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    • 专利摘要:
    powder composition containing water. the present invention relates to a powdery composition comprising a) at least one powder in the form of shell-core particles, the core comprising liquid water or a liquid aqueous phase and the shell comprising hydrophobic or hydrophobized particles and b) at least one powder comprising the carrier and b1) at least partially water-soluble liquid and / or b2) a water-reactive substrate each located within or on the carrier. The process for producing a creamy powdery composition according to claim 1 is activated by means of an energy input in the form of pressure, shear, temperature, vibration and / or solvent addition, the energy input being sufficient to release the liquid water or liquid aqueous phase from the shell-core material, liquid water or liquid aqueous phase subsequently is a) dissolve or wash the at least partially water-soluble liquid from the carrier and / or b) activate the water-reactive substrate in or on the carrier and subsequently dissolving or enriching the product or products obtained by activating the carrier.
    公开号:BR112012018812B1
    申请号:R112012018812-7
    申请日:2010-11-26
    公开日:2020-12-15
    发明作者:Jennifer C. Eng；Matthew Romaine；Christopher Proulx
    申请人:Evonik Operations Gmbh；
    IPC主号:
    专利说明:

    Field of the Invention
    [0001] The invention relates to a powder composition containing water and a process for producing a creamy composition from this powdery composition. Background of the Invention
    [0002] Solid cosmetic preparations, such as powders, with a high water content are known in the prior art. The basis of some patent applications is the fact that it has long been known that in the presence of a hydrophobic powder, such as a hydrophobic silicon dioxide powder, water can be dispersed in fine drops and surrounded by the hydrophobic material, thereby avoiding the droplets to collect. A powdery substance with a high water content, known as "dry water", is formed in this way (Fine Particles serié n ° 11, Evonik Degussa). Cosmetic formulations based on "dry water" are described in Seifen, Fette, Ole, Wachse (SOFW), 8 (2003), pages 1 to 8. These are free flowing, fine powders, which liquefy when rubbed over the skin. Liquefiable powder compositions, containing water, based on this principle are further described in several patent and patent applications.
    [0003] US 4,274,883 describes an aqueous dispersion of hydrophobic silica consisting of 0.1 to 50 parts of hydrophobic silica, in a given case of up to 3 parts of wetting agent and 99.9 to 50 parts of water. It is produced by intensive mixing of hydrophobic silica with water with the "dry water phase" known as an intermediate step. In a given case it can additionally be used as a wetting agent in which the case of the "dry water phase" does not occur. The dispersion of the hydrophobic silicas can be mixed without the additional steps or materials with rubber latex.
    [0004] DE-A-1467023 describes the use of aqueous solutions comprising cosmetic ingredients instead of pure water for the preparation of dry water.
    [0005] EP-A-1206928 describes a water-containing composition comprising powdered aqueous gel cores coated with hydrophobic particles.
    [0006] JP 2000-309505 describes a cosmetic powder being liquefied by means of embracement including from 2 to 20 by weight of a hydrophobic silica having a specific surface area of at least 60 m2 / g and an oil-in-emulsion composition Water.
    [0007] EP-A-1235554 describes a cosmetic or pharmaceutical powder-in-liquid composition comprising hydrophobically coated silica particles in which water and a water-soluble polymer are incorporated, the composition containing less than 1% oil.
    [0008] EP-A-1386599 describes a method for the production of dry water composed of an aqueous ingredient coated with a hydrophobic powder to form a powder state capable of liquefaction in the packaging at the time of use, comprising loading a powder hydrophobic and an aqueous ingredient into a hollow container forming a hydrophobic enclosure within it, followed by high-speed stirring in the hollow hydrophobic container to form fine aqueous droplets, and then allowing the surface of the thin aqueous droplets to be uniformly adsorbed with the hydrophobic powder.
    [0009] WO 01/85138 A2 describes an encapsulation system comprising an aqueous liquid core having at least 5% by weight of water therein, and an encapsulant surrounding the core to form stable encapsulated particles, the encapsulant comprising at least one layer of hydrophobic particles in contact with and around the core, the core and hydrophobic particles providing an encapsulated system that has a weighted average particle diameter of 0.05 to 25 micrometers, at least 25% of the encapsulated particles are spherical and can support their own weight.
    [00010] EP-A-855177 describes a bleaching powder comprising from 0.1 to 7% by weight of the trimethylsiloxylated silica having a specific surface area of at least 80 m2 / g and a degree of hydrophobicization of at least 50%, from 5 to 40% by weight of a polyhydric alcohol, from 50 to 94% by weight of water and from 0.01 to 5% by weight of a bleaching ingredient.
    [00011] WO 2005/058256 describes cosmetic preparations of a cream- or paste-like consistency, comprising 50 to 95% by weight of water, hydrophobized silicon dioxide powder, at least one relevant cosmetically active ingredient, or adjuvant that is soluble in water or that can be dispersed or emulsified in an aqueous medium and a viscosity regulator. The above description is produced by continuously adding the hydrophobized silicon dioxide powder with mixing, to a solution or dispersion of at least one relevant cosmetically-active ingredient and mixing is continued until a pasty consistency is achieved.
