DISSOLVABLE FIBROUS BLANKET STRUCTURE ARTICLE INCLUDING ACTIVE AGENTS

专利摘要:
article of a dissolvable fibrous web structure comprising active agents. these are personal care compositions of the present invention in the form of an article comprising a dissolvable fibrous batt structure. the fibers of the dissolvable fibrous batt structure comprise a surfactant; a water-soluble polymeric builder; and a plasticizer. additionally, the ratio of water-soluble polymeric builder to active agent in the fiber is 3.5 or less.
公开号:BR112012033414B1
申请号:R112012033414-0
申请日:2011-06-30
公开日:2021-07-13
发明作者:Robert Wayne Glenn Jr.；Rajeev Chhabra；William Maxwell Allen Jr.；Jonathan Paul Brennan
申请人:The Procter & Gamble Company；
IPC主号:

专利说明:

FIELD OF THE INVENTION
Described in the present invention is a personal care, oral care, health care and home care composition that delivers active agents to hair, hair follicles, skin, teeth, oral cavity, tissue and hard surfaces in the form of an article that it is a dissolvable fibrous mat structure. BACKGROUND OF THE INVENTION
Most consumer products on the market today are sold as liquid products. Although they are widely used, liquid products have disadvantages in terms of packaging, storage, transportation and convenience of use.
Consumer liquid products are typically sold in bottles, which entails significant costs as well as packaging waste, many of which end up in landfills.
Traditionally, the release of active agents from multi-component fibers is the result of fibers comprising typical thermoplastic polymers such as polyolefins', which are insoluble in water, ie the fiber does not completely dissolve. Additionally, the active agent component of such fibers traditionally incorporates active agents only in a minor proportion, for example, up to about 5% by weight.
The production of micron and submicron dissolvable fibers (and corresponding mats thereof) from aqueous processing blends comprising active agents and water-soluble polymers would be advantageous due to the very high surface area to weight ratio (immediately after fiber spinning ) which would significantly reduce the drying energy and time required to produce the solid form while still providing the highly open pore structure needed for potentially fast dissolution rates. However, the inclusion of active agents can adversely affect the rheological extension properties of the water-soluble polymer composition and the ability to produce fiber. Traditionally, fibers from poly(vinyl alcohol) solutions have been included by incorporating lower/low levels of ingredients such as plasticizers (polyethylene glycol, glycerin), extenders (clay, starch) and crosslinking agents, all of which are generally known as be compatible with fiber formation processes. However, the inclusion of high levels of ionic surfactants (anionic surfactants, amphoteric surfactants, zwitterionic surfactants, cationic surfactants) can be difficult as it can result in generally non-cohesive phase structures of the liquid/paste type (vermicular micelle; liquid crystal and phases) hexagonal) even at high concentrations.
The present inventors have surprisingly discovered the ability to produce dissolvable fibers that comprise significant levels of active agents, including ionic surfactants. In certain cases, an extensive rheology modifier is included within the compositions to improve fiber-forming ability in the presence of active agents.
Therefore, it is an object of the present composition to provide a dissolvable fibrous consumer product that can be conveniently and quickly dissolved in the consumer's palm to reconstitute a liquid product for ease of application to the target consumer substrate while providing sufficient release of active agents for the purpose. intended on target consumer substrates (with performance similar to current liquid products). A further objective is to provide such a product which can be economically produced by spinning fibers comprising the active agents. SUMMARY OF THE INVENTION
An article comprising a dissolvable fibrous batt structure comprising a significant number of fibers having an average diameter less than about 10 microns. The fibers are produced from a composition comprising: from about 10% to about 75% of a surfactant; from about 10% to about 70% water-soluble polymeric builder; and from about 1% to about 25% plasticizer; with the ratio of water-soluble polymeric builder to active agent in the fiber being 3.5 or less. BRIEF DESCRIPTION OF THE DRAWINGS
Although the specification ends with claims which specifically point out and distinctly claim the present invention, it is believed that this will be better understood from the description of the embodiments below taken in conjunction with the accompanying drawings, in which reference numbers similar are used to designate identical elements, provided that:
Figure 1 is a schematic view of a circular fluid film fibrillation nozzle for forming fibers from the processing mixing fluid;
Figure 2 is a schematic view of a slit fluid film fibrillation nozzle for forming fibers from the processing mixing fluid.
Figure 3 is a scanning electron microscopy (SEM) photomicrograph (50x) of fibers containing fused fibrillated surfactant;
Figure 4A is a configuration diagram for mixing fiber spinning processing on a four-hole continuous spinning support;
Figure 4B is a scanning electron microscopy (SEM) photomicrograph of fibers containing continuous spinning surfactant;
Figure 4C is an investigation of. microscopic dissolution of continuous spinning fibers. DETAILED DESCRIPTION OF THE INVENTION
In all embodiments of the present invention, all percentages are by weight of the total composition, unless otherwise specified. All reasons are reasons in weight, except where specified to the contrary. All ranges of values are inclusive and combinable. The number of significant figures is not representative of either the limitation of quantities indicated or the accuracy of measurements.1 All numerical quantities are understood to be modified by the word "about" unless specifically stated otherwise. Except where otherwise noted, it is understood that all measurements should be taken at 25°C and under ambient conditions, with "ambient conditions" meaning conditions under about one atmosphere of pressure and about 50% relative humidity. All of these weights, as per the ingredients listed, are based on the active level and do not include carriers or by-products that may be included in commercially available materials, except where otherwise noted. Definitions
For use in the present invention, the term "hair treatment composition" means a composition that can be applied to the hair and skin of mammals without undesirable undue effects.
The article of fibrous dissolvable mat structure may be referred to in the present invention as an "article" or "dissolvable article". All references are intended to mean the dissolvable fibrous mat structure article. A "consumer product article" for use in the present invention means the article that delivers a desired benefit to the consumer, most likely through the use of a benefit and/or active agent, e.g., a beauty care agent.
For use in the present invention, "dissolvable" means the article that satisfies the >J manual dissolution value. In one modality, the article has a manual dissolution value from about 1 to about 30 courses, in another modality, from about 2 to about 25 courses, in another modality, from about 3 to about 20 courses, and in yet another modality, from about 4 to about 15 courses, as measured by the manual dissolution method.
The article may constitute one or more layers of fibrous batt which are optionally bonded together through a bonding means (including heat1, moisture, ultrasonic, pressure, etc.).
The article has a basis weight of about 30 g/m2 to about 1000 g/m2, in another embodiment from about 60 g/m2 to about 800 g/m2, in another embodiment about 90 g/m2 m2 to about 700 g/m2 and in yet another modality from about 120 g/m2 to about 650 g/m2; and a thickness, as defined hereinafter, of from about 0.25mm to about 10mm, in one embodiment from about 0.5mm to about 7mm, and in another embodiment from about 0 .75mm to about 6mm.
The article comprises a significant number of dissolvable fibers with an average diameter of less than about 150 micrometers, in a mode of about 100 micrometers, in another mode of about 10 micrometers, and yet another mode of about 1 micrometer with a relative standard deviation less than 100%, alternatively less than 80%, alternatively less than 60%, alternatively less than 50%, as in the range of 10% to 50%, for example. As presented in the present invention, the significant number means at least 10% of all dissolvable fibres, in another modality at least 25% of all dissolvable fibres, in another modality at least 50% of all dissolvable fibres, in yet another modality at least 75% of all dissolvable fibers. In a particular modality, the significant number may be at least 99% of all dissolvable fibers. In an additional modality, at least 50% of all dissolvable fibers may have an average diameter less than about 10 micrometers. The dissolvable fibers produced by the method of the present description have a significant number of dissolvable fibers having an average diameter less than about 1 micrometer or submicron fibers. In one embodiment, the article comprising the article may have at least 25% of all dissolvable fibers with an average diameter less than about 1 micrometer, in another embodiment at least 35% of all. dissolvable fibers having an average diameter less than about 1 micrometer, in another embodiment at least 50% of all dissolvable fibers having an average diameter less than about 1 micrometer, and in yet another embodiment at least 75% of all dissolvable fibers with an average diameter less than about 1 micrometer.
For use in the present invention, the "average diameter" is calculated by an arithmetic average of the diameters of all dissolvable fibers in the measured sample. The relative standard deviation of fiber diameter is calculated by dividing the statistical standard deviation of the diameter by the average diameter of all fibers in the measured sample. The fiber diameter measurement method is described later in the description.
The basis weight of the article of the present invention is calculated as the article weight per article area (g/m2 ). The area is calculated as the projected area over air: flat surface perpendicular to the outer edges of the article. For a flat object, the area is thus computed based on the area enclosed within the outer perimeter of the sample. For a spherical object, the area is thus computed on the basis of the average diameter as 3.14 x (diameter/2)2. For cylindrical objects, the area is thus computed based on the average diameter and average length as diameter x length. For an irregularly shaped three-dimensional object, the area is calculated based on the side with the largest outside dimensions projected onto a flat surface oriented perpendicular to that side. This can be accomplished by carefully detecting the outer dimension of the object on a piece of graph paper with a pencil and then calculating the area by counting the approximate squares and multiplying by the known area, or taking a photo of the dashed area (preferably shaded for contrast) including a scale and using image analysis techniques.
Article thickness is obtained using a micrometer or thickness gauge such as the Mitutoyo Corporation Digital Disk Stand Micrometer model number IDS-1012E (Mitutoyo Corporation, 965 Corporate Blvd, Aurora, IL, USA 60504). The micrometer has a 2.54 cm (1 inch) diameter print roller weighing about 32 grams, which measures thickness at an application pressure of about 0.28 MPa (40.7 psi (6, 32 g/cm2)) .
The thickness of the article is measured by raising the impression roller, placing a section of the sample on the holder under the impression roller, carefully lowering the impression roller to contact the sample, releasing it the impression roller and measuring the sample thickness in mm on the digital display. The specimen should be fully extended to all edges of the platen roll to ensure thickness is measured at the lowest possible surface pressure, except for the case of stiffer specimens that are not flat. For stiffer samples that are not completely flat, a flat edge of the sample is measured using only a portion of the impression roller pressing down on the flat portion of the sample.
The article has a dry density of about 0.01 g/cm3 to about 0.6 g/cm3 in one embodiment from about 0.03 g/cm3 to about 0.5 g/cm3 in one embodiment from about 0.04 g/cm3 to about 0.4 g/cm3, and in another embodiment from about 0.06 g/cm3 to about 0.3 g/cm3.
The dry density of the article is determined by the equation: calculated density = article basis weight / (article thickness x 1,000). The basis weight and thickness of the article are determined in accordance with the methodologies described herein. "Personal care composition," for use in the present invention, means a composition that can be applied to mammalian keratinous tissue without undue undesirable effects." Fabric keratinous," for use herein, means layers containing keratin disposed as the outermost protective layer of mammals and includes, but is not limited to, the skin, hair, scalp and nails. "Beauty Benefit," as used herein invention, in reference to mammalian keratinous tissue, includes, but is not limited to cleaning, inhibiting sebum, reducing greasiness and/or shiny appearance of skin and/or hair, reducing dryness, itching and/or scalyness, reducing skin and/or hair. skin pore size, exfoliation, flaking, improving the appearance of keratinous tissue, conditioning, softness, etc. "Beauty benefit agent" for use in the present invention refers to cosmetics. materials that may be included in the composition to provide one or more beauty benefits. "Skin treatment actives" or "actives" for use in the present invention means compounds which, when applied to the skin, provide a benefit or enhancement to the skin. . It should be understood that the skin care actives are useful not only for application to the skin, but also to the hair, scalp, nails and other keratin tissue of mammals.
The articles described herein may be useful for conditioning treatment of keratinous tissue (e.g., hair, skin, or nails). Depending on the use in question, "treating" or "treating" or "treating" includes the regulation and/or immediate improvement of the cosmetic appearance of the keratinous tissue and/or sensation. For example, the term "regulation of skin, hair, or nail conditioning" includes: Thickening of skin, hair, or nails (eg, construction of epidermal and/or dermal and/or) subdermal layers [eg, subcutaneous fat or muscle], and where applicable to the keratin layers of the nail and hair strand) to reduce atrophy of the skin, hair or nails, increasing the convolution of the dermal-epidermal surface (also known as reticulated crest), preventing skin loss or hair elasticity (loss, damage and/or inactivation of functional skin elastin) such as elastosis, sagging, recovery from skin or hair loss; change, whether or not related to melanin, in the color of the skin, hair or nails, such as dark circles, spotting (for example, irregular red coloration resulting, for example, from rosacea) (from this point on: in front of this document called " red spots"), yellowing (pale color), discoloration caused by telangiectasia or vascular spider, and gray hair. Consumer Product Article
The present inventors have surprisingly found that an article of . A consumer formed from a fibrous batt can be produced in which each fiber comprises a significant level of one or more active agents through a fiber spinning process. This can now be accomplished by preparing a processing mixture comprising active and/or dissolved water-soluble polymeric builder agent and optionally plasticizer and spinning the composition in the presence of a pressurized gas stream (preferably heated air ) to remove most of the water and produce solid fibers; and forming the fibers into a batt, including optional bonding techniques, with a desired final moisture content, in an embodiment of about 0.5% to about 15% moisture, to form the consumer product article.
It has been found that fibers can be produced comprising. * a significant level of active/agents, specifically when the active/agent encompasses an ionic surfactant system that is generally known to form liquid/paste type non-cohesive phase structures, specifically at higher concentrations, and thereby delay the ability to produce fibers. The ability of the ionic surfactant system to produce highly elongated micelles (typically with a significant percentage of amphoteric surfactants and/or zwitterionic surfactants in synergy with anionic surfactants) can result in -synergy with the water-soluble polymeric builder resulting in viscoelasticity and rheology. extensive (viscosity) sufficient to generate the fibers.
In a further embodiment, an extensive rheology modifier can be incorporated into the processing blend composition. I
The fibers presented in the present invention comprise a water-soluble polymeric builder and an active agent with the ratio between the weight of the water-soluble polymeric builder and the active/agent in the fibers being about 3.5 or less and/or less than about 2.5 and/or less than about 1.5. and/or less than about 1.0 and/or less than about 0.5 and/or less than about 0.3 and/or to about 0.1 and/or to about 0.15 and/ or at about 0.2 . 1. Composition
The articles described here can be foamed or non-foamed in accordance with the relevant consumer instructions for use. A. Sparkling articles
Foaming articles for foaming and/or cleaning purposes comprise from about 10% to about 75%, in one modality from about 30% to about 70%, and in another modality from about >40 % to about 65%, by weight, of the surfactant personal care article; wherein the surfactant comprises one or more group I surfactants, group I including anionic surfactants which are suitable for use in hair care or other personal care compositions, and optionally one or more group II surfactants, wherein group II includes a surfactant selected from the group consisting of amphoteric, zwitterionic and combinations thereof suitable for use in hair care compositions or other personal care compositions; the ratio of group I to group II surfactants being about 100:0 to about 30:70. In another embodiment, the ratio of group I to group II surfactants is from about 85:15 to about 40:60. In yet another modality, the ratio of group I to group II surfactants is from about 70:30 to about 55:45.
Some non-limiting examples of anionic surfactants are described in US Patent Nos. 2,486,921, 2,486,922 and 2,396,278. The anionic surfactant may be selected from the group consisting of alkyl and alkyl ether sulphates, sulphated monoglycerides, sulphonated olefins, alkylaryl sulphonates, primary or secondary alkane sulphonates, alkyl sulfosuccinates, acid taurates, acid isethionates, ether sulphonate. glyceryl alkyl, sulfonated methyl esters, sulfonated fatty acids, alkyl phosphates, acyl glutamates, acyl sarcosinates, alkyl lactylates, anionic fluorosurfactants, sodium lauroyl glutamate, and combinations thereof.
Some non-limiting examples of suitable amphoteric or zwitterionic surfactants are described in US Patent Nos. 5,104,646 (Bolich Jr.' et al.) and 5,106,609 (Bolich Jr. et al.). The zwitterionic surfactant can be selected from the group consisting of cocamido ethyl betaine, cocamido propylamine oxide, cocamido propyl betaine, collagen hydrolyzed with cocamido propyl dimethylamino hydroxypropyl, collagen hydrolyzed with cocamido propyl dimonium hydroxy propyl sulfaine, cocamido propyl hydroxypropyl starch coco-betaine, coco-hydroxy sultaine, coco/oleamidopropyl betaine, coco-sultaine, lauramide propyl betaine, lauryl betaine, lauryl hydroxy sultaine and lauryl sultaine. The amphoteric surfactant can be selected from the group consisting of sodium cocoamphoacetate, sodium cocoamphodiacetate, sodium lauroamphoacetate, sodium lauroamphodiacetate, ammonium lauroamphoacetate, ammonium cocoamphoacetate, triethanol amine lauroamphoacetate and triethanolamine cocoamphoacetate.
Suitable additional group I and group II surfactants include those disclosed in US Patent Application No. 61/120,765 and the surfactants disclosed in McCutcheon's Detergents and Emulsifiers, US Edition (1986), Allured Publishing Corp.; McCutcheon's, Functional Materials, US Edition (1992), Allured Publishing Corp.; and patent no. US3,929,678 (Laughlin et al.). Other non-limiting examples of suitable surfactants are included in US document serial no. 61/120,790. B. Non-sparkling items
Non-foaming articles comprise from about 10% to about >75%, in another modality from about 15% to about 60%, and in another modality from about 20% to about 50%', in weight, of the personal surfactant article; the surfactant comprising one or more of the surfactants described below, however, with the anionic surfactants being included at a level of less than about 10%. 1. Anionic surfactants
If the article is non-foaming, the substrate may comprise a maximum level of about 10% (or less than about 10%) of anionic surfactants. 2. Non-ionic surfactants
The non-foaming articles comprise from about 10% to about 75%, in another embodiment from about 15% to about 60%, and in another embodiment from about 20% to about 50%, by weight , from the personal care article of non-ionic surfactants. In one embodiment, nonionic surfactants are included as a process aid in producing a stable article. Suitable nonionic surfactants for use include those described in McCutcheon's Detergents and Emulsifiers, US Edition (1986), Allured Publishing Corp., and McCutcheon's Functional Materials, US Edition (1992). Suitable nonionic surfactants for use in personal care compositions include, but are not limited to, polyoxyethylenated alkyl phenols, polyoxyethylenated alcohols, polyoxyethylene polyoxypropylene glycols, glyceryl esters of alkanoic acids, polyglyceryl esters of alkanoic acids, esters of propylene glycols. alkanoic acids, sorbitol esters of alkanoic acids, polyoxyethylenated sorbitol esters of alkanoic acids, polyoxyethylene glycol esters of alkanoic acids, polyoxyethylenated alkanoic acids, alkanolamides, N-alkyl pyrrolidones, alkyl glycosides, alkyl polyglycosides, alkyl amine oxides polyoxyethylene silicones. 3. Cationic surfactants
The non-foaming articles comprise from about 10% to about 75%, in another embodiment from about 15% to about 60%, and in another embodiment from about 20% to about 50%, by weight, of the personal care article of cationic surfactants. In one embodiment, cationic surfactants are included as a process aid in the production of an article. Cationic surfactants suitable for use include those described in McCutcheon's Detergents and Emulsifiers, US Edition (1986), Allured Publishing Corp., and' McCutcheonxs Functional Materials, US Edition (1992). Suitable quaternary ammonium cationic conditioner actives may include cetyl trimethyl ammonium chloride, behenyl trimethyl ammonium chloride (BTAC), stearyl trimethyl ammonium chloride, cetylpyridinium chloride, octadecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium chloride, octyl chloride dimethyl benzyl ammonium, decyl dimethyl benzyl ammonium chloride, stearyl dimethyl benzyl ammonium chloride, didodecyl dimethyl ammonium chloride, dioctadecyl dimethyl ammonium chloride, distearyl dimethyl ammonium chloride, tallow trimethyl ammonium chloride, coconut trimethyl ammonium chloride, coconut chloride dipalmitoyl. ethyl dimethyl ammonium, PEG-2 oleylammonium chloride and salts thereof, where the chloride is replaced by halogen, (eg, bromide), acetate, citrate, lactate, glycolate, nitrate phosphate, sulfate, or alkyl sulfate.
In one embodiment, the cationic quaternary ammonium conditioner actives for use in the invention is cetyl trimethyl ammonium chloride, commercially available, for example, as GENAMIN CTAC from Clariant ahd Arquad 16/29, supplied by Akzo Nobel, behenyl trimethyl chloride ammonium (BTMAC) as GENAMIN KDMP, supplied by Clariant, and distearyl dimethyl ammonium chloride as GENAMIN DSAP, supplied by Clariant. Mixtures of any of the aforementioned materials may also be suitable. In another embodiment, the quaternary ammonium cationic conditioner active is behenyl trimethyl ammonium chloride (BTMAC). 4. Polymeric surfactants
Polymeric surfactants can also be surfactants to be employed as a process aid in the production of the article, alone or in combination with ionic and/or non-ionic surfactants. Suitable polymeric surfactants for use in the personal care compositions of the present invention include, but are not limited to, block copolymers of ethylene oxide and fatty alkyl residues, block copolymers of ethylene oxide and propylene oxide, hydrophobically modified polyacrylates, hydrophobically modified celluloses, silicone polyethers, silicone copolyol esters, diquaternary polydimethyl siloxanes and co-modified amino/polyether silicones. C. Additional Components 1. Water-soluble polymer ("polymeric builder")
The article comprises water-soluble polymers which function as a builder. For use herein, the term "water-soluble polymer" is broad enough to include both water-soluble and water-dispersible polymers, and is defined as a polymer having a solubility in water, measured at 25°C. °C, of at least about 0.1 gram/liter (g/L). In some embodiments, the polymers have a solubility in water, measured at 25°C, of from about 0.1 gram/liter (g/L) to about 500 g/liter (g/L). (This indicates production of a macroscopically Isotropic or transparent, colored or colorless solution). The polymers for manufacturing these articles can be of synthetic or natural origin and can be modified through chemical reactions. These may or may not be film formers. These polymers must be physiologically acceptable, that is, they must be compatible with the skin, mucous membrane, hair and scalp.
The one or more water-soluble polymers can be present from about 10% to about 70%, by weight, of the article, in one embodiment from about 15% to about 60% of the article, and in another embodiment from about 20% to about 50% by weight of the article, and in yet another embodiment from about 25% to about 40% by weight of the article.
The one or more water-soluble polymers of the present invention can be selected such that the weight average molecular weight is from about 40,000 to about 500,000, in one embodiment, from about 50,000 to about 400,000, in a further another modality, from about 60,000 to about 300,000, and, in yet another modality, from about 70,000 to about 200,000. The weighted average molecular weight is computed by summing the average molecular weight of each polymer raw material multiplied by their respective relative percentages, by weight, of the total weight of polymers present in the article.
In one embodiment, at least one of these one or more water-soluble polymers is chosen such that a 2% by weight of the water-soluble polymer solution provides a viscosity at 20°C of about 4 centipoise to about 80 centipoise; In another embodiment, from about 5 centipoise to about 70 centipoise; and in another embodiment from about 6 centipoise to about 60 centipoise. The water soluble polymer(s) of the present invention may include, but are not limited to, synthetic polymers as described in US Pat. Serial No. 61/120,786, including polymers derived from acrylic monomers such as ethylenically unsaturated carboxylic monomers and ethylenically unsaturated monomers as described in US Patent No. 5,582,786 and EP-A-397410. The water soluble polymer(s) that are suitable may also be selected from polymers from natural sources, including those of plant origin, examples of which are described in US Serial No. 61/120,786. Modified natural polymers are also useful as water soluble polymer(s) and are included in US Serial No. 61/120,786. In one embodiment, water-soluble polymers include polyvinyl alcohols, polyacrylates, polymethacrylates, acrylic acid and methyl acrylate copolymers, polyvinyl pyrrolidones, polyalkylene oxides, starch and starch derivatives, pullulan, gelatin, hydroxy propyl methyl celluloses, methyl celluloses and carboxy methyl celluloses. In another embodiment, the water-soluble polymers include polyvinyl alcohols and hydroxypropylmethylcelluloses. Suitable polyvinyl alcohols include those available from Celanese' Corporation (Dallas, TX, USA) under the trade name of. CELVÒL®. Suitable hydroxy propyl methyl celluloses include those available from The Dow Chemical Company (Midland, MI, USA) under the trade name METHOCEL®.
