpatrick skin classification is based on the response of the skin's unprotected appearance for the first 30 to 45 minutes of sun exposure after a winter without sun exposure. The categories of skin types are as follows:
[00348] [00349] [00350] [00351] [00352] [00353]
Inclusion:
I Always burns easily, never tans
II Always burns easily, tans minimally
III Burns moderately, tans gradually
IV Burns minimally, always tans well
V It rarely burns; tans profusely
VI Never burns; deeply pigmented [00354] 30-65 years old [00355] Female [00356] Fitzpatrick skin types I-IV
139/160 [00357] Shows some visible signs of aging on the face including, but not limited to: large pores, wrinkles and fine lines, or weak skin tone / texture [00358] Willingness to cooperate and participate in study requirements below for the duration of the study and report any adverse symptoms immediately [00359] Little or no erythema due to sun exposure, at the treatment site at the time of treatment [00360] Able to avoid using topical skin care products not included in the study in the areas treatment during the course of the study.
Exclusion:
[00361] Fitzpatrick skin types V-VI [00362] Individuals with a known history of sensitivity or allergy to the cosmetic ingredients in the study cream [00363] Individuals with atopic skin diseases or neurodermatitis [00364] Women who know they are pregnant , breastfeeding or planning to become pregnant within 6 months [00365] Individuals who know they are being treated for cancer or a history of cancer [00366] Individuals with observable burns, tan, scarring, irregular pigmentation / tone, or other skin conditions in the test areas that can influence test results [00367] Any active dermatological condition that may interfere with clinical evaluations (eg, tattoos, eczema, psoriasis, rosacea, acne, etc.).
[00368] Study Procedure: Table 2 below describes the procedures performed at each study visit:
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Table 2
Order of events on each day Day 1Time 0 Day 1Time6 + h Day 8Time 0 Day 8Has-powder6 + h Informed consent, qualify x History of cosmetic product application taken x Sensitivity to arm formulation testing x Cleaning the face of the panelist x x Basal photograph taken x x Applied formulations x x Photo taken after application x x Live evaluation performed after application x x Picture taken after duration x x Live evaluation after duration x x Removed articles from the test x x Application of moisturizer x x
[00369] Preparation: Before the panel arrived, the two formulations were randomized so that the investigator and the photographer do not know the identity of each formulation.
[00370] Photograph: The panel members were photographed under two different lighting conditions (parallel polarized lighting and transverse polarized lighting) and at two different angles in relation to the face plane (90 °, 45 °). The panel members were positioned in a facial positioning system to reduce dorsal-ventral rotation and to position the face at approximately the same location in relation to the chamber each time. See the section on the example Photo capture adjustment in the Image analysis measurements section
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Visit 1:
[00371] Upon arrival, individuals were assessed against the exclusion / inclusion criteria and were recruited for the study if the requirements were met [00372] After recruitment, the subjects received a brief description of the study and an informed signed consent form (along with a witness) after all questions about the study had been properly answered [00373] After signing all the paperwork, the subjects were assigned the next available subject number [00374] The two formulations were tested on that subject from according to the randomization scheme were then applied by the investigator to a small area on the subject's arm leaving for 5 minutes to determine any sensitivity to the products [00375] If the panelist was not sensitive to the product, then his face was clean with a mild facial cleanser [00376] After washing the face, a baseline photograph was taken of the entire face of the subject [00377] After the basal photograph, the subject was asked to apply the test materials to the entire upper half of his face (below the eyes to the hairline, avoiding the areas below the facial bones), using his thumb to apply, under supervision [ 00378] The panelist was then photographed after 2-5 min to obtain the photo after application [00379] The panelist was then asked to complete a questionnaire on the test products applied [00380] The investigator completed an assessment by panelist alive for effectiveness against baseline situation [00381] The panelist was left for 6-8 hours and received the following instructions
142/160 [00382] Do not rub or scratch the face [00383] Do not rinse or wet the face [00384] Do not apply other products to the face [00385] If no adverse event occurred in the application area, the panelist could call the investigator and return for evaluation and removal of the film.
[00386] Once the panelist returned he was photographed and he and the investigator completed the evaluation forms [00387] If an expert advisor was scheduled for that night, then the panelist was instructed to wait until the evaluation by a period at which the assessors rated the appearance of the panel members against their baseline photographs [00388] After evaluation, the panel member received an evaluation form to leave his impressions and comments on each product [00389] After the evaluation was completed, the panelist The panel was then instructed on product removal using makeup remover [00390] A commercial skin care moisturizer with SPF 15 was then applied to the panel member's face as a moisturizer [00391] The panel member was then released Visit 2 :