    [00012] Although prior art includes concepts such as water encapsulation, the problem with this concept is the amount of additives that can be added while maintaining a stable powder ranging from 0 to 3% by weight depending on additive properties, such as the polarity and chain length of the additives. Limiting the formulation to 0 to 3% by weight of an additive, and limiting additives, reduced the viability of the original concept. Even with the guidance of the industries that tried to use this concept, it had been unable to overcome limitations on the variety of additives or the amount of additive. Detailed Description of the Invention
    [00013] It is, therefore, an object of the present invention to provide a concept that overcomes past difficulties. The concept should not be restricted to cosmetic purposes, but should also allow for introduction into other industries, such as personal care or home care.
    [00014] The present invention provides a powdery composition comprising a) at least one powder in the form of shell-core particles, the core comprising liquid water or a liquid aqueous phase and the shell comprising hydrophobic or hydrophobized particles and b) at least one powder comprising a carrier and b1) a liquid at least partially soluble in water and / or b2) a reactive substrate in water one located inside and / or in the carrier.
    [00015] The water-soluble liquid and the substrate react with water, are reversibly linked to the carrier by capillary action / absorption / adsorption and can be washed or dissolved from the carrier partly or completely, by the liquid water or the liquid aqueous phase of the shell-core particles. The carrier itself may be water-soluble or not.
    [00016] The core shell particles as part of the composition according to the invention refer to a powder material, which contains liquid water or a liquid aqueous phase, but in which the coalescence of the individual water droplets is avoided by means of a shell of hydrophobic or hydrophobic particles. The shell is capable of releasing the liquid aqueous phase or liquid water from the core when activated by means of pressure, shear, temperature, vibration and / or addition of one or more solvents or one or more surfactants. This type of core shell particles is known as "dry water". The aqueous phase can be an aqueous solution, an aqueous dispersion or an aqueous emulsion.
    [00017] Hydrophobic particles are understood to be hydrophobic particles per se, whereas hydrophobic particles are those obtained by reacting the surface of a hydrophilic particle with a hydrophobic surface of the modifying agent. Generally, a covalent bond is formed between the reactive groups on the surface of the particles, for example, hydroxyl groups, and reactive groups on the surface modifying agent.
    [00018] In general "hydrophobic" means that there is only little or no interaction with water and the affinity for water is small or zero. A methanol wettability can be employed as a quantitative measurement of hydrophobicity. The bark particles of the present invention must have a methanol wettability of at least 40, preferably 50 to 80, more preferably 60 to 70. For the determination of methanol wettability, in each case 0.2 g (± 0.005 g) of the hydrophobic or hydrophobic particles are weighed in transparent centrifuge tubes. 8.0 ml portions of a methanol / water mixture with 10, 20, 30, 40, 50, 60, 70 or 80% by volume of methanol are added for each sample. The tubes are shaken for 30 seconds and then centrifuged at 2500 min-1 for 5 minutes. The wettability of methanol is defined as the volume percent of methanol so that the volume of sediment is 100%. The higher the number the higher the hydrophobicity.
    [00019] The hydrophobic or hydrophobized shell of the shell core particles usable in the present invention comprises, for example, inorganic powders such as talc, kaolin, mica, sericite, dolomite, phlogopite, synthetic mica, lepidolite, biotite, mica litia, vermiculite , magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungsten acid salts, magnesium, silica, zeolite, barium sulfate, sulfate calcium, calcined calcium phosphate, hydroxyapatite, fluorapatite, titania, pyrogenic titania, alumina and smoked alumina.
    [00020] Among these hydrophobized silica particles, which form a three-dimensional network, an aggregate structure is a preferred coating material. The silica can be a precipitated silica or a smoked silica, the latter being preferred. Colloidal silica is obtained in a flame hydrolysis or flame oxidation process. Its purity is greater than 99% by weight, Generally greater than 99.8% by weight. Smoked silica normally forms a three-dimensional network of primary particle aggregates. The primary smoked silica particles support hydroxyl groups on their surface and are non-porous.
    [00021] Pyrogenic and precipitated silica particles, as well as other particles suitable as particles are hydrophilic shell particles that need to be hydrophobized in a subsequent step. Procedures for this step are known to the person skilled in the art.
    [00022] Suitable surface modifying agents can be the following silanes, which can be used individually or as a mixture.
    [00023] Organosilane (RO) 3Si (CnH2n + 1) and (RO) 3Si (CnH2n-1) with R = alkyl, such as methyl, ethyl, n-propyl, isopropyl, butyl and n = 1-20.
    [00024] Organosilane R'x (RO) ySi (CnH2n + 1) and R'x (RO) ySi (CnH2n-1) with R = alkyl, such as, methyl, ethyl, n-propyl, isopropyl, butyl; R '= alkyl, such as, methyl, ethyl, n-propyl, isopropyl, butyl; R '= cycloalkyl; n = 1-20; x + y = 3, x = 1, 2; y = 1, 2.
    [00025] Halo-organosilane X3Si (CnH2n + 1) and X3Si (CnH2n-1) with X = Cl, Br; n = 1-20.
    [00026] Halo-organosilane X2 (R ') Si (CnH2n + 1) and X2 (R') Si (CnH2n-1) with X = Cl, Br, R '= alkyl, such as, methyl, ethyl, n- propyl, isopropyl, butyl-; R '= cycloalkyl; n = 1 - 20.
    [00027] Halo-organosilane X (R ') 2Si (CnH2n + 1) and X (R') 2Si (CnH2n-1) with X = Cl, Br; R '= alkyl, such as methyl-, ethyl-, n-propyl-, isopropyl-, butyl-; R '= cycloalkyl; n = 1 - 20.