In a particular embodiment, the water soluble polymer(s) mentioned above may be mixed with any single starch or combination of starches as a filler material in an amount which allows to reduce the general level of water soluble polymers required, as long as it helps to provide the personal care article with the indispensable physical/chemical structure and characteristics as described in the present invention.
In such instances, the combination of the weight percentages of the water-soluble polymer(s) and the starch-based material generally is in the range of from about 10% to about 50% by weight in one embodiment. from about 15% to about 40%, and in a specific embodiment, from about 20% to about 30%, by weight, relative to the total weight of the article. Water soluble(s) and the weight of the starch-based material can generally range from about 1:10 to about 10:1, in one embodiment, from about 1:8 to about 8:1, in another embodiment from about 1:7 to about 7:1, and in yet another embodiment from about 6:1 to about 1:6.
Typical sources of starch-based materials can include cereals, tubers, roots, vegetables and fruits. Native sources may include corn, pea, potato, banana, barley, wheat, rice, sago, amaranth, tapioca, arrowroot, sugarcane, sorghum, and waxy or high amylase varieties thereof. Starch-based materials can also include native starches that are modified by any modification process known in the art, including those described in US Serial No. 61/120,786. 2. Plasticizer
The article described herein may further comprise a water soluble plasticizer suitable for use in personal care compositions. In one embodiment, "the one or more plasticizers may be present from about 1% to about 25% by weight of the article; in another embodiment from about 3% to about 20%; in another embodiment from about 5% to about 15%. Some non-limiting examples of suitable plasticizing agents include polyols, copolyols, polycarboxylic acids, polyester and dimethicone copolyols. Examples of useful polyols include, but are not limited to, glycerin, diglycerin, propylene glycol, ethylene glycol, butylene glycol, pentylene glycol, cyclohexane dimethanol, hexane diol, polyethylene glycol (200-600), sugar alcohols such as sorbitol, mannitol, lactitol and other low molecular weight monoalcohols and polyhydric alcohols (for example , C2-C8 alcohols); mono, di, and oligosaccharides such as fructose, glucose, sucrose, maltose, lactose, and high fructose and ascorbic acid corn syrup solids. Suitable examples of polycarboxylic acids for use in the present invention are given in the docu. US Serial No. 61/120,786.
In one embodiment, plasticizers include glycerine or propylene glycol and combinations thereof. EP No. 283165B1/ discloses other suitable plasticizers, including glycerol derivatives such as propoxylated glycerol. 3. Extensive rheology modifier
The article may comprise an extensive rheology modifier. The extensive rheology modifier can be combined with the aforementioned water-soluble polymeric builders to obtain desirable rheological properties for fiber formation. Critical rheological properties for fiber formation include: shear viscosity, elongation viscosity, elasticity and others.
The weight average molecular weight of the extensive rheology modifier can be from about 500,000 to about 10,000,000, in one embodiment from about 1,000,000 to about 8,000,000, and in another embodiment from about 2,000,000 to about 6,000,000. The extensive rheology modifier may be present from about 0% by weight to about 5% by weight of the article of an extensive rheology modifier, alternatively from about 0.1% by weight to about 4% by weight in one embodiment from about 0.25% by weight to about 3% by weight and in another embodiment from about 0.5% by weight to about 2% , by weight, of the article of an extensive rheology modifier. In such cases, the weight percent of the extensive rheology modifier may be less than about 10%, in another embodiment less than 5%, and in yet another embodiment less than 2% by weight of the processing mixture it forms. the article.
In one embodiment, two or more extensive rheology modifiers of different molecular weights can be combined at various ratios in one embodiment to obtain a desired weight average molecular weight and total molecular weight distribution suitable for forming fibers, provided that each of the polymers individually sourced has a weight average molecular weight of from about 500,000 to about 10,000,000. In one embodiment, a high weight average molecular weight polymer can be combined with a low weight average molecular weight polymer to obtain rheological properties such as shear viscosity, elongation viscosity and elasticity of the processing mixture desirable for fiber formation. . One of ordinary skill in the fiber-forming art may be able to optimize the ratio of high weight average molecular weight to low weight average molecular weight polyethylene oxide to obtain desirable fiber-forming rheological properties.
Extensive rheology modifiers can be selected from polyvinyl alcohols, polyvinyl pyrrolidones, polyalkylene oxides, polyacrylates, caprolactams, polymethacrylates, polymethylmethacrylates, polyacrylamides, polymethylacrylamides, polydimethylacrylamides, polyethylene glycol monomethacrylates, polyvinyl acetates, polyurethane acids polyesters, polyamides, polyamines, polyethyleneimines, maleic/(acrylate-or methacrylate) copolymers, methylvinyl ether and maleic anhydride copolymers, vinyl acetate and crotonic acid copolymers, vinylpyrrolidone and vinyl acetate copolymers, vinylpyrrolidone copolymers and. of caprolactam, vinyl pyrolidone/vinyl acetate copolymers, copolymers of anionic, cationic and amphoteric monomers, karaya gum, gum tragacanth, gum arabic, acemannan, coniaco manan, acacia gum, gati gum, whey protein isolate and soy protein isolate; seed extracts including guar gum, locust bean gum, quince seed, and plantago seed; kelp extracts such as carrageenan, alginate, and agar; fruit extracts (pectins); those of microbial origin including xanthan gum, gellan gum, pullulan, hyaluronic acid, chondroitin sulfate, and dextran; and those of animal origin including casein, gelatin, keratin, keratin hydrolysates, sulphonic keratins, albumin, collagen, glutelin, glucagons, gluten, zein, shellac, cellulose derivatives such as hydroxypropylmethylcellulose, hydroxymethylcellulose, hydroxyethylcellulose, methylcellulose, hydroxypropylcellulose, ethylcellulose , carboxymethylcellulose, cellulose acetate phthalate, nitrocellulose and other cellulose esters/ethers; guar gum derivatives such as hydroxypropyl guar gum; and combinations thereof.
In one embodiment, extensive rheology modifiers include polyethylene oxides.
In another embodiment, a polyethylene oxide of weight average molecular weight of about 8,000,000 can be combined with a polyethylene oxide of weight average molecular weight of about 1,000,000 in ratios in the range of about 5:95 to about 95:5 by weight. In another embodiment, a polyethylene oxide of weight average molecular weight of about 6,000,000 can be combined with a polyethylene oxide of weight average molecular weight of about 2,000,000 in ratios in the range of about 5:95 about 95:5 by weight; In yet another embodiment, a polyethylene oxide of weight average molecular weight of about 10,000,000 can be combined with a polyethylene oxide of weight average molecular weight of about 1,000,000 in ratios in the range of about 1:99 to about 99:1 by weight. Without being bound by theory, the combination of a small percentage of a very high molecular weight polymer such as a polyethylene oxide of molecular weight of about 10,000,000 with a lower molecular weight polymer such as a polyethylene oxide of a molecular weight of about 10,000,000 about 1,000,000 provides elasticity and high elongation viscosity while minimally impacting the shear viscosity of a polymer solution or molten material to form fibers. The blend ratio between high and low molecular weight polymers depends on the rheological properties as a whole and the surface tension of the processing mixture, and the fiber forming processing conditions. 4. Optional Ingredients
The article may further comprise other optional ingredients that are known for use or otherwise useful in consumer product compositions, provided such optional materials are compatible with the selected essential materials described herein, or do not otherwise unduly harm the performance of the composition.
Optional ingredients may comprise active/agents which may be selected from the group consisting of: personal conditioning and/or cleansing agents such as hair care agents, hair conditioning agents, skin care agents and skin conditioning agents; conditioning and/or laundry care agents such as fabric care agents, fabric conditioning agents, fabric softening agents, fabric anti-crease agents, fabric care antistatic agents, fabric treatment stain removal agents, fabric care agents, soil release, dispersing agents, soil suppression agents, defoamers and fabric renewal agents; hard surface care and/or treatment agents such as liquid dishwashing agents, powdered dishwashing agents, polishing agents, microbicidal agents, perfume, bleaching agents (such as oxygen bleaching agents, hydrogen peroxide, bleaching agents of percarbonate, perborate bleaching agents, chlorine bleaching agents), bleach activating agents, chelating agents, builders, gloss agents, dye transfer inhibiting agents, water softening agents, water hardening agents, bleaching agents pH adjustment, acids, bases, medicinal agents, lotions, tooth whitening agents, dental care agents, mouthwash agents, periodontal gum care agents, sunscreens, enzymes, flooculating agents, effervescent agents/preservatives, agents cosmetics, make-up removing agents, foaming agents, deposition aiding agents, <decoat forming agents weeds, clays, thickening agents, latexes, silicas, drying agents, water treatment agents, odor controlling agents, antiperspirant agents, cooling agents, heating agents, absorbent gelling agents, anti-inflammatory agents, ■ dyes , pigments, edible agents, dietary agents, vitamins, minerals and combinations thereof.
Optional ingredients may also include those materials approved for use in cosmetics and which are described in reference books such as the CTFA Cosmetic Ingredient Handbook, Second Edition, The Cosmetic, Toiletries, and Perfume Association, Inc. 1988, 1992. Examples of such ingredients options are shown in US Serial Nos. 12/361,634, 10/392,422 filed March 18, 2003; and in publication US2003/0215522A1, dated November 20, 2003.
Other optional ingredients include organic solvents, especially water-miscible solvents and co-solvents useful as solubilizing agents for polymeric structurants and as drying accelerators. Examples of suitable organic solvents are given in US Serial No. 12/361,634. Other optional ingredients include: latex or emulsion polymers, thickeners such as water soluble polymers, clays, silicas, ethylene glycol distearate, deposition aids, including coacervate forming components. Additional optional ingredients include anti-dandruff actives which include, but are not limited to, zinc pyrithione, selenium sulfide and the actives disclosed in US Publication No. 2003/0215522A1. Additionally, optional ingredients may comprise cationic surfactants as included above.
In one embodiment, the articles can comprise the active agents in the form of a physically adsorbed surface resident coating, as a thin liquid film or as fine particulates. In one embodiment, the ratio of the article to the coating that is on the surface comprising said at least one active agent is from about 110:1 to about 0.1:1, in another embodiment, from about 20 :1 to about 0.2:1, and in another embodiment, from about 10:1 to about 0.3:1, and in yet another embodiment, from about 1:1 to about 0.4: 1. The surface coating may comprise from about 10% to about 100% active agents, by weight, of the surface coating, in one embodiment from about 30% to about 100%, and in another modality from about 50% to about 100%.
The coating which is on the surface comprising the one or more active agents is situated on at least a portion of the surface of the article and can permeate the article in whole or in part. Alternatively, the coating that is on the surface can be included between two separate layers of the article (e.g., sandwiched or wrapped). The surface coating can be sprayed, atomized, dripped, coated, surface-printed (for example, in the shape of an ornament, decoration or desired pattern), poured over, injected into the interior, dipped, or any other suitable means, such as by use of a depositor, sieve, or bed of powder. Those skilled in the art should understand that the coating can be applied as a powder coating or it can be a fluid coating. For example, where the coating is a fluid coating, the coating can be sprayed, spread, dripped, stamped, sandwiched between different articles or different portions of the same article, layered, injected, rolled over, or dipped. The coating can be applied over entire portions or regions of the outer surface of the article and can be applied in a manner to adorn, decorate, form a logo, models, etc. In one embodiment, the fibrous articles comprise one or more water-releasable matrices that comprise active agents. The one or more water-releasable matrix complexes comprising active agents can be incorporated into the composition that is manipulated to form the article. The water-releasable matrix complexes comprising the active agents can be incorporated into a coating that is on the surface. In one embodiment, the coating that is on the surface comprises from about 10% to about 100% of one or more water-releasable matrix complexes comprising active agents, in another embodiment from about 25% to about 100% and in yet another modality from about "40% to about 100%.'
The ratio of the water-releasable matrix material to the one or more active agents in the complex is, in one embodiment, from about 0.5:1 to about 19:1, in another embodiment, from about 0. 7:1 to about 6:1, and in yet another embodiment, from about 1:1 to about 3:1. The water-releasable -matrix complexes comprising active agents according to the invention are in particulate form and may have a particle size of from about 1 µm to about 200 µm, in another embodiment, from about 2 µm to about 100 µm, and in yet another modality, from about 3 µm to about 50 µm.
The water-releasable matrix materials of the present invention can include cyclodextrins as well as high surface area particles that form complexes such as starches, polyethylenes, polyamides, polystyrenes, polyisoprenes, polycarbonates, polyesters, polyacrylates, polyurethanes from vinyl polymers, amorphous silica, amorphous silica gel, precipitated silica, pyrolyzed silica, aluminosilicates such as zeolites and alumina, silicates, carbonates, and mixtures thereof. Preferred water-releasable matrix materials include cyclodextrin complexes, silicates, silicas, carbonates and starch-based materials.
In a further embodiment, the articles comprise one or more microcapsules that comprise active agents. The one or more microcapsules comprising active agents can be incorporated into the composition that is manipulated to form the article. Microcapsules comprising the active agents can be incorporated into the coating that is on surfaces. In one embodiment, the coating that is on the surface comprises from about 10% to about 100% of one or more microcapsules comprising active agents, in another embodiment from about 25% to about 100%, and in yet another embodiment from about 40% to about 100%. Except where otherwise indicated, the terms "perfume nanocapsule" and "microcapsule" fall within the scope of the term "perfume microcapsule".
Microcapsules can be formed by various procedures including, but not limited to, coating, extrusion, spray drying, and interfacial, in-situ, and matrix polymerization. Possible capsule materials vary widely in their stability to water. Among the most stable are polyoxy methylene urea (PMU) based materials, which can keep certain agents active even for long periods in an aqueous solution (or a product). Suitable microcapsules may include those described in the following references: US patent applications nos.: 2003/0125222 A1; 2003/215417 Al, 2003/216488 Al, 2003/158344 Al, 2003/165692 Al, 2004/071742 Al, 2004/071746 Al, 2004/072719 Al, 2004/072720 Al, 2006/0039934 Al, 2003/203829 Al, 2003/195133 Al, 2004/087477 Al, 2004/0106536 Al; and US patents: 6,645,479 Bl; 6,200,949 Bl; 4,882,220; 4,917,920; 4,514,461; 6,106,875, 4,234,627, 3,594,328 and US RE 32713.
In one embodiment, the articles can comprise chemical foaming agents. These agents can be processing aids to form the articles or enhance the performance of the active agent in the articles. Chemical foaming agents can be exothermic (heat released through foaming) or endothermic (heat absorbed during foaming): The endothermic chemical foaming agent can be useful during fiber formation to absorb heat and foam to provide fibers with lower density. Some suitable non-limiting examples of endothermic foaming agents include sodium bicarbonate, citric acid and its derivatives, and combinations thereof, which begin to emit gas (mostly carbon dioxide) to foam at around 120°C. Some non-limiting examples of exothermic chemical foaming agents include azodicarbonamide (ADC), 4,4'-oxybis(benzol-sulfonylhydrazide)-, '5-phenyltetrazole, p-toluilensulfonyl-semicarbazide, p-toluilensulfonyl-hydrazide, and combinations thereof. These exothermic chemical foaming agents become active (mostly emit nitrogen gas to form foam) at temperatures above 100°C and release heat (exothermics), which may need to be removed by cooling or other means. When used as a processing aid to form articles, selection of the appropriate chemical foaming agent is highly dependent on specific application conditions and requirements, specifically, the composition of the processing mix and the process conditions and control. It is desirable for the chemical foaming agent to completely decompose and be held in the processing mixture fluid solution until the fluid mixture exits the matrix or nozzle. Then, the gas must be allowed to expand into the solid phase in the article. Gas can escape from the article to form open cell fibers or it can remain trapped. Hydrocerol® (available from Clariant Masterbatches, Holden, Massachusetts, USA), Tracei® (available from Tramaco, Pinneberg, Germany), and OnCap™ (available from poliOne, Avon Lake, Ohio, USA) are some non-limiting examples of commercially available chemical foaming agents. Defoamers may be added to the article after the gas from the chemical foaming agents has been released so that the chemical foaming agent left in the article does not interfere with the performance of the article, such as during use. D. Product form
The article may be produced in any of a variety of product forms, including articles used alone or in combination with other consumer product components. of product intended for the consumer.
The article may be in the form of one or more flat sheets or plates of a suitable size so that it is capable of being easily handled by the user. This article can be square, rectangular, disk, or any other suitable format. The plates may also be in the form of a continuous strip including a dispenser applied over a cylinder-shaped tape with individual portions dispensed through perfutations and/or a cutting mechanism. Alternatively, the articles are in the form of any other shaped object.
The article may comprise one or more textured, corrugated or otherwise topographically shaped surfaces, including letters, logos or figures. The textured article preferably results from the shape of the article, in which the outermost surface of the article contains portions that are elevated relative to other areas of the surface. Raised portions may result from the shape of the formed article, for example the article may be originally formed into a wavy or waffle texture. The raised portions can also be the result of processes of: creping, printed coatings, embossing patterns, lamination to other layers that have raised portions, or the result of the physical form of the article itself. Texturing can also be the result of laminating the 1 article to a second article that is textured.
In a particular embodiment, the article may be perforated with holes or penetrating channels to or through the article. These perforations can be formed as part of the mat production process through spikes that extend from the surface of a belt, drum, adjacent roller, or other surface. Alternatively, these perforations can be formed after the mat manufacturing process through holes or jabs in the articles with pins, needles or other sharp objects. These perforations can be numerous by surface area, but not so much as to sacrifice the physical integrity or appearance of the article. It has been found that such perforations can increase the rate of dissolution of articles in water relative to non-perforated articles. E. Product Types
Some non-limiting examples of product type modalities for use by the article and methods include personal care articles, oral care articles, personal health care articles, home care articles, and other cleaning articles. Some non-limiting examples of personal care articles include hand cleaning substrates, hair shampoo, hair conditioner, hair color treatment substrates, facial cleaning substrates, body cleaning substrates, shaving or waxing preparation substrates, substrates for pet care, personal care substrates containing pharmaceutical active or other skin care active, wetting substrates, sunscreen substrates, chronic skin benefit agent substrates (eg substrates containing vitamin, substrates containing alpha-hydroxy acid, etc.), deodorizing substrates, anti-acne substrates, wrinkle treatment substrates and combinations thereof,• fragrance-containing substrates and combinations thereof. Some non-limiting examples of oral care items include tooth cleaning items, tooth whitening items, dental care items, periodontal gum care items, denture cleaning items, tongue cleaning items, refreshing items breath, fluorine-containing articles, mouthwash articles, anti-cavity articles and combinations thereof. Some non-limiting examples of healthcare articles include pharmaceutical drug containing form articles, over-the-counter drug containing dosage form articles, probiotics containing articles, bactericidal substrates, fungicidal substrates, anesthetic substrates, health care substrates wound, analgesic substrates, antiseptic substrates, anti-inflammatory substrates and combinations thereof. Some non-limiting examples of home care articles include fabric care substrates, dish care substrates, hard surface cleaning substrates, automotive care substrates, fabric fragrance delivery substrates, fabric softener substrates, cleaning substrates for laundry, fabric stain removal substrates, anti-wrinkle fabric substrates, static control fabric substrates, instant fabric stain removal substrates, automatic dishwasher cleaning substrates, and more. II. Production method >
The article may be prepared by the process comprising: (1) preparing a processing mixture comprising active agent(s), dissolved polymer builder(s), plasticizer(s) and other optional ingredients; (2) fibrillating the processing mixture forming fibers by a film fibrillation process comprising a pressurized gas stream directed against a liquid film of the premix to form the fibers and partially drying the fibers by another or the same stream of pressurized gas; (3) depositing the partially dried fibers onto a surface to form a mat in one or more desired shapes to form one or more partially dried shaped articles; and (4) optionally drying the partially dried shaped article to a final desired moisture content (eg, from about 0.5% to about 15% moisture, by adding energy). Optionally, a coating that is on the surface can be applied to the article. The coating that is on the surface can be applied over the surface of fibers when the fibers are on their way to the collector before forming a mat or after the mat has been dried, as explained later in the coating that is on the surface. A. Preparation of the processing mix'
The processing mix is generally prepared by dissolving the polymeric builder in the presence of water, active agent(s), plasticizer, • surfactant and other optional ingredients by heating followed by cooling. This can be achieved through any heated batch agitation system or through any suitable continuous system involving single screw or double screw extrusion or heat exchangers associated with high shear or static mixing. Any process can be envisioned such that the polymer is ultimately dissolved in the presence of water, active agent(s), plasticizer and other optional ingredients, including stepwise processing through premix portions of any combination of ingredients. .
Processing mixtures can comprise: from about 15% to about 60% solid, in one embodiment, from about 20% to about 55% solid, and in another embodiment, from about 25% to about 50% solid, by weight, of the processing mixture prior to fiber formation; and have a viscosity of about 5,000 centipoise to about 150,000 centipoise, in one embodiment from about 10,000 centipoise to about 125,000 centipoise, in another embodiment from about 15,000 centipoise to about 100,000 centipoise, in another embodiment of about from 20,000 centipoise to about 75,000 centipoise, and in yet another modality from about 25,000 centipoise to about 60,000 centipoise.
The % solids content is the sum of the percentages by weight of the total processing mixture of all solid components, and liquids without water and any obviously volatile materials such as low boiling alcohols. Process mix viscosity values are measured using a TA Instruments AR500 rheometer with a 4.0 cm diameter parallel plate and range from 1,200 microns at a shear rate of 1.0 second reciprocal over a period of 30 seconds at 23°C. B. Fiber formation from the processing mixture
Fibers can be formed by many processes including, but not limited to, the blow spinning process, continuous spinning processes, carded filament mat processes, melt fibrillation and electrospinning and combinations thereof. The method for producing the fibers can include a single-step fibrillation process. Single-step fibrillation processes used for thermoplastic polymers include melt blowing, melt film fibrillation, continuous spinning, melt spinning in a typical extraction/spinning process and combinations thereof.
Continuous spin fibers refer to small diameter fibers that are formed by extrusion of molten thermoplastic material as filaments of a plurality of fine usually circular capillaries of a spinner with the diameter of the extruded filaments which are then rapidly reduced as described. in US Patent Nos. 3,692,618, 3,802,817, 3,338,992, 3,341,394, 3,502,763, 3,502,538 and 3,542,615.