[00392] Upon arrival, the panelist had his face cleaned with a mild facial cleanser [00393] After washing the face, a baseline photograph was taken of the subject's entire face [00394] After the basal photograph, the subject was instructed on the application method (see below) for each formulation and allowed to apply each formulation on its upper half of the face according to the randomization scheme in annex A (changing the application side compared to the previous visit) [00395] The procedure then continued as in step 7 of visit 1
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Photography analysis:
[00396] After the study was completed, the basal photos, after application, and after 6-8 hours were compiled on a blind deck and submitted to an expert advisor to classify the wrinkle in each photograph using the Griffiths scale exemplified below:
[00397] 0-1: No damage [00398] 2-3: Slight damage [00399] 4-5: Moderate damage [00400] 6-7: Moderate to severe damage [00401] 8-9: Serious damage [00402] The support was mounted so that the time point for the figure to be evaluated was not known. This was done to eliminate any tendency towards an unexpected result from the assessment. Due to the fact that the Griffiths score is an absolute, the differences from baseline were calculated later in the data analysis. Results:
[00403] Evaluation forms: From the investigator's evaluation forms, a scale of -2, -1, 0, +1, +2 (for strong reduction / elevation, some reduction / elevation, no reduction / elevation, any increase / fall and strong increase / fall), was created for all the different parameters evaluated. For each formulation, the average value on this scale was determined through the panel members along with the standard deviation to generate a performance indicator for each attribute being evaluated.
[00404] From the assessor's assessment forms, the same scale of -2, -1, 0, +1, +2 was applied to obtain statistical data in relation to the assessments they contained. From these average values and standard deviations, confidence in the ability of each individual formula to affect the parameter being investigated was determined.
[00405] Panelist evaluation forms were
144/160 on a scale of -1, 0, +1 for each attribute being evaluated. The average value on this scale was determined per panelist both after application and after duration to generate an indication of short and long term performance. The trend of this result was assessed against the assessor and researcher assessment results for correlation. [00406] The comments of all three forms were drawn and evaluated for any similarities.
[00407] Due to the assessment of the expert advisor not having an assessment for each week, only the forms of the investigator and the panelist were compared throughout the week for consistency in effectiveness for each formulation independent of the side to which it was applied .
[00408] Photography analysis: For post-clinical photographic analysis, each image was assigned a Griffiths score by the evaluator. The average change in this score from the corresponding baseline image for each formulation generated an indication of its effectiveness in smoothing out the appearance of fine lines and wrinkles as well as creating a more youthful appearance. These results were compared to live assessments for correlation.
[00409] Week 2 results overview: Table 3 below shows, 60-140-LX2 was much less durable compared to 60-140-1.
Table 3
Formula Failure% n = 60-140-LX2 65.38% 26 60-140-1 86.84% 38
[00410] The investigator's assessment of the panel members revealed significant differences between the performance of the two formulations (see Figure 3). Formulation 60-140-LX2 showed a significantly general improvement in the appearance of forehead wrinkles. On the other hand 60140-1 showed a more significant improvement in the appearance of wrinkles
145/160 under the eyes. This is significant in that it confirmed the hypothesis that a milder formulation could be applied to the thinner skin under the eyes to obtain a positive result. Alternatively, due to the thicker skin on the forehead, a stiffer film may be needed to produce a stronger wrinkle reduction. Matification, reduction of fine wrinkles and pore reduction were the three main general actors according to the researcher's assessment.
[00411] The assessors were able to distinguish differences in three attributes between the two formulations (see Figure 4). Formulation 60-140-LX2 showed a significant improvement in younger looking and natural feeling vs. 60-140-1, while formulation 60140-1 showed a significant improvement in stiffened vs. 60-140-LX2. All other attributes showed no significant difference between the two formulas. The three main attributes for the greatest overall change observed showed that regardless of the maturation formula, reduced pores and fine wrinkles consistently showed the greatest perceived improvement vs. basal. [00412] Panelist data showed no significant differences between the two formulas tested (see Figure 5). The main average classifier for 60-140-LX2 was the most stiff-looking attribute. The difference between 60-140-LX2 and 60-140-1 for this attribute was not significant (p ~ 0.24), but this was the most significant different attribute from those evaluated below. The sample size was too small for this study so the difference may not be significantly detectable without another test. One hypothesis by which this attribute is above younger appearance, extension of wrinkling and matification is that the panel member may have perceived the feeling of more stiffened in 60-140-LX2 thus classifying that formula more than 60-140- 1. Discounting this result, the three main performance attributes are younger in general,
146/160 reduced wrinkling and matting. The pore size does not stand out among panel members although for both advisers and researchers, this attribute has always been highly rated. It may be that the panel members did not remember their basal pore size.