    [00028] Organosilane (RO) 3Si (CH2) m-R 'with R = alkyl, such as, methyl-, ethyl-, propyl-; m = 0 - 20, R '= methyl, aryl, such as, -C6H5, substituted phenyl radicals, C4F9, OCF2-CHF-CF3, C6F13, OCF2CHF2, Sx- (CH2) 3Si (OR) 3.
    [00029] Organosilane (R ") x (RO) ySi (CH2) m-R 'with R" = alkyl, x + y = 3; cycloalkyl, x = 1, 2, y = 1, 2; m = 0.1 - 20; R '= methyl, aryl, such as, C6H5, substituted phenyl radicals, C4F9, OCF2-CHF-CF3, C6F13, OCF2CHF2, Sx- (CH2) 3Si (OR) 3, SH, NR'R''R' ' 'with R' = alkyl, aryl; R '' = H, alkyl, aryl; R '' '= H, alkyl, aryl, benzyl, C2H4NR' '' 'R' '' '' with R '' '' = H, alkyl and R '' '' '= H, alkyl.
    [00030] Halo-organosilane X3Si (CH2) m-R 'with X = Cl, Br; m = 0 - 20; R '= methyl, arial, such as, C6H5, substituted phenyl radicals, C4F9, OCF2-CHF-CF3, C6F13, O-CF2-CHF2, Sx- (CH2) 3Si (OR) 3, where R = methyl, ethyl, propyl, butyl ex = 1 or 2, SH.
    [00031] Halo-organosilane RX2Si (CH2) mR 'with X = Cl, Br; m = 0 - 20; R '= methyl, aryl, such as, C6H5, substituted phenyl radicals, C4F9, OCF2-CHF-CF3, C6F13, O-CF2-CHF2, -OOC (CH3) C = CH2, -Sx- (CH2) 3Si ( OR) 3, where R = methyl, ethyl, propyl, butyl and x = 1 or 2, SH.
    [00032] Halo-organosilane R2XSi (CH2) mR 'with X = Cl, Br; m = 0 - 20; R '= methyl, aryl, such as, C6H5, substituted phenyl radicals, C4F9, OCF2-CHF-CF3, C6F13, O-CF2-CHF2, -Sx- (CH2) 3Si (OR) 3, where R = methyl , ethyl, propyl, butyl ex = 1 or 2, SH.
    [00033] R'R2SiNHSiR2R 'silazanes with R, R' = alkyl, vinyl, aryl.
    [00034] Cyclic polysiloxanes D3, D4, D5 and their homologues, with D3, D4 and D5 meaning cyclic polysiloxanes having 3, 4 or 5 -O-Si (CH3) 2 units, for example, octamethylcclotetra-siloxane = D4 .
    [00035] Polysiloxanes or silicone oils of the Y-O type [[- SiRR'-O] m- [SiR'’R '' ’'' - O] n] u-Y with R = alkyl; R '= alkyl, aryl, H; R '' = alkyl, aryl; R '' '= alkyl, aryl, H; Y = CH3, H, CzH2z + 1 with z = 1 - 20, Si (CH3) 3, Si (CH3) 2H, Si (CH3) 2OH, Si (CH3) 2 (OCH3), Si (CH3) 2 (CzH2z +1) ez = 1 -20, m = 0, 1,2, 3, ..., n = 0, 1,2, 3, ..., u = 0, 1,2, 3, ... .
    [00036] The surface modifying agents of the following compounds may be preferred: octyltrimethoxysilane, octyltriethoxysilane, hexamethyldisilazane, hexadecyltrimethoxysilane, hexadecyltriethoxysilane, dimethylpolysiloxane, nonafluoroexyltrimethoxyloro, tridecafluoro, tridecafluoro, tridecafluoro With particular preference it is possible to employ hexamethyldisilazane, octyltriethoxysilane and dimethyl polysiloxanes.
    [00037] The particles of the shell of the powdery composition according to the invention can be particles of hydrophobized silica having a BET surface area preferably of 30 m2 / g to 500 m2 / g, more preferably of 100 m2 / g to 350 m2 / g . Due to the reaction with the surface modifying agent, these particles may contain from 0.1 to 15% by weight, usually from 0.5 to 5% by weight, of carbon.
    [00038] Typical examples that can be used as a coating material are
    [00039] Aerosil® R104 (octamethylcyclotetrasiloxane; 150 m2 / g; 55); AEROSIL® R106 (octamethylcyclotetrasiloxane; 250 m2 / g; 50), AEROSIL® R202 (polydimethylsiloxane; 100 m2 / g; 75), AEROSIL® R805 (octylsilane; 150 m2 / g; 60), AEROSIL® R812 (hexamethyldisilazane; / g; 60), AEROSIL® R812S (hexamethyldisilazane; 220 m2 / g; 65), AEROSIL® R8200 (hexamethyldisilazane; 150 m2 / g; 65).
    [00040] The indication in parentheses refers to the surface modifying agent, the approximate BET surface area and the approximate methanol wettability, determined by means of the procedure given in the specification.
    [00041] The particle material of the house particularly useful are the hydrophobized silica particles which are obtained by means of a hydrophilic reaction of the pyrogenic silica particles having a BET surface area from 270 to 330 m2 / g with hexamethyldisilazane. The hydrophobized silica particles obtained have a BET surface area from 200 to 290 m2 / g, a carbon content of 2 to 4% by weight and a methanol wettability of at least 50, more preferred from 50 to 70 .