Fibers produced by extrusion into blocks with the passage of hot air at high velocity (meltblown) means fibers formed by extrusion of a molten thermoplastic material through a plurality of usually circular thin matrix capillaries such as strands or filaments fused in converging gas streams with high velocity that attenuate the molten thermoplastic material filaments ■ to reduce their diameter, which can be to microfiber diameter. Consequently, the fibers produced by molten blow are carried by the gas stream at high velocity and deposited on a collecting surface to form a mat of randomly distributed fibers produced by molten blow. Such a process is disclosed in US Patent No. 3,849,241.
Methods for producing fine fibers further comprise melt fibrillation and electrospinning. Fused fibrillation is a general class of fiber production defined by the fact that one or more polymers are fused and extruded into various possible configurations (eg co-extrusion, homogeneous or bicomponent films or filaments) and then fibrillated or converted into filaments. Blown wiring is a specific method (as described in this document). Fused film fibrillation is another method that can be used to produce fibers. A molten film is produced from the molten material, and then a fluid is used to form fibers from said molten film. Examples of this method include US Patent Nos. 6,315,806, 5,183,670 and -4,536,361, to et al., and US Patent Nos. 6,382,526, 6,520,425 and 6,695,992, to Reneker et al. and attributed to the University of Akron. The process according to Torobin uses one or an arrangement of coagulating nozzles to form a fluid film that is fibrillated by high-velocity air flowing within this annular film. Other melt film fibrillation methods and systems are described in US Patent Nos. 7,666,343 and 7,931,457 to Johnson, et al., US Patent No. 7,628,941 to Krause et al. and U.S. Patent No. 7,722,347 to Krause, et al., and provide narrow and uniform fiber distribution, reduced or minimal fiber defects such as non-fiber polymer fusion (generally called "strips"), bounce and dust, by example. These methods and systems additionally provide uniform non-woven mats for absorbent toiletries.
Electrospinning is a commonly used method of producing submicrometer fibers. In this method, typically, a polymer is dissolved in a solvent and placed in a sealed chamber at one end and with a small opening in a neck-down portion at the other end. A high voltage potential is then applied between the polymer solution and a collector near the open end of the chamber. The production rates of this process are very slow and the fibers are typically produced in small quantities. Another spinning technique for producing submicron fibers is solution or fast spinning, which uses a solvent.
There is a distinct difference between diameter fibers made with electrospinning versus those made with molten fibrillation, namely the chemical composition. Submicron electrospinning fibers are produced from generally soluble polymers of lower molecular weight than fibers made by melt fibrillation. Commercially viable electrospinning methods have been described in US Patent No. 7,585,437, to Jirsak et al., US Patent No. 6,713,011 to Chu et al., US Patent Publication No. 2008/0237934, to Reentre et al. US Patent Publication 2008/0277836 and 2008/0241297, to Park, and Patent Publication No. 2009/0148547, to Petas et al.
In one embodiment, a form of the cast film fibrillation process is used. In general, this process involves providing a thermoplastic polymeric melt, using a pressurized gas stream to impinge on the polymeric melt to form multiple fine fibers. Suitable deep-film fibrillation methods are described in, for example, U.S. Patent Nos. 4,536,361, 6,315,806 and 5,183,670 to Torobin; US Patent Nos. 6,382,526, 6,520,425 and 6,695,992 to Reentre; US Patent No. 7,666,343 to et al; US Patent No. 7,628,941 to et al, and US Patent Publication No. 2009/0295020, to Krause, et al, published December 3, 2009, all incorporated herein by reference in their entirety. Cast film fibrillation methods may use different processing conditions. The method of Torobin and Reentre more specifically includes the steps of feeding molten polymer material into an annular column and forming a film or tube at the outlet of the annular column in which a gas jet space is formed. ‘ A gas column then supplies pressures on the inner circumference of the polymeric film. When the polymeric molten material film leaves the gas jet space, it is shredded into many small fibers, including due to the central expansion gas.
While the cast film fibrillation • methods, included as reference above, describe the use of thermoplastic film cast material, it was surprising and unintuitive to find that a film fibrillation method can be used to produce fibers from mixing fluids. processing. Specifically, as used, a fluid film fibrillation process comprises a pressurized gas stream that flows within a confined gas passage, which comprises upstream converging wall surfaces and downstream divergent wall surfaces in which the fluid is mixing Processing is introduced to provide a fluid film of. processing mixture extruded onto a heated wall surface which is impacted by the gas stream flowing within the gas passage, effective to fibrillate the film of process mixture fluid forming fibers. "Converging" means that the cross-sectional area decreases in the direction of gas flow; and "divergent" means that the cross-sectional area increases in the direction of gas flow. In one embodiment, the gas passage comprises a first upstream section in which gas enters from a supply end, a transition region, and a second downstream section in which gas flows to an outlet end. that the transition region fluidly connects the first section to the second section, and the gas passage ends at the outlet end of the second section. In a particular embodiment, the first section of the gas passage has a monotonously decreasing cross-sectional area from the supply end to the transition region, and the second section of the gas passage has; a monotonically increasing cross-sectional area from the transition region to the exit end of the second section. At least one flowing stream of process mixture fluid is transmitted through at least one enclosed passageway which terminates in at least one opening in at least one of the opposing heated walls. The processing mixing fluid is heated sufficiently in transit to make and maintain this flowable introduced into the gas passage. Each stream of processing mixing fluid is encased in the form of a film from each opening. Each film of processing mixing fluid - extruded joins with the gas stream and the film; of processing mixture fluid is fibrillated to form fibers exiting the outlet end of the second section of the gas passage. For purposes of the present invention, "area •. in monotonically decreasing cross-section" means "area in strictly decreasing cross-section" from the upper end (inlet) to the lower end of the upstream nozzle section, and "area in monotonically increasing cross-section " means "a strictly increasing cross-sectional area" from the top end to the outlet end of the section downstream of the nozzle.
In a particular embodiment, each extruded film of processing mixing fluid joins with the gas stream in the second section of the gas passage. Introducing the processing mixing fluid into the second section of the nozzle system on a heated divergent support wall specifically facilitates the production of high quality fibers and resulting mats. In a further embodiment, the location where the extruded processing mixing fluid film joins with the gas in the second downstream section in order to produce the best quality fibers and mats depends on the type of gas, the geometry of the nozzle, including angles and transitions and gas pressure, and may be located in the upper half of the second section as for low gas pressure conditions and may be located in the lower half downstream of the second section as for high gas pressure conditions. In a particular embodiment, only a film of processing mixture fluid forms on at least one of the heated walls, the gas pressure exceeds about 0.069 MPa (10 psi), and each processing mixture passage opening from the which the processing mix film is extruded is situated in a second half downstream of the second section between the transition region and the exit end of the second section. It was concluded that the second half of the second downstream section can provide an ideal gas velocity region where fluid film fibrillation is performed very efficiently,' producing superior quality fibrous product.
For the purposes of this description, the enclosed passages for pressurized gas and processing mixing fluid together will be called 1 "nozzle" or "nozzle system". The nozzle may have passageways enclosed in rectangular slit configurations or round configuration, elongated oval configuration, or any configuration that would allow the formation of one or more films of processing mixture fluid to collide by one or more streams of pressurized gas. In particular, for a rectangular slit configuration, one or more pressurized gas streams may flow through a delimited rectangular slit passage to collide with the film of processing mixture fluid that forms on a rectangular wall surface to form the fibers of the processing mixture. In such a rectangular slit configuration, the enclosed passage for one or more processing mixing fluids may be circular, elongated oval, rectangular slit or any other shape.
An example of a circular nozzle and a slit nozzle for fluid film fibrillation method is further illustrated in figures 1 and 2 respectively. These preferred embodiments illustrate a nozzle 7, 20 with orifice 7a which forms the fibers 17. The process more specifically includes the steps of heating the processing mixing fluid 2 and forming a liquid film 9 along an orifice 7a. The processing mixing fluid will contain the water-soluble polymer and any other desired ingredients. The processing mixing fluid 2 is extruded through an orifice 7a, which in turn. instead, it contains a pressurized gas stream 10 such that the processing mixing fluid 2 is extruded as an elongated film 12. Orifice 7a can be part of a nozzle 7 and nozzle 7 can be optimized for process stability. A fibrillation fluid stream 10, such as a pressurized gas stream, is blown to form an elongated film 12. The fibrillation fluid stream 10 will then provide pressure on the inner surface (fibrillation fluid stream together) of the film. elongated 12. Weakened or thin-walled portions may be formed in film 12 to more easily and controllably allow the formation of fibers including nanofibers 17. Weakened portions may result from notches or projections located on the outer surface of the jet 10 or on the inner surface of the processing mixing fluid extrusion port 7a. Weakened portions can also result spontaneously due to local surface pressure in the fluid film and/or fluid film flow rate differences along the perimeter of the film. The elongated processing mixing fluid film 12 is then subjected to a fluid to form a multiplicity of fibers 17. This fluid can be pressurized gas stream 10 or an incoming fluid 14 or any fluid stream. The incoming fluid 14 is transverse jet 13. If advantageous, a nozzle 18 which supplies heating or cooling fluid 19 to the formed fibers 17 can be used.
Processing mixture 2 is typically heated to form a liquid and easily flowable. The processing mixing fluid 2 may be at a temperature of from about 0°C to about 150°C, in one embodiment from about 10°C to about 120°C, and in another embodiment from about 20 °C to about 100 °C. The temperature of polymer 2 depends on the composition of the processing mixing fluid. The heated processing mix fluid 2 is at a pressure of from about 0.10 MPa (15 psia) to about 1.52 MPa (220 psia), or preferably from about 0.14 MPa to about 1, 03 MPa (about 20 psia to about 150 psia), or more preferably from about 0.17 MPa to about 0.69 MPa (25 psia to about 100 psia).
In some cases, the process mixture fluid film may coalesce immediately after formation. In the case of the coalesced film, it may be preferable to have thin walls or weakened portions in the film to aid fibrillation. Some non-limiting examples of fibrillation fluid are gases such as nitrogen or, in another embodiment, air or any other fluid compatible (defined as reactive or inert) with the processing mixture composition. The fibrillation fluid 10 may be at a temperature close to the temperature of the heated processing mixing fluid 2. The temperature of the fibrillation fluid 10 may be a temperature higher than the heated processing mixing fluid 2 to aid in the flow of the fibrillation fluid. processing mixture 2 and fluid film formation 9. Alternatively, the temperature of the fibrillation fluid 10 may be below the temperature of the heated processing mixture fluid 2. In one embodiment, the temperature of the fibrillation fluid is about 100°C. °C above the heated processing mixing fluid 2, in another embodiment about 50°C above the heated processing mixing fluid 2, or exactly the temperature of the heated processing mixing fluid 2. fibrillation 10 is sufficient to fibrillate the processing blend fluid forming fibers 17 and is above the pressure of the heated processing blend fluid as it is extruded out of the orifice 7a.
The fibrillation fluid 10 can have a velocity of more than about 200 meters per second at the fibrillation site of the film. In one embodiment, at the film fibrillation site, the fibrillation fluid velocity will be greater than about 300 meters per second, ie, transonic velocity; In another modality, more than about 330 meters per second, that is, sonic velocity; and in yet another modality from about 350 to about 800 meters per second, that is, supersonic speed. The fibrillation fluid may be pulsating or it may be of steady flow.
The yield of the processing mixing fluid 2 will depend primarily on the specific processing mixing fluid used, the nozzle design, and the temperature and pressure of the processing mixing fluid. The yield of processing mixing fluid 2 will be greater than about 1 gram per minute per orifice, for example, in a circular nozzle illustrated in Figure 1. In one embodiment, the yield of processing mixing fluid will be greater than about 10 grams per minute per hole and in another modality greater than about 20 grams per minute per hole, and in yet another modality greater than about 30 grams per minute per hole. In a slit nozzle embodiment, as illustrated in Figure 2, the processing mixture fluid yield will be greater than about 0.5 kilogram per hour per meter width of the slit nozzle. In another slit nozzle modality, the processing mixing fluid yield will be greater than about 5 kilograms per hour per meter of slit nozzle width, and in another slit nozzle modality, the fluid yield of processing mixture will be greater than about 10 kilograms per hour per meter of slot nozzle width, and in yet another mode of slot nozzle, the processing mixing fluid yield will be greater than about 20 kilograms per hour per meter width of the slit nozzle. In certain slit nozzle embodiments, the processing mixing fluid yield can exceed about 40 kilograms per hour per meter of slit nozzle width. There will likely be several holes 7a operating at the same time which further increases the total production throughput. Efficiency, together with pressure, temperature and velocity are measured at the die orifice outlet for circular nozzles 7a and at slits 20.
Fiber fibrillation can occur before the fibers and fluid exit the orifice. Once the elongated film exits the hole, fibers are formed.
Fiber formation commonly occurs immediately upon exiting the orifice. One or more streams of fluid can be used to form the multiplicity of fibers. The pressurized fluid or gas stream 10 can be the fluid stream that joins the process mixing fluid film, an incoming fluid, or any other fluid stream. Optionally, an incoming fluid 14 can be used to induce a pulsating or oscillating pressure field to aid in the formation of a multiplicity of fibers 17. Some non-limiting examples of the incoming fluid 14 are pressurized gas stream such as compressed air, nitrogen, oxygen, superheated stream or any other fluid compatible (defined as reactive or inert) with the processing mix composition. As shown in Figures 1 and 2, the incoming fluid 14 can be supplied by a transverse jet 13 which is situated to direct the incoming fluid flow 14 above and around the film 12 and fiber forming region 17. The incoming fluid 14 it can have a low speed or a high speed, such as near sonic or supersonic speeds. A low velocity incoming fluid will typically have a velocity of about 1 to about 100 meters per second and in a mode of about 3 to about 50 meters per second. It is desirable to have low turbulence in the incoming fluid stream 14 to minimize fiber to fiber entanglements, which usually occur due to the high turbulence present in the fluid stream. The temperature of the incoming fluid 14 can be the same as the temperature of the fibrillation fluid 10 above, or a higher temperature to aid in fiber drying, and is in the range of from about 80°C to 300°C and typically from about 100 °C to about 250 °C. The moisture content or relative humidity of the incoming fluid 14 when used as a drying fluid is very low, generally less than 20%, in another modality less than 10%, in another modality less than 5%, and in still another modality less than 1%.
Optionally, an additional fluid stream, drying or heating fluid 19, can also be used. The additional fluid stream 19 may be a pressurized gas stream such as compressed air, nitrogen, oxygen, superheated stream or any other fluid compatible (defined as reactive or inert) with the processing mixture composition. This additional fluid stream 19 is situated to direct fluid to the fibers 17 to dry the fibers. It is desirable to have low turbulence in the incoming fluid stream 19 to minimize fiber to fiber entanglements, which usually occur due to the high turbulence present in the fluid stream. If additional fluid is used as a heating or drying fluid, this is at a temperature of from about 80°C to 300°C and typically from about 100°C to about 250°C. The moisture content or relative humidity of the additional fluid stream when used as a drying fluid is very low, generally less than 20%, in another modality less than 10%, still in other modality less than 5%, and in yet another modality less than 1%. The additional fluid stream 19 can form a "curtain" or "cover" around the fibers of the processing mixture exiting the nozzle. Suitable examples of such a "curtain" or "cover" are set forth in US Patent No. 7,628,941 to Krause, et al and US Patent No. 6,382,526 and 6,695,992 to Reentre, respectively, which are incorporated in the present invention as reference in its entirety. Any fluid stream can contribute to fibrillation of the processing mixing fluid and can therefore generally be called fibrillation fluids.
The fibers of the processing mixture can be partially or completely subjected to drying on the way to the collector by any one or a combination of the fibrillation fluids - the pressurized gas stream of fibrillation fluid 10, the incoming fluid 14 or the fibrillation fluid stream. additional fluid 19. Alternatively, the pressurized gas stream of fibrillation fluid 10 or the first pressurized gas stream may be the only fluid stream used for fibrillating and partially or completely drying the fibers of the processing mixture. In such a case, the drying fluid stream is the continuation of the first fluid stream 10. Alternatively, the first fibrillation fluid stream 10 and the second incoming fluid stream 14 may be the fluid streams used for fibrillation and drying, respectively. Alternatively, the first fibrillation fluid stream 10 and the additional second fluid stream 19 may be the fluid streams used for fibrillating and drying, respectively. In a particular embodiment, the additional drying fluid stream 19 may be adjacent to the first fibrillation fluid stream 10. In another embodiment, the additional drying fluid stream 19 may be at an angle to the first fluid stream. of fibrillation 10 after exiting the mouthpiece. The angle of the additional drying fluid stream 19 may range from about 0° (parallel) to 90° (perpendicular) to the first fibrillation fluid/fluid stream 10 as it exits the nozzle. Fluid stream 19 can have a low velocity or a high velocity, such as near sonic or supersonic velocities. The additional incoming fluid stream at a low velocity will typically have a velocity of from about 1 to about 100 meters per second and in a mode of from about 3 to about 50 meters per second. One or more streams of drying fluid at least partially dry the fibers along the process mixture film. In a particular embodiment, one or more streams of drying fluid can dry the fibers to the desired moisture content of the article of about 0.5% to about 15% moisture. The temperature and moisture content of one or more streams of drying fluid can be optimized to dry the fibers to the desired moisture content by an element of common knowledge in the dry spinning technique.
After the accessory accessory fluid film has been formed, the film or fibers can alternatively be subjected to an additional process that promotes the formation of micro and nanofibers with a diameter less than about 1 micrometer. Further processing would take place immediately after the formation of the elongated film. Further processing can utilize one or more Laval nozzles to accelerate gas velocities into the sonic and/or supersonic range. When the processing mixture is exposed to these high gas velocities, it breaks up into a multitude of fine fibers. Examples of a Laval nozzle are described in Nyssen et al., US Patent No. 5,075,161 (included herein as a reference in its entirety), in which a method of breaking polyphenylene sulfide molten material into thin filaments is presented. The Laval nozzle can be positioned right after the nozzle when the elongated film and processing mix are produced. Alternatively, the Laval nozzle could be positioned just after the fibers have been formed to further reduce fiber size. Fibers can be produced by subjecting the processing mix streams to extraction and extruding them into a gaseous medium that flows essentially parallel to the processing mix streams and achieves sonic or supersonic velocity. Simultaneous deformation and cooling generate fine or extremely fine fibers of finite length. The spinning speed, temperature and position of the Laval nozzle are properly configured to achieve the desired fineness and dryness of the fibers.
Various processes and a combination of processes can be used to produce the blankets described here. Fiber firing, as shown in U.S. Patent No. 7,326,663 to Sodemann et al., can be combined with fluid film fibrillation here debris in two separate bundles in a single line. Various aspects of fiber disruption can be incorporated into fluid film fibrillation, such as producing fibers of different strengths and diameters to provide a desired combination of properties. Alternatively, fluid film fibrillation aspects can be included in other fibrillation processes to increase the throughput rate through the use of fluid film fibrillation to form fibers. For example, the fluid film fibrillation process described herein could be modified to include a Laval nozzle to assist in extracting the fibers. Extraction can aid in further attenuation of the fibers.
The fibers described herein can also be produced by other spinning methods that typically produce fibers from. Such methods include electrospinning, electroblowing and fast spinning. In general, electrospinning employs an electrostatic force to extract a charged liquid polymeric formulation from a source to a collector. An electrostatic field is used to accelerate the liquid formulation from the source to the collector where the fibers are collected. Non-limiting and suitable examples of electrospinning methods for producing fibers as described in the present invention have been described in US Patent No. 7,585,437, to Jirsak et al., US Patent No. 6,713,011 to Chu et al., patent publication US 2008/0-237 934, to Reentre et al, US patent publication numbers 2008/0277836 and 2008/0241297, to Park, US patent publication no. 2009/0148547, to Petas et al, and US patent publication no. 2006/0264130, by Parles, et al.
The electroblowing method comprises feeding a polymer solution to a spinning nozzle to which a high voltage is applied while the compressed gas is used to envelope the polymer solution in a forward gas stream as it exits the nozzle, and collecting the mat. resulting nanofiber in a grounded suction manifold. Suitable, non-limiting examples of electroblowing methods, included herein by reference in their entirety, comprise US Patent No. 7,582,247 to Armantrout et al, US Patent No. 7,585,451 to Bryner et al, US Patent No. 7,618,579 of Kim et al, US Patent Publication No. 2006/0097431 of, US Patent Publication No. 2006/0012084 of et al, and US Patent Publication No. 2005/0073075 of Cu et al.
Another process for producing fibers described herein is fast spinning, described in U.S. Patent No. 3,081,519 to Buckets and White (non-limiting example). In the fast spinning process, a polymer solution at a temperature above the boiling point of the solvent and at a pressure at least autogenous is extruded into a medium of lower temperature and substantially lower pressure. The sudden boiling that occurs at this point causes fibrillated structures or networks to form. Fibrillated materials tend to form when pressure changes are more severe or when more dilute solutions are used. Under these circumstances, the vaporizing liquid within the extrudate forms bubbles, cracks through the confinement walls, and cools the extrudate, causing solid polymer to form therefrom. The resulting multifibrous strand has a fine internal structure or morphology characterized as a three-dimensional integral plexus that consists of a multiplicity of interconnecting, random length, essential longitudinally extended fibrous elements, called film fibrils. These film fibrils are shaped like thin strips of a thickness typically less than 4 micrometers. Other suitable, non-limiting examples of the fast spinning process, included herein by reference in their entirety, include US Patent Nos. 5,977,237 and 5,250,237 to Shin et al, US Patent No. 5,788,993 to Bryner et al, US Patent No. 6,638,470 to Schweiger, US Patent No. 4,260,565 to D'Amico et al, and US Patent No. 7,118,698 to Armantrout et al.
In a particular embodiment, the processing mixture can be spun in submicron (diameter less than about 1 micrometer) or microfiber (diameter in the range of about 1 micrometer to about 10 micrometers) using methods selected from the group of fluid film fibrillation, melt fibrillation, electrospinning, electroblowing, fast spinning or combinations thereof.
The above methods, such as fluid film fibrillation, fiber disruption, electrospinning, or electroblowing, produce a significant number of dissolvable fibers with an average diameter less than about 1 micrometer, or submicron fibers. In one embodiment, the article comprising the article may have at least 25% of all dissolvable fibers having an average diameter less than about 1 micrometer, in another embodiment at least 35% of all dissolvable fibers having an average diameter less than about 1 micrometer. than about 1 micrometer, in another embodiment at least 50% of all dissolvable fibers with an average diameter less than about 1 micrometer, and in yet another embodiment at least 75% of all dissolvable fibers with an average diameter less than about 1 micrometer. -However, it may be desirable that a particular article produced by the methods described herein is such that the methods are optimized to produce a significant number of dissolvable fibers with an average diameter less than about 150 micrometers, in a modality of less than about 100 micrometers , in another modality smaller than about 10 micrometer, and yet another modality smaller than about 1 micrometer with a relative standard deviation smaller than 100%, alternatively smaller than 80%, alternatively smaller than 60%, alternatively smaller than 50%, as in the range of 10% to 50%, for example. As mentioned earlier in this description, the significant number means at least 10% of all dissolvable fibers, in one mode at least 25% of all dissolvable fibers, in another mode at least 50% of all dissolvable fibers, still another modality is at least 75% of all dissolvable fibers. C. Formation of the fibrous blanket structure