[00413] Finally, advisers were asked to estimate the age of the panelist in each assessment. The difference between this age and their actual ages was then calculated and it was shown that 60-140-LX2 had a more significant effect on the age estimate by -8.7 years compared to -7.7 years with 60-140-1. (see Figure 6). [00414] Panel members were further evaluated on the Griffith scale, using before and after images. Figure 7 illustrates the result of the Griffith mean score from the blind assessment of the panelist's photographs. For both examples, the mean Griffith score was reduced by 2.15 and 1.25 points, after applying the formula 60-140-LX2 and 60-140-1, respectively. This result is consistent with Figures 4 and 5, where the panel members appeared younger after applying the formulation.
[00415] Study Investigator Assessments: A significant improvement was seen in the reduced appearance of wrinkles, pores and shine. Treatments using two selected formulations from the first week (60-140-LX2 and 60-140-1) on the upper half of the face of the panel member in reduced appearance of fine wrinkles of the panel members according to the study investigator's assessments . 60140-LX2 reduced the appearance of fine wrinkles by 100% while 60140-1 reduced them by 96% (table 4). These formulations still reduced deep wrinkles but to a lesser extent (75% and 67% respectively) compared to fine wrinkles.
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Table 4
Reduction ofwrinkle Target Reductionobserved No reduction or worsening In 60-140-LX2 Deep wrinkles 75.49% 24.51% 102 Fine wrinkles 100.00% 0.00% 78 60-140-1 Deep wrinkles 67.11% 32.89% 152 Fine wrinkles 95.76% 4.24% 118
[00416] Among different types of wrinkles, forehead wrinkles (94% and 93%) and crow's feet (96% and 87%) have been shown to be reduced to the maximum in formulations 60-140-LX2 and 60-140-1. The wrinkles under the eyes still showed to be moderately reduced (81% and 79%) along with the frown wrinkles (the deepest # 11's), which were only marginally reduced (58% and 31%) (table 5) . Table 5
Reduction ofwrinkle Target Reductionobserved No reductionor worse In 60-140-LX2 Forehead wrinkles 94.23% 5.77% 52 # 11's Deep wrinkles 58.33% 41.67% 24 Wrinkles crow's feet 96.15% 3.85% 52 Wrinkles under the eyes 80.77% 19.23% 52 60-140-1 Forehead wrinkles 92.50% 7.50% 80 # 11's Deep wrinkles 32.15% 68.75% 32 Wrinkles crow's feet 87.18% 12.82% 78 Wrinkles under the eyes 78.75% 21.25% 80
[00417] The pores on the forehead appeared to be reduced by 100% for both treatments and pores on the cheeks also appeared to be reduced by 50% and 67% in the treatment using 60-140-LX2 and 60-140-1 (table 6).
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Table 6
Pores Target Reductionobserved No reductionor worse In 60-140-LX2 Pores on the forehead 100.00% 0.00% 26 Pores on the cheeks 50.00% 50.00% 8 60-140-1 Pores on the forehead 100.00% 0.00% 40 Pores on the cheeks 66.67% 33.33% 6
[00418] Both formulations reduced the appearance of shine on the treated skin of the panel members (table 6).
Table 7
Brightness Observed reduction No reduction or worsening In 60-140-LX2 100.00% 0.00% 26 60-140-1 95.00% 5.00% 40
[00419] In general, the aesthetic performance of these two formulations was comparable in terms of reduction in wrinkles, pores and shine. However, the mechanical performance showed the difference in terms of intact film and breakage where the more rigid film showed modes of breaking such as flaking and fractionation (see tables 8 and 9)
Table 8
Formula Failure% In 60-140-LX2 65.38% 26 60-140-1 86.84% 38
Table 9
Other questions Fractionation Flaking Whitening In 60-140-LX2 26.92% 11.54% 34.62% 26 60-140-1 2.63% 2.63% 44.74% 38
149/160 [00420] Formulation 60-140-1 showed greater film durability after formed on the skin surface and only about 13% showed breakage of the film as determined by fractionation and flaking of the film. 60-140-LX2, however, showed greater film breakage (35%) indicating poor film durability when formed on the skin which resulted in more cases of film fractionation (27%) and flaking (12%). In short, 60-140-1 was able to provide a film of daily duration and was a desirable skin care treatment for improving skin appearance in reducing wrinkles, pores and shine.
[00421] Assessors 'assessment: The assessors' assessment showed a reduction of wrinkles, pores and shine on the applied skin of the panel members. The wrinkle reduction by the treatment of 60-140-LX2 and 60-140-1 was comparable (table 10).
Table 10
Wrinkles ShortQ Groupimproved No change or worsening In 60-140-LX2 General wrinkles 80.22% 19.78% 182 Deep wrinkles 70.73% 29.27% 82 Fine wrinkles 88.00% 12.00% 100 60-140-1 General wrinkles 80.70% 19.30% 285 Deep wrinkles 66.93% 33.07% 127 Fine wrinkles 91.77% 8.23% 158
[00423] The assessors noted a large reduction in the pores (table 11) and an improvement in matification (table 12) in the skin of the panel members after treatment. The skin tone of the panel members was further improved slightly and the skin appeared more stiff based on assessors' assessments (table 11).
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Table 11
Pore size Improved group No change or worsening In 60-140-LX2 95.92% 4.08% 98 60-140-1 93.13% 6.88% 160 Skin tone Improved group No change or worsening In 60-140-LX2 67.00% 33.00% 100 60-140-1 58.23% 41.77% 158 Tensed appearance Improved group No change or worsening In 60-140-LX2 78.79% 21.21% 99 60-140-1 75.00% 25.00% 152
Table 12
Matification Improved group No change or worsening In 60-140-LX2 99.00% 1.00% 100 60-140-1 98.13% 1.88% 160
[00424] While both formulations appear to generate a more youthful appearance to the skin, 60-140-LX2 showed a greater improvement in creating a youthful appearance (90%) and containing a natural feeling (86%) compared to the 60-140- 1 (73% and 79% respectively) (table 13). Impressive observations were also made on the tactile sensations of the skin treated with these formulations.
Table 13
Younger Improved group No change or worsening In 60-140-LX2 89.90% 10.10% 99 60-140-1 72.50% 27.50% 160 Natural appearance Natural Artificial or very artificial In 60-140-LX2 55.00% 45.00% 100 60-140-1 55.00% 45.00% 160 Natural feeling Natural Artificial or very artificial In 60-140-LX2 86.00% 14.00% 100 60-140-1 78.21% 21.79% 156