    [00042] It may also be beneficial to use hydrophobized pyrogenic silica particles in compacted form or as granules.
    [00043] The other part of the core shell particles to be discussed is the core. The core contains liquid water, either in the form of liquid water itself, or as an aqueous liquid solution, an emulsion containing liquid water or as an aqueous dispersion. The dissolved or emulsified material in the case of an aqueous liquid solution or emulsion or the solid material in the case of an aqueous dispersion should be selected from those materials that neither significantly reduce the surface tension of the core nor cause the hydrophobic or hydrophobized particles to become wetted from a bark. For the aqueous liquid solution, this means that the solution must not contain more than 10% by weight, preferably not more than 3% by weight, of dissolved material. Liquid water is the most preferred core material itself.
    [00044] The core can be composed of an aqueous liquid phase containing up to 10% by weight of the compounds typically used in the fields of care, cosmetic personal or household care can be used, as long as they do not reduce the surface tension of the core or cause wetting of the hydrophobic or hydrophobicized particles of the shell. Typical example will be discussed together with the carrier containing a liquid, at least partially soluble in water and / or a substrate reacts with water.
    [00045] The water content of shell-core particles is generally in the range of 75 to 95% by weight, based on the core-shell particle.
    [00046] The powdery composition according to the invention consists of a powder next to the core-shell particles consisting of at least one other powder, defined as a carrier containing at least a partially water-soluble liquid or a water-reactive substrate, each located inside and / or in a carrier.
    [00047] The water-soluble liquid is capable of being washed or dissolved from the carrier, in parts or completely, by the core material of the shell-core particles in the case of the shell core particles are activated by means of pressure, shear, temperature, vibration and / or addition of one or more more solvents or one or more surfactants. This means that the water-soluble liquid is either partially or completely dissolved from the carrier by water or the aqueous phase of the core. Or the water-soluble liquid can be washed, partially or completely, to form the carrier by water or in the aqueous phase of the core.
    [00048] The same applies for a water-reactive substrate. A water-reactive substrate is a material that is not soluble in water or soluble in only a small amount. When activated by water or an aqueous phase that is transformed into a reaction product or products that are essentially or totally soluble in water.
    [00049] The carrier is preferably selected from the group consisting of silica, silica-mixed metal oxides, such as silica-aluminum mixed oxides, silica-titania mixed oxides, phyllosilicate, starch, hollow glass spheres, nylon, sugar, cyclodextrins and polysaccharides.
    [00050] In a special embodiment of the invention, the carrier is selected from smoked silica or precipitated silica, good results have been obtained with hydrophilic forms, as well as hydrophobized.
    [00051] In another special embodiment of the invention, the carrier is a precipitated silica having a) a BET surface area of 50 to 1000 m2 / g, preferably 100 to 700 m2 / g, more preferably 150 to 500 m2 / g, b) a particle size d50, determined by laser diffraction, from 2 to 100 μm, preferably from 3 to 20 μm, more preferably from 4 to 10 μm and c) an absorption of DBP (dibutyl phthalate) ), in g of DBP / 100 g of silica, from 200 to 400, preferably from 250 to 350.
    [00052] The BET surface area is determined according to ISO 5794-1, Annex D, the particle size D50 is determined according to ASTM 690-1992, and the DBP absorption is determined according to ASTM D 2414, based on the substance after drying.
    [00053] Special types of precipitated silica comprise a material having a BET surface area from 400 to 500 m2 / g, a d50 particle size of 4 to 6 μm and a DBP absorption of 300 to 350 g of DBP / 100 g of silica. Also another having a BET surface area from 150 to 250 m2 / g, a d50 particle size of 4 to 7 μm and a DBP absorption of 250 to 300 g of DBP / 100 g of silica. Typical examples are SIPERNAT® 500 LS and SIPERNAT® 22 LS, both by Evonik Degussa.
    [00054] The weight ratio of the at least partially water-soluble liquid and / or water-reactive substrate to the carrier is determined by means of multiple factors, such as the viscosity of the water-soluble liquid, the carrier structure comprising the pore size, pore volume and BET surface area. It is generally in the range of 10 to 90, a range of 60 to 75 being preferred.
    [00055] The weight ratio of the carrier including the at least partially water-soluble liquid and / or water-reactive substrate for the shell-core particles is generally 1: 1 to 1: 9.
    [00056] The average particle size of the carrier and of the particles with nucleus and layers, determined, for example, by transmission electron microscopy, can generally vary, independently of each other, from 2 to 20 µM. An average particle size of the core shell particles of 50 to 150% of the average carrier particle size may be preferred.
    [00057] The aqueous phase of the core of the shell-core particles and / or the at least partially water-soluble liquid and / or water-reactive substrate, each inside and / or in the carrier comprises at least one of the materials of the group consisting of comprises at least one of the materials in the group consisting of UV light protection filters, antioxidants, humidifying substances, deodorant, active antiperspirant compounds, biogenic substances, insect repellent active compounds, antioxidant bleaching agents, discoloration, antibacterial substances, antifungal substances , flavorings, fragrances, acids, alkalis, enzymes or mixtures thereof.