Fibers partially dried or dried to the desired moisture content of the processing mix are laid in a manifold to form a mat. The collector is typically a conveyor belt or drum. The collector can be porous and vacuum can be applied to provide suction to aid fiber settlement in the collector. The distance between the orifice and the collector, commonly called the matrix to collector distance (DMC), can be optimized for the desired blanket properties. It may be desirable to use more than one DMC in a blanket, change the DMC during production, or have different beams with different DMCs. It may be desirable to form a blanket with different uniformities by changing the DMC. If the DMC is such that the fibers are not sufficiently dry before depositing in the collector, the wet or insufficiently dry fibers may coalesce to form bubbles or bundles which may not be desirable and would constitute defects. Alternatively, it may be desirable for an article to have some or all of the fibers coalesced completely or partially, for example, to have structural integrity. If the DMC is large and such that the fibers are dry enough, the fibers may intertwine or stick together, but not coalesce, to form bundles or cords that may not be desirable. Therefore, depending on the desired article, the DMC can be configured to form the fibrous batt with desirable uniformity and sufficient dryness. Alternatively, mats of desirable uniformity can be further dried to obtain the desired moisture content in the article.
Additionally, the distance from the matrix to the collector can be changed along with the vacuum below the collector to obtain the desired density of the mat. In general, the shorter DMC and/or higher vacuum provides denser mats compared to the higher DMC. At shorter DMC and/or higher vacuum, the fibers tend to be "forced" tightly by the fibrillation fluid jet and/or vacuum suction, while at higher DMC and/or lower vacuum, the fibers remain soft and hence way, the density is lower. Therefore, depending on the desired article density, it may be desirable to optimize the DMC and/or vacuum for uniformity, dryness and density.
The fibrous batts of the processing mix can be formed into a desired shape or shapes including, but not limited to (i) depositing the fibrous batt into specially designed molds comprising a non-stick and non-interacting surface including Teflon, metal, HDPE, polycarbonate, neoprene, rubber, LDPE, glass and the like; (ii) deposition of the fibrous batt in cavities printed on dry granular starch contained in a shallow tray, otherwise known as patterned starch forming technique; and (iii) deposition of the fibrous mat on a continuous mat or screen comprising any non-interacting or non-stick materials, such as Teflon, metal, HDPE, polycarbonate, neoprene, rubber, LDPE, glass and the like that can be later stamped, cut, embossed or stored in a cylinder. D. Optional drying of the processing mix fibrous mat
Optional drying of the partially dried fibrous batt formed from the processing mixture may be accomplished by any suitable means including, but not limited to (a) multi-stage in-line dryers using convection drying or forced pass drying of air; (b) superheated steam dryers; (c) drying chamber(s) including chambers with temperature and pressure control or atmospheric conditions; (d) ovens including non-convection or convection ovens with controlled temperature and, optionally, humidity; (e) truck/tray dryers, shock ovens; (f) rotary ovens/dryers; (g) in-line roasters; (h) rapid heat transfer ovens and dryers; (i) double full space roasters, and (j) conveyor dryers.
Optional ingredients can be checked during any of the processing steps described above or even after the drying process.E. Optional preparation of the coating that is on the surface comprising the active agent
The preparation of the coating that is on the surface comprising the active agent may include any suitable mechanical, chemical or other means suitable for producing a particulate composition comprising the active agent including any optional material as described in the present invention, or a coating of a fluid.
Optionally, the coating that is on the surface may comprise a water-releasable matrix complex comprising the active agent(s). In one embodiment, water-releasable matrix complexes comprising active agent(s) are prepared by spray drying, the active agents being dispersed or emulsified in an aqueous composition, which comprises the matrix material dissolved under high shear (with optional emulsifying agents) and spray dried to a fine powder. Optional emulsifying agents may include gum arabic, specifically modified starches or other surfactants as presented in the spray drying technique (see Flavor Encapsulation,' edited by Sara J. Risch and Gary A. Reineccius, pages 9, 45 to 54 (1988) , which is incorporated herein by reference). Other known methods of making water-releasable matrix complexes comprising active agent(s) may include, but are not limited to, fluid bed agglomeration, extrusion, cooling/crystallization methods and the use of transfer catalysts. to promote interfacial polymerization. Alternatively, the active agent(s) may be adsorbed or absorbed onto or combined with a • water-releasable matrix material that was previously produced by a variety of mechanical mixing media (spray drying, paddle mixers, crushing, grinding etc.)!. In one embodiment, the water-releasable matrix material in pellet or granular form or in solid-based form (and comprising any minor impurities as supplied by the supplier including residual solvents and plasticizers) can be crushed or ground into a fine powder. in the presence of the active agent(s) through a variety of mechanical means, for example, in a crusher or grinding hammer.
Where the article has a particulate coating, the particle size is known to have a direct effect on the reactive potential of the surface area of the active agents and thereby have a substantial • effect on how fast the active agent-' delivers the beneficial effect upon dilution with water. In this sense, active agents with smaller particle sizes tend to generate a shorter and faster live effect, while active agents with larger particle sizes tend to generate a slower and longer live effect. In one embodiment, the coatings that are on the surface can have a particle size from about 1 µm to about 200 µm, in another embodiment from about 2 µm to about 100 µm, and in yet another embodiment, from about from 3 µm to about 50 µm.
In some embodiments, it is useful to include inert carrier materials in the grinding process such as, for example, aluminum starch octenyl succinate under the trade name DRY-FLO® PC and available from Akzo Nobel, at a level sufficient to optimize the properties of powder flow and to mitigate adhesion or agglomeration between particles during powder production or handling. Other optional cosmetic excipients or actives, as described in the present invention, may be incorporated during or after the powder preparation process, e.g. grinding, milling, mixing, spray drying, etc. The resulting powder may also be blended with other inert powders, inert materials or other active powder complexes, and which include water absorbing powders as described in the present invention.
In one embodiment, the active agents may be surface coated with non-hygroscopic solvents, anhydrous oils and/or waxes as defined hereinafter. This may include the steps of: (i) coating the water sensitive powder with non-hygroscopic solvents, anhydrous oils and/or waxes; (ii) reducing the particle size of the active agent particulates, before, during or after a coating is applied, by known mechanical means to a predetermined size or selected size distribution; and (iii) mixing the resulting coated particulates with other optional ingredients in particulate form. Alternatively, the coating of non-hydroscopic solvents, anhydrous oil and/or waxes can be simultaneously applied to the other optional ingredients, in addition to the active agents, of the coating composition that are on the surface and with subsequent particle size reduction in accordance with the procedure described above.
Where the coating is applied to the substrate as a fluid (such as through a spray coating, a gel, or a cream), the fluid can be prepared prior to application to the substrate or the fluid ingredients can be applied separately to the substrate. such as through two or more separate steam feed components by spraying the fluid onto the substrate. F. Optional combination of the coating that is on the surface comprising the active agents with the article
Any suitable application method can be used to apply the surface resident coating comprising the active agent to the personal care article so as to form a part of the personal care article. For example, the article can have a tacky surface by drying the surface of the article to a specified water content prior to powder application to facilitate adhesion of the coating which is on the surface comprising the active agents to the article. In one modality, the article is dried to a moisture content of about 0.1% to about 25%, in one modality from about 3% to about 25%, in another modality from about 5% to about 25%. 20%, and in yet another modality from about 7% to about 15%. Alternatively, the surface of the pre-dried article can be made to reversibly absorb a desired level of atmospheric moisture prior to application of the powder in a controlled humidity environment for a specified period of time until equilibrium is reached. In one modality, the ambient humidity is controlled from about 20% to about 85% relative humidity; In 1 another modality, from about 30% to about 75% relative humidity; and in yet another modality, from about 40% to about 60% relative humidity.
In another modality, the article is placed in a bag, tray, mat or drum containing or otherwise exposed to powder and agitated, rolled, brushed, vibrated or agitated to apply and distribute the powder, by batch or in a manner continuous production. Other methods of powder application can include strainers,; powder, electrostatic coating, tribo charging, fluidized beds, powder coating guns, corona guns, drums, electrostatic fluidized beds, electrostatic magnetic brushes and/or powder spray chambers. The coating which is on the surface comprising the active agent can be applied over portions or entire regions of the outer surface of the article, and can be applied in a manner to adorn, decorate, form a logo, models, etc.
The coating that is ; on the surface comprising the active agents can be directly applied to the fibers as they are formed. Referring to Figures 1 and 2, the coating that is on the surface may be included in any one of pressurized gas streams 10, 14, or 19, or any additional pressurized gas stream added to the nozzle system. The coating which is on the surface may adhere and/or become embedded in the surface of partially or desirably dry fibers. Some non-limiting and suitable examples of application of surface coatings on fibers, included as references to the present invention in their entirety, include US Patent Nos. 7,291,300 and 7,267,789 to Chhabra and Isele, and US Patent Nos. 6,494,974 and 6,319,342' to Riddell.
Where the coating is applied to the substrate in a fluid, it is preferred that if water is present in the fluid, the water is not sufficient to cause the substrate to dissolve undesirably. In preferred embodiments, the active agent(s) to be applied as an adsorbed thin coating is an anhydrous oil or substantially anhydrous oil. Other non-aqueous solvents such as organic solvents that do not cause the substrate dissolution. Any suitable application method can be used to apply the active agents in liquid form to the article so that it forms a coating that is on the surface that is adsorbed onto at least a portion of the solid/air interface of the article as a thin film. For example, this can be sprayed, poured, applied in drops, printed, sandwiched between different articles or different portions of the same article, layered, injected, laminated or immersed. The active agent can be applied over portions or all the regions of the outer surface of the article, and can be applied to adorn, decorate, form a logo, model, etc.
To obtain the desired fibrous structure, the methods described in the present invention can be combined. In one embodiment, dissolvable fibers produced from one or more methods described herein can be mixed homogeneously or layered to perform as desired for the articles described herein. Different methods described herein can be optimized to produce dissolvable fibers with substantially or otherwise different actives or use of a particular surfactant, extensive rheology modifier, plasticizer, polymer builder, water soluble polymer or other optional or required ingredients. Yet alternatively, different methods can be optimized to produce dissolvable fibers with different dissolution rates and/or different diameter, in a particular embodiment, the submicron dissolvable fibers produced by the fluid film fibrillation method can be mixed homogeneously or layered with the dissolvable fibers produced from the fiber breakage, electrospinning or electroblowing method. In some embodiments, the dissolvable fibrous batt structure produced by one or more methods or by the same method may have a mixture of fibers having fiber diameter distributions, compositions, coatings that are on the surface, dissolution rates or combinations thereof substantially or marginally different. At the . In the case of an embodiment with a blend of fibers having significantly different fiber diameter distributions, the average fiber diameter of the different fiber diameter distributions may range from about 0.1 micrometer to about 150 micrometer.
Homogeneous blending of fibers produced by one or more methods can have an optimization performance advantage, such as reducing or speeding up dissolution rates for a particular modality of article, eg for controlled or timed release of actives. The formation of layers of fibers produced by one or more methods may have a performance advantage in varying the dissolution rate during article use, for example, certain actives or composition ingredients may need to be delivered at different times during use of the article. article, such as timed release of surfactant and conditioner, or detergent and bleach, or detergent and softener, and so on. Other advantages of blending dissolvable fibers produced by the methods described herein may be specific to a particular article.
Homogeneous mixing of fibers can be achieved during the formation of the fibrous mat structure, such as through the use of different nozzles or nozzle blocks or nozzle bundles that employ different methods in a simultaneous manner, for example, nozzles arranged in a misaligned configuration in two (flat) and/or three-dimensional, or simply dissolvable fiber streams at various angles with fiber deposition on the collector. Examples of homogeneously blended fibers that use an array of plurality of fiber producing nozzles that employ the fluid film fibrillation process are provided by. Torobin in US Patent Nos. 6,183,670 and 6,315,806, which are incorporated herein by reference in their entirety. The formation of fiber layers can be achieved during the formation of the fibrous batt structure, as nozzles of different methods arranged adjacent to each other or one after the other separated by a particular distance along the machine direction (the direction in which the conveyor belt is moving) in a continuous manner, eg nozzles in separate blocks or bundles which are arranged in a line along the machine direction. Alternatively, dissolvable fiber mat structures produced by different methods can be combined off-line in batches by layering one on top of the other before or after drying to desired moisture content. When combined as layers, the one or more dissolvable fibrous batt structures produced by one or more methods can have fibers that are substantially different in layers different from the dissolvable fibrous batt. The difference in fibers can be substantially or marginally different in diameter distributions, compositions, coatings that are on the surface, dissolution rates, porosities or combinations thereof. For example, the substantially different fiber diameter distribution of fibers in different layers can have average diameters in the range of about 0.1 micrometer to about 150 micrometer.
The article may comprise one or more dissolvable fibrous batt structures combined (e.g. laminated, layered, sandwiched, embedded and the like) with one or more other types of batt structures and/or articles as described in the Background above. Some non-limiting and suitable examples of articles that may be combined include US Patent Publication No. 2004/0048759 to Ribble et al, US Patent No. 6,106,849 to Malkan et al, US Patent Publication No. 2007/0225388 to Cooper et al, U.S. Patent No. 5,457,895 to Kearney et al, U.S. Patent Publication No. 2009/0232873 to Glenn et al, U.S. Patent No. 7,196,026 and PCT Application No. WO2001/47567 to: Di Luccio et al. al, PCT application No. WO2007/093558 to Simon et al, US patent application publication: numbers 2008/0035174, 2008/0269095, 2007/0128256 and 2007/0134304 to Auburn-Sonneville et al, US patent application publication 2006/0159730 to Simon, and US Patent Nos. 5,342,335 and 5,445,785 to Rhim. III Physical characteristics
A. Dissolution rate
The article has a dissolution rate that allows for rapid disintegration during water use application. The article dissolution rate is determined according to the two methodologies described below.
Conductivity dissolution method: In a 250 mL beaker, weigh 150 +/- 0.5 grams of distilled water at room temperature. The beaker is placed in an orbital shaker, eg a VWR model DS-500E and started at 150 RPM. A conductivity probe, for example a Model 2052 VWR connected to the VWR conductivity meter, is submerged just below the surface of the water so that the conductivity probe remains stationary with respect to the movement of the beaker and never touches the side of the beaker. 0.20 +/- 0.01 gram of the article is weighed and placed in water. Conductivity data is logged every 15 seconds for 6 minutes, then once every minute for up to 30 minutes. The final value is noted when the conductivity values stop changing or when 30 minutes have elapsed, whichever comes first. The conductivity dissolution time is taken as the time in ' seconds until the conductivity values stop changing or, at the most, in 30 minutes, whichever comes first.
The article has a conductivity dissolution time from about 100 seconds to about 1200 seconds, in another embodiment, from about 110 seconds to about 900 seconds, in yet another embodiment, from about 120 seconds to about 600 seconds , and in yet another mode, from about 130 seconds to about 300 seconds.
Manual dissolving method: 0.5 g of the article is placed in the palm of an individual wearing nitrile gloves. Quickly apply 7.5 cm3 of warm tap water (from about 30°C to about 35°C) applied to the product by syringe. Using a circular motion, the palms are rubbed in 2 steps at a time until dissolution occurs (up to 30 strokes). Undissolved material (after 30 strokes) is placed in a pre-weighed weighing vessel. The dry weight of undissolved material is measured the next day. The manual dissolution value is reported as the number of courses needed to complete the dissolution or in 30 courses maximum.
The article has a manual dissolution value of from about 1 to about 30 courses, in one modality from about 2 to about 25 courses, • in another modality from about 3 to about 20 courses, and in another modality of about 2 to about 25 courses modality from about 4 to about 15 courses. B. Foam volume
The article provides a sparkling profile as described later in this document. The foam volume assessment is performed on 59.1 g/m (15 g/10 inch) straight, virgin, and oriental hair strands that have been treated with 0.098 g of artificial liquid tallow [10 to 22% of oil. olive, 18 to 20% coconut oil, 1-8 to 20% oleic acid, 5 to 9% lanolin, 5 to 9% squalene, 3 to 6% palmitic acid, 3 to 6% oil. paraffin, 3 to 6% dodecane, 1 to 4% stearic acid, 1 to 4% cholesterol, 1 to 4% coconut fatty acid, 18 to 20% decholet-24]. The lock of hair is rinsed with 9-11 hardness water, 38°C (100°F) at 5.7 L/min (1.5 gallons/min) for 20 seconds with a shower nozzle. To test the liquid control products, 0.75 cm3 of liquid product is applied to the center of the lock, the lower portion of the hair in the lock is then rubbed into the product 10 times in a circular motion, followed by 40 back strokes forward (a total of 80 courses) . The foaming speed is noted as the number of strokes when the first foam is clearly generated during the 80 strokes. The foam from the operator's gloves is transferred to a graduated cylinder with an internal diameter of 3.5 cm and total capacities of 70 mL, 110 mL or 140 mL, depending on the total amount of foam generated ( modification in height of standard size graduated cylinders through a glass shop). The hair foam is collected by squeezing tightly and pushing down (one stroke) the lock of hair, then it is placed inside the cylinder. The total volume of foam is noted in milliliters. Three rounds are performed per test sample and the average of the three values is calculated. To test the article, 0.20 +/- 0.01 gram of product is weighed, with the aid of scissors if necessary, and applied to the swab and then an additional 2 cm3 of water is added to the product via a syringe. The foaming technique is then carried out as described for liquid products after a waiting period of 10 seconds. C. Fiber Diameter
The diameter of dissolvable fibers in a blanket sample is determined using a scanning electron microscope (SEM), an optical microscope, and image analysis software. A magnification of 200 to 10,000 times is chosen so that the fibers are properly enlarged for measurement. When using SEM, samples are diffused with a compound of gold or palladium to prevent electrical charging and vibrations of the fibers in the electron beam. A manual procedure to determine the fiber diameter is used from the image (on montior screen) taken with the , SEM or optical microscope. Using a mouse and cursor tool, the edge of a randomly selected fiber is fetched and then measured by its width (ie, perpendicular to the fiber direction at that point) to the other edge of the fiber. A scaled and calibrated image analysis tool provides the scaling to obtain an actual reading in micrometers, (μm). Several fibers are, therefore, randomly selected along the sample of the mat using a scanning electron microscope (SEM) or optical microscope. At least two specimens from the blanket (or orders within a product) are cut and tested in this way. In total, at least 100 such measurements are made and then all data are recorded for statistical analysis. The recorded data is used to calculate the mean (mean) of the fiber diameters, standard deviation of the fiber diameters, and the median of the fiber diameters. Another useful statistic is to calculate how much of the fiber population falls below a certain upper limit. To determine this statistic, the software is programmed to count how many fiber diameter results are below an upper limit and that count (divided by the total number of data and multiplied by 100%) is reported in percentage as a percentage below the upper limit, as a percentage below 1 micrometer in diameter or %-submicron, for example. The measured diameter (in microns) of an individual circular fiber is di.
In case the fibers have non-circular cross sections, the fiber diameter measurement is determined as and set equal to the hydraulic diameter, which is four times the fiber cross-sectional area divided by the perimeter of the: fiber crossover (perimeter external in the case of hollow fibers). The number mean diameter, alternatively mean diameter is calculated as,
IV. Described methods of use can be used to treat hair, hair follicles, skin, teeth, oral cavity, tissue and hard surfaces. The method for treating such consumer substrates may comprise the steps of: a) applying an effective amount of the article by hand, b) wetting the article with water to dissolve the solid, c) applying the dissolved material to the target consumer substrate as to treating, and d) rinsing the diluted treatment composition from the consumer substrate. These steps can be repeated as many times as desired in order to obtain the desired cleaning and/or treatment benefits. Alternatively, the article can be inserted into a machine (such as a washing machine or dishwasher) in a unit dose and the machine can perform the dissolution, treatment and rinsing steps. A method is provided to provide a benefit to the hair, hair follicles, skin, teeth, oral cavity, tissue and hard surfaces, comprising the step of applying a composition according to the first modality to those target consumer substrates in need of regulation.
Described herein is a method for regulating the condition of hair, hair follicles, skin, teeth, oral cavity, tissue and hard surfaces, which comprises the step of applying one or more compositions described herein to those target consumer substrates in need of regulation.
The amount of composition applied, frequency of application and period of use will vary widely depending on the purpose of application, the level of components of a given composition and the level of regulation desired. For example, when the composition is applied to the treatment of the whole body or hair, effective amounts will generally range from about 0.5 grams to about 10 grams; in one embodiment, from about 1.0 gram to about 5 grams; and, in yet another embodiment, from about 1.5 grams to about 3 grams. V. Commercial article
Described herein is a commercial article comprising one or more compositions described herein, and a communication directing a consumer to dissolving the article and applying the dissolved mixture to hair, hair follicles, skin, teeth, oral cavity, tissue; and hard surfaces to produce a cleaning effect, a benefit to the target consumer substrate, a fast foaming, a quick rinse foam, a clear rinse foam and combinations thereof. Communication can consist of printed material attached directly or indirectly to the packaging containing the composition, or to the composition itself. Alternatively, the communication can be an electronic or telecommunications message that is associated with the article of manufacture. Alternatively, the communication may describe at least one possible use, capability, distinguishing feature and/or property. of the article of manufacture. 5 VI. Examples
The following examples describe and demonstrate, in more detail, the modalities described here. The examples are provided for illustrative purposes only and should not be considered as a limitation, as many variations of the same are possible without departing from the character and scope of the invention. All exemplified amounts are weight concentrations of the total composition, i.e., weight/weight percentages, unless otherwise noted. Example 1: Preparation of shampoo or body wash article by a continuous spinning process The following liquid processing composition of surfactant/polymer is prepared according to the percentages by weight indicated, as described in table 1 below.