151/160 [00425] Silky, smooth and soft are the three main descriptors that the assessors chose to describe the sensation of treated skin. (table 14)
Table 14
SensationDesc: Aspe-frog Blurs-tea Sedo-sa Soft Soft Adhesiongo Dry In 60-140- 3.00% 20.00% 53.00 69.00 70.00 2.00% 0.00 10 LX2 % % % % 0 60-140-1 3.13% 12.50% 56.25 71.25 78.13 0.63% 0.63 16 % % % % 0
Example 7: Development of cleaner to remove corrective body compositions [00426] It has been demonstrated that commercially available cleaners have not been effective in removing the film formed when applying the corrective body compositions of the invention. To assess the performance of cleansers, the film was applied to the facial skin of volunteers. After six to eight hours, the cleaner was passed over the film and left on the film for 30 seconds. The subject was then instructed to remove the film with a towel with a certain surface roughness by gently rinsing the swollen film from the skin. The following commercially available products have been tested:
[00427] Philosophy Purity Made Simple [00428] Shiseido Benefiance Creamy Cleansing foam [00429] Noxema [00430] Estee Lauder Perfectly Clean Splash Away Foaming Cleanser [00431] Makeup forever sens'eyes [00432] Loreal go 360clean deep [00433] Remover naturally smooth eye makeup Clinique [00434] 7 in 1 anti-aging cleanser Olay Total Effects
152/160 [00435] Olay double action cleanser pore exfoliator [00436] Garnier Skin Renew [00437] Lancome Bi-Facil double action make-up remover [00438] Neutrogena invigorating sparkling deep cleanser [00439] Daily regenerating cleanser Olay regenerist [00440] CVS Pharmacy Deep Clean Makeup Remover [00441] Neutrogena Ageless essentials Continuous Hydration Cream Cleanser [00442] CVS Makeup Cleaner and Remover [00443] Natural shine facial wipes Yes to cucumbers [00444] Like none of the aforementioned products was effective in removing the film, a cleaner was prepared to disrupt the mechanical integrity of the film and to facilitate the release of the cleaning components in the film. Without wishing to be bound in theory, the removal mechanism can be described in four stages with the key components of the formula for each stage indicated in parentheses:
[00445] Film wetting (Silsoft 034, Silsoft ETS, 5CS dimethicone) [00446] Penetration of formula components (siloxane emulsifiers, siloxane phase, glycols, Cremaphor EL) [00447] Film swelling (Silsoft 034, Silsoft ETS, Isododecane, 5CS dimethicone) [00448] Release of skin film (glycols, water) [00449] Silsoft 034, Silsoft ETS, 5CS dimethicone readily moisten the surface of the film. Siloxane emulsifiers or Cremaphor EL incorporate the aqueous phase into the siloxane phase, and can facilitate the release of the swollen components of the film in the film. Silsoft 034,
153/160 isododecane, and Silsoft ETS contribute to film swelling and mechanical breakage. This allows the penetration of the aqueous phase, hydrates the skin and reduces the adhesion of the film to the skin.
[00450] Tables 15-17, below, provide compositions that were effective in removing the film:
Table 15
Siloxane phase p / p gm Silsoft 034 (caprilil meticona) 9.7% 5 Isododecane 19.4% 10 Silsoft ETS (ethyl trisiloxane) 19.4% 10 Airgel VM2270 1.5% 0.763 siloxane emulsifiers Shin Etsu KSG 820 3.9% 2 Shin Etsu KF 6038 3.9% 2 Water phase Propylene glycol 4.9% 2.5 butylene diglycol 4.9% 2.5 glycerol 1.9% 1 MPDiol 7.8% 4 DI water 19.4% 10 Neolone PE 0.5% 0.27 Optical Brite Chrono-Sphere 0.6% 0.3 Granpowder Nylon 2.1% 1.1
154/160
Table 16
No. of the component Component Formulation Percentage(%) 1 Glycerin 3.00% 2 Water 43.98% 3 dowanol DPM 6.00% 5 cremaphor EL 6.00% 6 silsoft ETS 30.00% 7 DM5 CS 10.00% 8 Prestige pearly beige 0.02% 9 Jeecide chap 5 1.00%
Table 17
No. of the component Component Formulation Percentage (%) 1 Glycerin 3.11% 2 Water 46.23% 3 dowanol DPM 6.20% 4 cremaphor EL 6.22% 5 silsoft ETS 12.43% 6 DC 200 Fluid (1cSt) 15.49% 7 DM5 CS 9.30% 8 Blue Xirona caribbean 0.02% 9 Jeecide chap 5 1.00%
155/160
Procedure:
[00451] Components 1 to 4 and 9 were mixed until a clear dispersion was formed (Phase A). Compounds 5-8 were mixed separately until uniform dispersion of the solids was formed. Phase A was subsequently added to Phase B and mixed.
Example 8: Viscosity Measurements [00452] The viscosity of a fluid can be measured by many methods known to a person skilled in the art. Specifically, The rheology handbook: for users of rotational and oscillatory rheometers By Thomas G. Mezger or ASTM standards such as ASTM D3835 - 08, ASTM D2857 - 95, ASTM D2196 - 10, and ASTM D2983 - 09 guide a specialist in the technique on how to measure the viscosity of a fluid. Illustrative methods still include the following methods:
Method A
Overview [00453] This protocol determines the viscosity (cP) on a Brookfield viscometer. This protocol can be performed in a wide variety of formulations including, among others, treatment of immediate and perfect effects.
II. Background [00454] The viscosity of the formulation is critical to its performance and aesthetics. In addition, a change in viscosity over time or exposure to a stress condition is an important indicator of formulation instability. As such, it is important to be able to reproduce and precisely assess the viscosity of the formulation. The following protocol can be used to determine the viscosity at a simple shear rate for a formulation whose viscosity is between 50 and 300 Pas.
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III. Materials [00455] A complete jar of 56 to 227g (2oz to 8oz) containing formulation of interest [00456] Brookfield viscometer DV-II + Pro EXTRA and RV-6 axes. [00457] Test requires ~ 5 minutes per sample
IV. Analytical Precautions [00458] Clean the geometry of the viscometer before use [00459] Insert the geometry to the appropriate depth in the center of the sample container [00460] Ensure that the container is stationary during the test
V. Protocol
5.1 Preparation of the equipment:
[00461] Turn on the Brookfield DV-II + Pro EXTRA viscometer by pressing a switch on the back of the instrument. Select External mode by pressing the up arrow on the instrument's control panel.
[00462] Start the Rheocalc software, a shortcut that can be found on the desktop [00463] Reset the viscometer by clicking on the ray symbol on the instrument panel key (the instrument geometry must NOT be installed) [00464] Find the RV test geometry -6 and clean with 50% / 50% IPA / mixture of mineral spirits, then dry with cloth [00465] Insert RV-6 geometry by pulling the fixing of the instrument geometry sleeve upwards.
[00466] Choose the test method by clicking on the Test button, and opening the Hold0.5-RV6-081511.RCP method.
5.2 Sample preparation:
[00467] No special sample preparation is required other than a visual inspection to ensure that the sample appears uniform.
157/160
5.3 Carry out viscosity measurement:
[00468] Insert the geometry in 56 to 227g (2oz to 8oz) of the sample under.
[00469] Ensure that the geometry is inserted to correct height measurement as indicated by the thin section on the geometry rod [00470] Ensure that the geometry is centered in the jar [00471] Adjust the support to keep the sample and geometry in appropriate relative position.
[00472] Click on the small play button on the test key to start the test [00473] Name the data files appropriately and save the file in the appropriate location [00474] Allow the test to run until completion, then save your data for further analysis Test another sample:
[00475] Slide the sample from the holder and remove the sample from the instrument [00476] Remove the geometry from the instrument and gently dry all surfaces with a 50% IPA mixture, 50% mineral spirit. Dry with a lint-free cloth.
[00477] Replace the geometry, go back to the test key and start the next test [00478] After finishing with the last sample, clean the geometry with a 50% IPA mixture, 50% mineral spirit, then dry and place in the geometry box.
SAW. Data analysis [00479] Open data file (* .DB) and click on the export button to obtain the excel file containing the data.
[00480] Locate the ViscometerPerfectorTemplate_JL-081511-v1beta1 .xlsx Excel template for data analysis
158/160 [00481] Paste the data in the first spreadsheet [00482] Record the average viscosity and standard deviation [00483] Save the model as an electronic record with a new name as a reference to the analyzed sample.
[00484] Repeat the analysis for each data set.
Method B
Overview [00485] This protocol determines the viscosity (Pas) at 0.5 1 / s, shear thinning factor (Pa * s ^A 2), and the stress rate of instability. This protocol can be performed in a variety of formulations including, among others, the treatment of immediate effects and perfection, along with another cream or lotion.
II. Background [00486] The viscosity of formulas and their alteration were correlated to the stability of formulations. As such, it is important to be able to reproducibly and accurately evaluate its viscosity properties to be used as a predictive tool for active prototypes of immediate effects. The following protocol can be used to determine viscosity, shear thinning factor, and stress rate of instability.
III. Materials [00487]> 1g Formulation of interest [00488] Bohlin CVO100 rheometer assembled with 20mm parallel plate geometry [00489] Test requires ~ 12 minutes per sample
IV. Analytical Precautions [00490] Cleaning the sides of the geometry is critical for accurate test results [00491] Any deviation should be noted
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V. Protocol [00492] Preparation of the equipment:
[00493] Adjust the Bohlin rheometer [00494] Turn on the instrument [00495] Turn on the temperature controller [00496] Start the Bohlin software [00497] Load the viscosity stability test model [00498] Ensure that both the geometry and plate are clean [00499] Install geometry [00500] Reset the instrument and you are ready to start the test. [00501] To test several samples simply lift and clean the geometry first with a dry cloth, then with a 50% / 50% IPA / mineral spirits mixture, then again with a dry cloth. Sample preparation:
[00502] No special sample preparation is required other than a visual inspection to ensure that the sample appears uniform.
SAW. Perform the Viscosity Test [00503] Place ~ 1g of mixed material on the bottom plate in a centralized mount below the geometry [00504] Lower the geometry to correct gap (250um) [00505] Clean excess material from the sides of the geometry using flat end of a spatula [00506] Allow the test to run until completion, then save your data for further analysis [00507] Continue with the next test, raise the geometry and remove the sample from the instrument. Gently clean all surfaces with 50% ipa / 50% mineral spirits mixture. Dry with a lint-free cloth.
[00508] Now you are ready to start the next cure test
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VII. Data analysis:
[00509] Locate the following Excel template for data analysis ViscosityStabilityTemplate061411-v2 [00510] Paste the raw instrument data from the appropriate Bohlin viscometer data files in A: 2 of worksheet 1 (near the left corner) of excel document [00511] Place the sample name in A: 1 of spreadsheet 1 of the Excel document [00512] Record the Viscosity (Pas) at 0.5 1 / s as calculated viscosity [00513] Record the shear thinning factor ( Pa * s ^A 2) as the calculated shear thinning factor [00514] Record the instability stress rate as the calculated stress stability (scale is 100) [00515] Save the complete model as an electronic record with a name appropriate file [00516] Repeat steps 2 to 7 for the remaining remaining data Equivalents [00517] Those skilled in the art will recognize, or be able to guarantee using, no more than routine experimentation, several polypeptide equivalents and nucleic acids, methods, assays and reagents described here. Such equivalents are considered to be within the scope of this invention and are covered by the following claims.
1/7