    [00058] UV light protection filters according to the invention are organic compounds that are liquid or crystalline at room temperature and are capable of absorbing ultraviolet rays and releasing the absorbed energy again in the form of radiation -longest wave, eg heat. UV filters can be oil-soluble or water-soluble. The oil-soluble substances are, for example: - 3-benzylidenocanfor and 3-benzylidenonorcanfor and their derivatives, - derivatives of 4-aminobenzoic acid, preferably 4- (dimethylamino) benzoic acid 2-2-ethylhexyl ester, 4-acid - (dimethyl-mino) benzoic ester of 2-octyl and 4- (dimethylamino) benzoic amyl ester-esters of cinnamic acid, preferably 4-methoxycinnamic acid 2-2-ethylhexyl ester, 4-methoxycinnamic acid propyl ester, 4-methoxycinnamic acid isoamyl ester, 2-cyano-3,3-phenylcinamic acid 2-2-ethylhexyl (octocrylene) ester - salicylic acid esters, preferably 2-2-ethyl- salicylic acid hexyl, salicylic acid 4-isopropyl-benzyl ester, salicylic acid homomentyl ester - benzophenone derivatives, preferably 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2,2'- dihydroxy-4-methoxybenzophenone - benzalmalonic acid esters, preferably 4-methoxybenzalmalonic acid 2-2-ethylhexyl diester - d-derivatives and triazine, such as, 2,4,6-trianilino- (p-carbo- 2'-ethyl-1'-hexyloxy) -1,3,5-triazine, octyl triazone and dioctyl butamido triazone - propane-1,3 -diones, such as 1- (4-tert-butylphenyl) -3- (4'-methoxyphenyl) propane-1,3-dione
    [00059] Possible water-soluble substances are: - 2-phenylbenzimidazole-5-sulfonic acid and alkali metal, alkaline earth metal, and their salts of glucammonium, ammonium, alkylammonium and alkanolamonium - derivatives of sulphonic acid from benzophenones, preferably acid 2-hydroxy-4-methoxybenzophenono-5-sulfonic acid and its salts - derivatives of 3-benzylidenocanfor sulfonic acid, such as, for example, 4- (2-oxo-3-bornylidenomethyl) benzene sulfonic acid and 2-methyl acid -5- (2-oxo-3-bornylidene) sulfonic acid and its salts.
    [00060] Typical UV-A filters are derived from benzoylmethane, such as 1- (4'-tert-butylphenyl) -3- (4'-methoxyphenyl) propane-1,3-dione, 4-tert-butyl- 4'-methoxydibenzoylmethane, 1-phenyl-3- (4'-isopropylphenyl) -propane-1,3-dione.
    [00061] UV-A and UV-B filters can certainly also be used in mixtures. Particularly favorable combinations include benzoylmethane derivatives, for example, 4-tert-butyl-4'-methoxydibenzoylmethane and 2-cyano-3,3-phenylcinamic acid 2-ethylhexyl ester (octocrylene) in combination with cinnamic acid esters , preferably 4-methoxycinnamic acid 2-2-ethylhexyl ester and / or 4-methoxycinnamic acid propyl ester and / or 4-methoxycinnamic acid isoamyl ester. Such combinations are advantageously combined with water-soluble filters, such as, for example, 2-phenylbenzimidazazole-5-sulfonic acid and alkali metal, alkaline earth metal, glucammonium, ammonium, alkylammonium, alkanolammonium and salts thereof.
    [00062] In addition to the organic substances mentioned, insoluble light protection pigments, namely, finely dispersed in metal oxide powder, as such or in the form of hydrophobized, and salts are also possible for this purpose. Examples of suitable metal oxide powders or hydrophobized metal oxide powders can be titanium dioxide powder, zinc oxide powder and / or a mixed oxide powder of these with the elements Si, Ti, Al, Zn, Fe, B, Zr and / or Ce.
    [00063] Typical examples are coated titanium dioxides such as UV-Titan M212, M and X 262 111 (Kemira), AEROXIDE® TiO2 P25, PF2, T 805 and T 817 (Evonik Degussa), MT Titanium Dioxide -150 W, MT-100 AQ, MT-100, SA, MT-100 HD, MT-100 TV (Tayca), Eusolex TM T2000 (Merck), neutral zinc oxide H and R and zinc oxide NDM (Haarmann and Reimer), as well as Z-Cote and Z-Cote HP1 (BASF).
    [00064] Dispersions such as, for example, TEGO dom TAQ 40, a weight 40.% Aqueous dispersion of a hydrophobized titanium dioxide (Evonik Goldschmidt) can also be used.
    [00065] Typical antioxidants as part of the powdery composition according to the invention may be - Amino acids such as glycine, tyrosine, histidine or tryptophan and their derivatives, - Imidazoles such as urocanic acid) and their derivatives, - Peptides, such as D, L-carnosine, D-carnosine, L-carnosine and their derivatives, - Carotenoids, carotenes, alpha-carotene, beta-carotene lycopene, and their derivatives, - Chlorogenic acid and its derivatives, - Liponic acid and its derivatives - Chelators such as alpha-hydroxy fatty acids, palmitic acid, phytic acid, - Alpha-hydroxy acids such as citric acid, lactic acid, acid-domálico - Unsaturated fatty acids and their derivatives, such as acid gamma-linolenic acid, linoleic acid, oleic acid, - Folic acid and its derivatives, - Ubiquinone and ubiquinol and their derivatives, - Vitamin C and its derivatives, such as ascorbyl palmitate, ascorbyl phosphate, ascorbyl acetate, - Tocopherols and derivatives, like vitamin E, vitamin E acetate, - Vitam ina A and its derivatives, such as vitamin A palmitate - Mannose and its derivatives, - Superoxide dismutase.