1 Sigma-Aldrich Catalog No. 363081, Molecular Weight 85.DOO-124,000, 87-89% Hydrolyzed 2 McIntyre Group Ltd, University ParK, IL, USA, Mackam HPL-28ULS3 UCARE™ Polymer LR-400, available from Amerchol Corporation ( Plaquemine, Louisiana, USA)
A target weight of the above composition is prepared using a conventional overhead stirrer (IKA® RW20DZM Stirrer available from IKA® Works, Inc., Wilmington, DE, USA) and a hot plate (Corning Incorporated Life Sciences, Lowell, MA, USA ) . In a clean, properly sized container, distilled water and glycerin are added with stirring at 100 to 150 rpm. The cationic polymer, when present, is then slowly added with constant agitation until homogeneity is achieved. The polyvinyl alcohol is weighed into a suitable container and slowly added to the main mixture in; small increments with the use of a spatula while continuing to stir, taking care to avoid the formation of visible lumps. Mixing speed is adjusted to minimize foaming. The mixture is slowly heated to 80°C and then the surfactants are added. The mixture is then heated to 85°C during stirring and then allowed to cool to room temperature. An additional amount of distilled water is added to compensate for the loss of water to evaporation (based on the original tare weight of the vessel). ■Final pH is between 5.2 - 6.6 and adjusted with citric acid or dilute sodium hydroxide if necessary. The viscosity of the resulting processing mixture is measured.
The processing mixture was processed through a four hole continuous spinning fiber spinning support, which comprised a heated spinning package at the end of which a spinning head with four holes with trilobal shape was fixed therein, three of these were capped with graphite (see figure 4A) . The processing mixture was heated to 93°C (200°F) in a hot-melt tank and pumped through a hose to the four-hole wiring package, adjusted to 97°C (207°F), via a plate adapter (figure 4A) . The processing mix was then extruded out of the spin package through the single open hole in the spin head. A hot air supplied air amplifier was available as needed for use to simultaneously extract and dry the extruded fiber. The mass yield of the premix was controlled by the speed of the hot-melt pump. Fibers containing surfactant were correctly made with widths in the range of 3 to 10 microns (figure 4B). Importantly, these fibers were shown to dissolve within less than one second of contact with water (figure 4C).
This example demonstrates the successful spinning of surfactant fibers from the above processing blend composition employing a continuous spinning approach. Surfactant fibers were prepared from a processing blend comprising 36% solids (35,400 cps) and the resulting solid fibers had the following estimated compositional parameters (assuming 0% moisture for ease of computing purposes — Note: Expect -if the actual humidity level varies in the range of 5% and 15% depending on the relative humidity 5 in a laboratory installation):