权利要求:
Claims (35)
[1]
1. Formulation for application to the skin characterized by the fact that it comprises:
a) a reactive reinforcement component comprising a reactive constituent and a reinforcement constituent, wherein the reactive constituent comprises at least one finished vinyl organopolysiloxane and at least one hydride functionalized polysiloxane; and
b) a cross-linking component comprising a metal catalyst;
wherein the reactive reinforcement component has a vinyl to hydride ratio between 1:10 and 1: 100; and wherein the crosslinking component catalyzes in situ crosslinking of the reactive reinforcement component, so that a film is formed on the skin.
[2]
2. Formulation according to claim 1, characterized by the fact that the reactive reinforcement component has a vinyl to hydride functional ratio between 1:15 and 1:90.
[3]
3. Formulation according to claim 1, characterized by the fact that the reactive reinforcement component has a vinyl to hydride functional ratio between 1:25 and 1:70.
[4]
4. Formulation according to claim 1, characterized by the fact that the reactive reinforcement component has a vinyl to hydride functional ratio between 1:30 and 1:60.
[5]
Formulation according to any one of claims 1 to 4, characterized by the fact that the reactive reinforcement component has a viscosity of 50,000 to 700,000 cSt or cP at 25 ° C.
[6]
6. Formulation according to any one of claims 1 to 5, characterized in that the reactive reinforcement component and the cross-linking component are prevented from reacting with each other before use.
Petition 870180007479, of 01/29/2018, p. 15/25
2/7
[7]
Formulation according to any one of claims 1 to 6, characterized in that the at least one finished vinyl organopolysiloxane has a viscosity between 100,000 and 500,000 cSt or cP at 25 ° C.
[8]
Formulation according to any one of claims 1 to 7, characterized in that the at least one finished vinyl organopolysiloxane is selected from the group consisting of: a finished vinyl polydimethylsiloxane, finished vinyl diphenylsiloxane copolymers, finished vinyl polyphenylsiloxane, vinylphenol vinilfenilmetil -fenilmetilsiloxano terminated copolymer, vinyl terminated trifluoropropilmetilsiloxano -dimetilsiloxano copolymer, vinyl terminated dietilsiloxano -dimetilsiloxano copolymer, vinylmethylsiloxane-dimethylsiloxane copolymer, trimethylsiloxy terminated, dimethylsiloxanes-vinylmethylsiloxane copolymer, silanol-terminated, dimethylsiloxanes-vinylmethylsiloxane copolymer, vinyl terminated, vinyl gums, homopolymers vinylmethylsiloxane , polymers of vinyl T structure, finished monovinyl polydimethylsiloxanes, vinylmethylsiloxane terpolymers, vinylmethoxysilane homopolymers and combinations thereof.
[9]
Formulation according to any one of claims 1 to 8, characterized in that the at least one finished vinyl organopolysiloxane has a vinyl equivalent per kilogram of 0.001 to 0.05.
[10]
Formulation according to any one of claims 1 to 9, characterized in that the reactive constituent comprises at least one high viscosity organopolysiloxane, at least one low viscosity organopolysiloxane, and at least one hydride functionalized polysiloxane, and wherein the high viscosity organopolysiloxane has a viscosity between 100,000 and 500,000 cSt or cP at 25 ° C, and the low viscosity organopolysiloxane has a viscosity between 1,000 and 50,000 cSt or cP at 25 ° C.
Petition 870180007479, of 01/29/2018, p. 16/25
3/7
[11]
11. Formulation according to any one of claims 1 to 10, characterized by the fact that said high viscosity organopolysiloxane has a vinyl weight percentage between 0.05 and 0.1, or a vinyl equivalent per kilogram between 0.001 and 0.01, or a combination of both.
[12]
Formulation according to any one of claims 1 to 11, characterized in that the at least one hydride-functionalized polysiloxane has a viscosity of 2 to 10,000 cSt or cP at 25 ° C.
[13]
13. Formulation according to any one of claims 1 to 12, characterized in that the at least one polysiloxane functionalized with hydride has a percentage content of SiH between 5 and 75%; or a SiH content of 0.5 to 10 mmol / g.
[14]
Formulation according to any one of claims 1 to 13, characterized in that the at least one polysiloxane functionalized with hydride is selected from the group consisting of: finished polydimethylsiloxane hydride, polyphenyl (dimethylhydrosiloxy) siloxane, finished hydride, copolymer methylhydrosiloxane-phenylmethylsiloxane, finished hydride, methylhydrosiloxane-dimethylsiloxane copolymers, finished trimethylsiloxy, polymethylhydrosiloxanes, trimethylsiloxy, polyethylhydrosiloxymethylsiloxymethylsiloxymethylsiloxymethylsiloxymethylsiloxymethylmethylsiloxane
[15]
Formulation according to any one of claims 1 to 14, characterized in that the hydride-functionalized polysiloxane has at least 2 Si-H units.
[16]
16. Formulation according to any one of claims 1 to 15, characterized by the fact that rganopolysiloxanes are polymers of formula II and polysiloxanes hydrated functionalized are a polymer of formula III:
Petition 870180007479, of 01/29/2018, p. 17/25
4/7 _R 1a '
I
Si-0
R ^3a
'R ^10a ' R ^9a ' |-Si-0 |Si-O- R ⁴³ ' R ⁵³ '
R® ³ '
Si ^
R® ³ ' _R 1b
R ^Jb -Si-O _R 3b
_R 10b-_R 3b Si-O Si-o- _R 4b_R 5b - rr 1
_R Sb
-Si-R ^7b _R Sb n
on what
R ^1a , R ^3a , R ^4a , R ^5a , R ^6a , R ^3a , R ^9a and R ^10a 'are each independently selected from C1-20 alkyl, C2-20 alkenyl, C ₅ . ₁₀ aryl, hydroxyl or C1-20 alkoxy, p and q are each independently an integer from 10 to 6000,
R ^1b , R ^2b , R ^3b , R ^6b , R ^7b and R ^3b are C1-20 alkyl, C2-20 alkenyl, C5.-10 aryl, hydroxyl or C1-20 alkoxy,
R ^4b , R ^5b , R ^9b and R ^10b are each independently selected from hydrogen, C1-20 alkyl, C2-20 alkenyl, C ₅ . ₁₀ aryl, hydroxyl or 0 ^ 20 alkoxy, where at least two of R ^4b , R ^5b , R ^9b and R ^10b are hydrogen, and each is independently an integer from 10 to 6000.