    [00066] Hydrating substance can be selected from the group consisting of ethylene glycol, butylene glycol, 2,3-butanediol, propylene glycol, dipropylene glycol, tripropylene glycol, hexylene glycol, diglycerin, glycerin, glucose, fructose, lactose, sucrose, maltose, mannitol, mannose, PEG-4 for PEG-800, such as PEG-4, PEG-6, PEG-7, PEG-8, PEG-9, PEG-10, PEG- 12, PEG-14, PEG-16, PEG-18, PEG-20, sorbitol, polyglyceryl sorbitol, xylitol urea, and mixtures thereof.
    [00067] Deodorant and active antiperspirant compounds can be at least one selected from the group consisting of - Astringent metal salts, such as aluminum hydrochlorides, aluminum hydroxylates, aluminum zirconium hydrochlorides and zinc salts - Germs of inhibitory agents, such as chitosan, phenoxyethanol, chlorhexidine gluconate or 5-chloro-2- (2,4-dichlorophenoxy) -phenol - Enzyme inhibitors, such as i) trialkyl citrates, such as trimethyl citrate, citrate tripropyl, triisopropyl citrate, tributyl citrate and triethyl citrate; ii) sterol sulphates or phosphates, such as lanosterol, cholesterol, campesterol, stigmasterol and sitosterol and phosphate sulphate, iii) dicarboxylic acids and their esters, such as, for example, glutaric acid, monoethyl acid ester glutaric acid, glutaric diethyl ester, adipic acid, adipic acid monoethyl ester, adipic acid diethyl ester, malonic acid and malonic acid diethyl ester, iv) hydroxycarboxylic acids and esters thereof, such as, for example, citric acid, malic acid, tartaric acid or ester of diethyl tartaric acid; or v) 4-hydroxybenzoic acid and its salts and esters, N- (4-chlorophenyl) -N '- (3,4-dichlorophenyl) urea, 2,4,4'-trichloro-2-hydroxy-diphenyl ether (Triclosan ) 4-chloro-3,5-dimethyl-phenol, 2,2'-methylene-bis (6-bromo-4-chlorophenol), 3-methyl-4- (1-methylethyl) -phenol, 2-benzyl-4 -chlorophenol, 3- (4-chlorophenoxy) -1,2-propanediol, 3-iodo-2-propynyl butylcarbamate, chlorhexidine, 3,4,4'-trichlorocarbanilide
    [00068] Thymol, thyme oil, eugenol, clove oil, menthol, mint oil, farnesol, phenoxyethanol, glycerol monocaproate, glycerol monocaprylate, glycerol monolaurate, diglycerol mocaproate (DMC), salicylic acid N-alkylamides, such as n-octylamide salicylic acid or n-decylamide salicylic acid. - odor absorbers or maskers such as benzyl acetate, p-tert-butylcyclohexyl acetate, linalyl acetate, phenylethyl acetate, linaloyl benzoate, benzyl formate, allylcyclohexyl propionate, styryl propionate and benzyl salicylate, benzyl ethyl ether, citral, citraldehyde-citronellaldehyde , cyclamenaldehyde, hydroxycitralal, jonones, methyl cedril keto, anethole, citronelol, eugenol, isoeugenol, geraniol, linalool, phenylethyl alcohol, terpineol or terpenes.
    [00069] Biogenic substances can be selected from at least one of the group consisting of tocopherol acetate, tocopherol, tocopherol palmitate, ascorbic acid, (deoxy) ribonucleic acid and fragmentation products thereof, beta-glucans , retinol, bisabolol, allantoin, phyanthriol, panthenol, pantothenic acid, fruit acids, alpha-hydroxy acids, amino acids, ceramides, pseudoceramides, essential oils, plant extracts, such as, for example, Prunus extract, Bambara nut extract and vitamin complexes.
    [00070] The active insect repellent compounds can be selected from the group consisting of N, N-diethyl-m-toluamide, 1,2-pentanediol, 3- (Nn-butyl-N-acetyl-amino) -propionic acid ethyl ester and butyl acetylaminopropionate.
    [00071] Examples of bleaching agents suitable for the present invention are zinc hydroquinone, peroxide, urea peroxide, hydrogen peroxide and / or organic peroxides.
    [00072] In a special embodiment of the invention, the core of the shell-core particles is water, and the shell consists of hydrophobic fumed silica particles that are obtained through the reaction of a hydrophilic fumed silica having a BET surface area from from 30 to 500 m2 / g.
    [00073] In addition, in an advantageous embodiment of the invention, the hydrophobic fumed silica particles are obtained by reacting a hydrophilic fumed silica having a BET surface area of 270 to 330 m2 / g with hexamethyldisilazane to give hydrophobic fumed silica particles. having a BET surface area from 200 to 290 m2 / g and a carbon content of 2 to 4% by weight and methanol wettability of at least 50.
    [00074] The special modality can also comprise as a carrier of precipitated silica having a BET surface area of 400 to 500 m2 / g, a particle size d50, determined by means of laser diffraction, from 4 to 6 μm and an absorption of DBP (dibutyl phthalate), in g of DBP / 100 g of silica, from 300 to 350.
    [00075] The special modality can also comprise as a carrier of precipitated silica having a BET surface area of 150 to 250 m2 / g, a particle size d50, determined by means of laser diffraction, from 4 to 7 μm and an absorption of DBP (di-butyl phthalate), in g of DBP / 100 g of silica, from 250 to 300.