Example 2: Preparation of solid dissolvable fibrous shampoo or article for body wash through a fluid fibrillation process
The following processing composition is prepared at the indicated weight percentages as described in Table 2 below.

1 Sigma-Aldrich Catalog No. 363081, Molecular Weight 85,000-124,000, 87-89% Hydrolyzed 2 McIntyre Group Ltd, University Park, IL, USA, Mackam HPL-28ULS3 UCARE™ LR-400 Polymer, available from Amerchol Corporation (Plaquemine, Louisiana, USA) 4 PM average 8,000,000, available from Sigma Aldrich, catalog number 372838
A target weight of the above composition is prepared using a conventional overhead stirrer (IKA® RW20DZM Stirrer available from IKA® Works, Inc., Wilmington, DE, USA) and a hot plate (Corning Incorporated Life Sciences, 5 Lowell, MA, USA). In a clean, properly sized container, distilled water and glycerin are added with stirring at 100 to 150 rpm. The cationic polymer and the poly(ethylene oxide) are then leptally added with constant stirring until homogeneous. The polyvinyl alcohol is weighed into a suitable container and slowly added to the main mix in small increments using a spatula while continuing to stir, taking care to avoid the formation of visible lumps. Mixing speed is adjusted to minimize foam shape. The mixture is slowly heated to 80°C and then the surfactants are added. The mixture is then heated to 85°C while stirring, and then allowed to cool to room temperature. An additional amount of distilled water is added to compensate for water loss through evaporation (based on the original tare weight of the container). The final pH is between 5.2 and 6.6 and adjusted with citric acid.
A hot melt tank was used to pump the heated processing mixture through a single-hole fluid film fibrillation nozzle system, keeping the process parameters mentioned below constant:

Air temperature, air pressure and die-to-collector distance (DMC) were varied to assess their impact on the spinning of the fiber processing mixture. The application of heated air produced significantly better results than room temperature air. For an air temperature range of 32°C to 204°C (89°F to 400°F), fiber formation quality was better at 204°C (400°F). The upper air pressure (100 ys. 0.57 MPa (86 psi) ) was also better for spinning. At a DMC of about 75 mm, the air velocity in the collection was high enough to widen the fibers containing the surfactant, causing them to agglomerate them in thick columns in the collection drum. When the DMC was increased to 130 mm, this effect was eliminated, and the laying uniformity of surfactant fibers was significantly improved. This example demonstrates the successful spinning of surfactant fibers from the above processing blend composition that employs a fluid film defibrillation approach . A scanning electron microscopy (SEM) image of the surfactant fibers is shown in Figure 3. The surfactant fibers were prepared from a processing mixture comprising 52.1% solids (and the resulting solid fibers had the following estimated compositional parameters assuming 0% humidity for ease of computation purposes -- Note: The actual humidity level is expected to vary in the range of 5% and 15% depending on the relative humidity in a laboratory facility):

The dimensions and values presented in the present invention are not to be understood as being strictly limited to the exact numerical values mentioned. Rather, unless otherwise specified, each of these dimensions is intended to mean both the mentioned value and a range of functionally equivalent values around that value. For example, a dimension displayed as "40 mm" is intended to mean "about 40 mm".
Each of the documents cited in this invention, including any cross-reference, related patent or patent application, is incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. Citation of any document is not an admission that it is technically straightforward in relation to any invention presented or claimed in this document, or that it, by itself or in any combination with any other reference or references, teaches, suggest or present any such invention. In addition, if there is a conflict between any meaning or definition of a term mentioned in this document and any meaning or definition of the same term in a document incorporated by reference, the meaning or definition ascribed to that term in this document shall take precedence.
While particular embodiments of the present invention have been illustrated and described, it should be apparent to those skilled in the art that various other changes and modifications can be made without departing from the character and scope of the invention. Therefore, it is intended to cover in the appended claims all such changes and modifications that fall within the scope of the present invention.