[17]
17. Formulation according to claim 16, characterized by the fact that R ^1a ', R ^3a ', R ^4a ', R ^5a ', R ^6a ', R ^8a ', R ^9a 'and R ^10a ' are each independently C1-20 alkyl, R ^1b , R ^2b , R ^3b , R ^6b , R ^7b and R ^3b are
20 alkyl, and R ^4b , R ^5b , R ^9b and R ^10b are each independently selected from the group consisting of hydrogen, C1-20 alkyl, and C ₅ . ₁₀ aryl, where at least two of R ^4b , R ^5b , R ^9b and R ^10b are hydrogen.
[18]
18. Formulation according to any one of claims 1 to 17, characterized in that the reinforcing constituent is selected from the group consisting of mica with optionally treated surface, zinc oxide, titanium dioxide, aluminum oxide, clay and silica.
[19]
19. Formulation according to any of claims 16 to 18, characterized by the fact that said constituent of
Petition 870180007479, of 01/29/2018, p. 18/25
5/7 reinforcement is silica, or preferably fumed silica.
[20]
Formulation according to any one of claims 1 to 19, characterized in that the metal catalyst is a platinum catalyst selected from the group consisting of platinum carbonyl cyclovinylmethylsiloxane complexes, platinum divinyl tetramethyldisoloxane complexes, cyclovinylmethylsiloxane platinum complexes , octanaldehyde / octanol platinum complexes and combinations thereof.
[21]
21. Formulation according to claim 18, characterized by the fact that the catalyst comprises between 0.005 and 0.04% of the cross-linking component.
[22]
22. Formulation according to any one of claims 1 to 21, characterized in that it comprises (i) 20% to 60% of the reactive constituent comprising at least one high viscosity finished vinyl polydimethylsiloxane and at least one finished vinyl polydimethylsiloxane low viscosity and at least one copolymer of methylhydrosiloxanedimethylsiloxane, finished trimethylsiloxy, and (ii) 8% to 13% silica, and wherein the cross-linking component comprises a platinum catalyst.
[23]
23. Formulation according to any one of claims 1 to 22, characterized in that the reactive reinforcement component comprises a finished vinyl organopolysiloxane having a viscosity between 150,000 and 185,000 cSt or cP at 25 ° C, and a functionalized polysiloxane with finished alkyl hydride having a viscosity between 30 and 100 cSt or cP at 25 ° C; and wherein the cross-linking component comprises a platinum catalyst.
Petition 870180007479, of 01/29/2018, p. 19/25
6/7
[24]
24. Formulation according to any one of claims 1 to 23, characterized by the fact that it comprises:
165,000 cSt or cP at 25 ° C finished vinyl dimethylpolysiloxane,
50 cSt or cP at 25 ° C polysiloxane functionalized with finished alkyl hydride and platinum divinyl tetramethyldisoloxane complex.
[25]
25. Formulation according to any one of claims 1 to 24, characterized in that the cross-linking component further comprises a finished vinyl organopolysiloxane.
[26]
26. Formulation according to any one of claims 1 to 25, characterized in that it further comprises one or more cosmetic or therapeutic agents.
[27]
27. Formulation according to claim 26, characterized by the fact that the one or more cosmetic or therapeutic agents is selected from sunscreens, anti-aging agents, anti-acne agents, anti-wrinkle agents, stain reducers, emollients, antioxidants, and vitamins.
[28]
28. Formulation according to any one of claims 1 to 27, characterized in that it further comprises one or more of sensation modifiers, adhesion modifiers, spreadability improvers, diluents, adhesion modifiers, optical modifiers, particles, siloxanes volatiles, emulsifiers, emollients, surfactants, thickeners, solvents, film-forming, humectants, preservatives or pigments.
[29]
29. Film characterized by the fact that it is prepared by a process comprising the step of applying the formulation as defined in any one of claims 1 to 28, so that a film is formed on the skin.
[30]
30. Film according to claim 29, characterized
Petition 870180007479, of 01/29/2018, p. 20/25
7/7 due to the fact that the film has a bond strength to the leather of more than 20 N / mm, a Young's modulus of 0.01 to 1 MPa, a fracture deformation of at least 150%, a hysteresis of less than 5%, an adhesion between 20 N / mm and 80 N / mm, a thickness of less than 100 microns, shrinks by less than 1 to 15%, or a combination thereof.
[31]
31. Method for correcting skin imperfections in a subject's skin, characterized in that it comprises applying to the subject's skin the formulation as defined in any one of claims 1 to 28, so that a film is formed on the skin, as well correcting skin imperfections.
[32]
32. Method according to claim 31, characterized in that the correction of skin imperfections in a subject's skin is selected to reduce or mask the appearance of wrinkles or bags under the eyes on a subject's skin.
[33]
33. Method for shaping a subject's body characterized by the fact that it comprises applying to the subject's body the formulation as defined in any of claims 1 to 28, so that a film is formed on the body, thus shaping the body.
[34]
34. Method according to claim 33, characterized by the fact that the film shapes the body by providing support for soft body tissues or prevents sagging of soft body tissues, in which the soft body tissue is selected from the group consisting of abdomen, buttocks, thighs, neck, forehead, jowls, breasts, the skin under the arms, and the skin around the eyes.
[35]
35. Method for delivering an agent to a subject characterized by the fact that it comprises applying to the subject's skin the formulation as defined in any of claims 1 to 28, so that a film is formed on the skin, thereby releasing the agent to the subject .
Petition 870180007479, of 01/29/2018, p. 21/25
1/7