    [00076] In addition, special modalities may also comprise at least liquid partially soluble in water and / or water-reactive substrate, each located inside and / or in the carrier, and filters for UV light protection, antioxidants, substances humidifying, deodorant, antiperspirant active compounds, biogenic substances, insect repellent active compounds, antioxidant bleaching agents, discoloration, antibacterial substances, antifungal substances, flavorings, fragrances, acids, alkalis, enzymes or mixtures thereof.
    [00077] Another object of the invention is a process for the production of a creamy composition, from the shape of the powdery composition according to the invention. This powdery composition is activated by means of an energy input in the form of pressure, cementation, temperature, vibration and / or solvent addition, the energy input being sufficient to release liquid water or the aqueous-liquid phase from the material shell-core, the liquid water or the liquid aqueous phase subsequently is a) dissolving or washing at least the partially water-soluble liquid from the carrier and / or b) activating the water-reactive substrate in and / or in the carrier and subsequently dissolving or washing the product or products obtained by activating the carrier.
    [00078] "Creamy" is understood to mean a range from more liquid compositions to more gel-like compositions for creamy compositions.
    [00079] Having generally described this invention, further understanding can be obtained by reference to certain specific examples which are provided for illustration only, and are not intended to be limiting. Examples Example 1: Powder Foundation in Cream Powder according to the state of the art
    [00080] To create the dry water formulation, 77.5 wt% deionized water (DI) was added to the KitchenAid # KSB5ER4 mixer model along with 10.48 wt% Carbowax ® Sentry Polyethylene Glycol 400 NF from The Dow Chemical Company, 5.27% by weight of dimethisil ® DM-20 (20cPs) from Chemsil Silicones, Inc., 1.75% by weight of the iron oxide pigments, AC-5 Red R516P, AC-5 Yellow LL-100P, AC-5 black BL-100P, and AC-5 TiO2 CR-50, from Kobo. AEROSIL ® R812S was added to 5.0% by weight over the mixture of water and PEG /// Dimeticone Pigments. The cap was placed firmly on the mixer and the mixture was mixed at the highest setting (Liquefy) at 9700 RPM for one minute. During one minute of mixing, the entire mixer was tilted at an angle of 50 to 60 from left to right, with waiting times of 10 seconds.
    [00081] The product is a cream / mousse texture that has a clear separation at the bottom after about 30 minutes. The process of adding PEG and dimethicone failed since none of the discrete stable droplets were formed when mixed together with the hydrophobic silica. Emollients are believed to have lowered the surface tension of water in such a way that it was able to overcome the interfacial tension between the droplets and R812S Aerosil ®. Example 2: Powder-based powder foundation according to the invention
    [00082] To prepare a new powdered cream foundation formulation according to the invention, a PEG Dimeticone // pigment / dilution of water Dl was created by mixing 42.9% by weight De PEG Sentry ® Polyethylene Glycol 400 NF a from The Dow Chemical Company, 21.4 wt. -% Dimethisil ® DM-20 (20cPs) of Chemsil Silicones, 28.6 wt -.% Deionized water (DI), and 7.1% by weight AC-5 iron oxide pigments from Kobo. This solution was then added to SIPERNAT ® 22LS in 3-4 addition steps using low shear mixing by hand, using a metal spatula. The powder product resulted in a mixture that consisted of 70% by weight of emollient / pigment solution, the liquid, and 30% by weight, of the carrier. This powder product will now be referred to as a liquid / carrier.
    [00083] Dry water was produced by adding 5% by weight of AEROSIL ® R812S, 20% by weight of iron oxide AC-5 pigments and 75% by weight of DI water. The cap was placed firmly on the mixer and the mixture was mixed at the highest setting (Liquefy) at 9700 RPM for one minute. During one minute of mixing, the entire mixer was tilted at an angle of 50-60 ° from left to right, with about 10 second hold times.
    [00084] Thirty-five percent by weight of the liquid / carrier was then gently mixed (tipped, stirred or folded in) with 65% by weight of water mix and dried to make the final cream foundation powder.
    [00085] This powder was then stored in a plastic container. The powdery composition was able to be created, and stay, like a powder Example 3: Cream Powder Vitamin Rub according to the state of the art
    [00086] 13.71% by weight of the emollient, polyethylene glycol (PEG Sentry ® Polyethylene Glycol 400 NF from The Dow Chemical Company), 2.75% by weight of Vitamin E (Jeen International Corp), 78.54% by weight of Dl water and 5.0% by weight of AEROSIL ® R812S were weighed and placed in a KitchenAid Model No. KSB5ER4 mixer and mixed at maximum speed (9700 rpm, Liquefied) for 1 minute. During the 1 minute of mixing, the blender was tilted at an angle of 45 degrees from left to right, with a waiting time of about 10 seconds each side.
    [00087] The final product was a cream / mousse texture that has a clear separation at the bottom after about half an hour.
    [00088] The process of adding the emollient and vitamin failed since none of the discrete stable drops were formed when mixed together with the hydrophobic silica. It is believed that the emollient and vitamin lowered the surface tension of water in such a way that it was able to overcome the interfacial tension between the droplets and Aerosil ® R812S. Example 4: Vitamin-Powder for Cream-Rub according to the invention
    [00089] A liquid mixture of 71.4% by weight Of polyethylene glycol (PEG Sentry ® Polyethylene Glycol 400 NF from The Dow Chemical Company), 14.3% by weight E Vitamin (from Jeen International Corp) and 14.3% by weight of Dl water was made. The liquid mixture was then used to make a 64.0 - weight. Liquid mixture%, by weight, for 36.0 -.% SIPERNAT ® 22LS as carrier. The liquid mixture was added slowly to Sipernat ® LS 22 in 3-4 addition steps, using low shear mixture (in this case, by hand) until the mixture was uniform.