权利要求:
Claims (8)
[0001]
1. Personal care article, comprising a dissolvable fibrous blanket structure, characterized in that it is selected from the group consisting of hand cleaning substrates, hair shampoo, hair conditioner, face cleaning substrates, body cleaning substrates, substrates for shaving preparation and in that the fibers are formed from a composition (processing mix) comprising: a. 10% to 75% of an active agent, by weight of the article; b. from 10% to 70% water-soluble polymeric builder, by weight of the article; and c. from 1% to 25% plasticizer, by weight of the article; d. that the ratio of the water-soluble polymeric builder to the active agent in the fiber is 3.5 or less; wherein the active agent comprises an ionic surfactant, the ionic surfactant comprising (i) one or more Group I surfactants, wherein Group I comprises anionic surfactants, and (ii) one or more Group II surfactants, where Group II comprises a surfactant selected from the group consisting of amphoteric and zwitterionic surfactants and combinations thereof; and wherein the ratio of group I to group II surfactants is from 100:0 to 30:70; wherein the plasticizer is selected from the group consisting of polyols, copolyols, polycarboxylic acids, polyesters and dimethicone copolyols wherein the total content of plasticizer is in the range of 1% to 25% by weight of the article; wherein the article is formed by means of a process comprising the steps of: e. preparing a processing mixture comprising one or more active agents, one or more water-soluble polymeric builders and one or more plasticizers, wherein the processing mixture is: (i) from 20% to 60% solids; and (ii) a viscosity of 5,000 centipoise to 150,000 centipoise; f. fibrillating the process mixture forming fibers by a fluid film fibrillation process comprising a first pressurized gas stream directed against a liquid film of the process mixture to form the fibres; g. at least partially drying the fibers of the processing mixture by a second stream of pressurized gas; h. depositing partially dried fibers onto a surface to form a batt of partially dried fibrous batt structures; i. optionally, drying the partially dried fibrous batt structure to a desired final moisture content; ej. cut the fibrous batt into one or more shapes to form the article.
[0002]
Article according to claim 1, characterized in that the dissolvable fibrous mat structure comprises fibers having an average diameter smaller than 10 micrometers.
[0003]
An article according to any one of the preceding claims, characterized in that it comprises one or more water-soluble polymeric builders selected from the group consisting of polyalkylene oxides, polyvinyl alcohols, polyacrylates, copolymers of acrylic acid and methacrylic acid, polyvinylpyrrolidones, starch and starch derivatives, pullulan, gelatin, hydroxypropylmethylcelluloses, methylcelluloses, carboxymethylcelluloses, salts and combinations thereof, preferably wherein the one or more water-soluble polymeric builders has a weight average molecular weight of from 40,000 to 500,000.
[0004]
4. An article according to any one of the preceding claims, characterized in that it comprises a plurality of dissolvable fibrous mat structures, which are bonded together through a bonding means selected from the group consisting of heat, moisture, ultrasonic , pressure and combinations thereof, such that the article has a basis weight of 30 grams per square meter to 1000 grams per square meter and a thickness of 0.25 mm to 10 mm, preferably wherein each layer of the fibrous batt structure Dissolvable comprises fibers having significantly different fiber diameter distribution, and wherein the fibers in each layer of the dissolvable fibrous batt structure have an average diameter in the range of 0.1 micrometer to 150 micrometer, even more preferably wherein each layer of the dissolvable fibrous batt structure comprises a different composition.
[0005]
5. Process for forming a personal care article selected from the group consisting of hand cleaning substrates, hair shampoo, hair conditioner, face cleaning substrates, body cleaning substrates, shaving preparation substrates, in the form of a dissolvable fibrous mat structure, characterized by comprising the steps of: a. preparing a processing mixture comprising one or more active agents, one or more water-soluble polymeric builders and one or more plasticizers, wherein the processing mixture has:i. from 20% to 60% solids by weight of the processing mixture prior to fiber formation; eii. a viscosity of 5,000 centipoise to 150,000 centipoise; b. fibrillating the process mixture forming fibers by a fluid film fibrillation process comprising a first pressurized gas stream directed against a liquid film of the process mixture to form the fibres; c. at least partially drying the fibers of the processing mixture by a second stream of pressurized gas; d. depositing partially dried fibers onto a surface to form a batt of partially dried fibrous batt structures; e. drying the partially dried fibrous batt structure to a desired final moisture content; and cut the fibrous batt into one or more shapes to form the article.
[0006]
Process according to claim 5, characterized in that the first and second pressurized gas streams are heated, preferably wherein the second pressurized gas stream is a continuation of the first pressurized gas stream.
[0007]
7. Process according to any one of claims 5 or 6, characterized in that the final desired moisture content is 1% to 15% moisture.
[0008]
Process according to any one of claims 5 to 7, characterized in that a significant number of fibers have an average diameter of less than 10,100 micrometers, preferably wherein a significant number of fibers has an average diameter of less than 10 micrometers.

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法律状态:
2018-01-16| B07D| Technical examination (opinion) related to article 229 of industrial property law [chapter 7.4 patent gazette]|

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2018-07-17| B07G| Grant request does not fulfill article 229-c lpi (prior consent of anvisa) [chapter 7.7 patent gazette]|

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2019-05-28| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|

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2021-05-04| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2021-07-13| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 30/06/2011, OBSERVADAS AS CONDICOES LEGAIS. PATENTE CONCEDIDA CONFORME ADI 5.529/DF, QUE DETERMINA A ALTERACAO DO PRAZO DE CONCESSAO. |

优先权:

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申请号 | 申请日 | 专利标题

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US36098210P| true| 2010-07-02|2010-07-02|

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US61/360,982|2010-07-02|

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PCT/US2011/042640|WO2012003349A2|2010-07-02|2011-06-30|Dissolvable fibrous web structure article comprising active agents|

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