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KR102227993B1|2019-09-24|2021-03-15|주식회사 엘지생활건강|Polymer reinforced with cerium oxide and 2 component type cosmetic composition using the same|

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WO2022004429A2|2020-07-02|2022-01-06|Shiseido Company, Ltd.|Compositions and methods for application over skin|

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WO2022030284A1|2020-08-07|2022-02-10|株式会社 資生堂|Base coat agent for coating-type body corrective film and method for using same|

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KR102289840B1|2020-11-25|2021-08-18|주식회사 메가코스|Cosmetic composition comprising reactive silicone|

法律状态:
2017-07-11| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|

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2017-10-31| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|

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2018-04-17| B06G| Technical and formal requirements: other requirements [chapter 6.7 patent gazette]|

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2018-05-29| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2018-07-31| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|

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2020-03-24| B25A| Requested transfer of rights approved|

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2020-04-07| B25A| Requested transfer of rights approved|

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2021-07-13| B25A| Requested transfer of rights approved|

优先权:

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申请号 | 申请日 | 专利标题

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US37850410P| true| 2010-08-31|2010-08-31|

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US61/378,504|2010-08-31|

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US41253110P| true| 2010-11-11|2010-11-11|

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US61/412,531|2010-11-11|

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US201161432458P| true| 2011-01-13|2011-01-13|

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US61/432,458|2011-01-13|

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US201161446377P| true| 2011-02-24|2011-02-24|

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US61/446,377|2011-02-24|

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US201161472995P| true| 2011-04-07|2011-04-07|

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US61/472,995|2011-04-07|

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US201161486643P| true| 2011-05-16|2011-05-16|

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US61/486,643|2011-05-16|

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US201161489119P| true| 2011-05-23|2011-05-23|

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US61/489,119|2011-05-23|

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US201161493020P| true| 2011-06-03|2011-06-03|

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US61/493,020|2011-06-03|

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US201161496420P| true| 2011-06-13|2011-06-13|

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US61/496,420|2011-06-13|

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US201161499002P| true| 2011-06-20|2011-06-20|

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US61/499,002|2011-06-20|

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US201161500455P| true| 2011-06-23|2011-06-23|

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US61/500,455|2011-06-23|

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PCT/US2011/050003|WO2012030984A2|2010-08-31|2011-08-31|Skin compositions and methods of use thereof|

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