    [00090] The powder obtained (30% by weight) was then delicately mixed (dropped, tossed or folded in) to 70% by weight of dry water.
    [00091] The powder was then stored in a plastic container. Table 1: Ingredients of the formulations of Examples 1 to 4 [% by weight]
    权利要求:
    Claims (9)
    [0001]
    1. Powdery composition, characterized by the fact that it comprises: (a) at least one powder in the form of shell-core particles, the core comprising liquid water or a liquid aqueous phase, and the shell comprising hydrophobized particles, in the form of particles of hydrophobized silica, which are obtained by reacting a hydrophilic pyrogenic silica having a BET surface area of 270 to 330 m2 / g with hexamethyldisilazane to generate hydrophobized particles of pyrogenic silica having a BET surface area of 200 to 290 m2 / g and a carbon content of 2 to 4% by weight and methanol wettability of at least 50; and (b) at least one powder comprising the carrier in the form of a precipitated silica having: (c) a BET surface area of 150 to 250 m2 / g, (d) a particle size d50, determined by means of diffraction laser, 4 to 7 μm, and (e) an absorption of DBP (dibutyl phthalate), in g of DBP / 100 g of silica, from 250 to 300, and (b1) at least partially water-soluble liquid, and / or (b2) a water-reactive substrate, which is not soluble in water and which, when activated by water or an aqueous phase, is transformed into a reaction product or products, which are soluble in water, each located inside and / or in the carrier; the water-soluble liquid and the water-reactive substrate are reversibly linked to the carrier by capillary action / absorption / adsorption and can be washed or dissolved from the carrier, partially or completely, by the liquid water or the liquid aqueous phase of the core-shell particles, whether the vehicle itself is soluble or not in water.
    [0002]
    2. Powdery composition according to claim 1, characterized in that the hydrophobized silica particles are aggregated pyrogenic silica particles.
    [0003]
    3. Powdery composition according to claim 1, characterized by the fact that the core essentially consists of water.
    [0004]
    4. Powdery composition according to claim 1, characterized by the fact that the water content of the shell-core particles is 75 to 95% by weight.
    [0005]
    5. Powdery composition according to claim 1, characterized by the fact that the weight ratio of the carrier including at least partially water-soluble liquid and / or water-reactive substrate to the shell-core particles is from 1: 1 to 1: 9.
    [0006]
    6. Powdery composition, according to claim 1, characterized by the fact that the average particular size of the carrier and of the shell-core particles is 2 to 20 μm.
    [0007]
    7. Powdery composition according to claim 6, characterized by the fact that the average particle size of the core shell particles is 50 to 150% of the average carrier particle size.
    [0008]
    8. Powdery composition according to claim 1, characterized by the fact that: (a) the aqueous phase of the core of the shell-core particles, and / or (b) the at least liquid partially soluble in water and / or substrate reactive in water, each in and / or in the carrier comprises at least one of the group's materials consisting of UV light protection filters, antioxidants, humidifying substances, deodorant, antiperspirant active compounds, biogenic substances, active insect repellent compounds, antioxidant bleaching agents, discoloration, antibacterial substances, antifungal substances, flavorings, fragrances, acids, alkalis, enzymes or mixtures thereof.
    [0009]
    9. Process for producing a creamy composition, characterized by the fact that the powdery composition, as defined as defined in any of claims 1 to 8, is activated by means of an energy input in the form of pressure, shear, temperature, vibration and / or addition of solvent, the energy input being sufficient to release the liquid water or the liquid aqueous phase of the shell-core material, the liquid water or the liquid aqueous phase subsequently is: (a) dissolving or washing the at least partially water-soluble liquid from the carrier, and / or (b) activating the water-reactive substrate in and / or in the carrier and subsequently dissolving or washing the products or products obtained by activating the carrier.
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    同族专利:
    公开号 | 公开日
    EP2515829A1|2012-10-31|
    JP2013515689A|2013-05-09|
    CN102686207A|2012-09-19|
    KR101431932B1|2014-08-19|
    KR20120091389A|2012-08-17|
    CA2785753C|2016-12-06|
    US20130022656A1|2013-01-24|
    CN102686207B|2014-05-28|
    US8647653B2|2014-02-11|
    MX2012007285A|2012-07-30|
    BR112012018812A2|2020-09-01|
    CA2785753A1|2011-06-30|
    WO2011076518A1|2011-06-30|
    JP5746210B2|2015-07-08|
    EP2515829B1|2016-08-10|
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    法律状态:
    2020-09-08| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2020-09-29| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-10-27| B25D| Requested change of name of applicant approved|Owner name: EVONIK OPERATIONS GMBH (DE) |
    2020-12-15| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 10 (DEZ) ANOS CONTADOS A PARTIR DE 15/12/2020, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    US29020509P| true| 2009-12-26|2009-12-26|
    US61/290,205|2009-12-26|
    PCT/EP2010/068324|WO2011076518A1|2009-12-26|2010-11-26|Water containing powder composition|
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