Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
  • A61K8/89—Polysiloxanes
  • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
• • A—HUMAN NECESSITIES
  • A45—HAND OR TRAVELLING ARTICLES
  • A45D—HAIRDRESSING OR SHAVING EQUIPMENT; EQUIPMENT FOR COSMETICS OR COSMETIC TREATMENTS, e.g. FOR MANICURING OR PEDICURING
  • A45D33/00—Containers or accessories specially adapted for handling powdery toiletry or cosmetic substances
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/31—Hydrocarbons
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
  • A61Q1/02—Preparations containing skin colorants, e.g. pigments
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
  • A61Q1/02—Preparations containing skin colorants, e.g. pigments
  • A61Q1/04—Preparations containing skin colorants, e.g. pigments for lips
  • A61Q1/06—Lipsticks
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
  • A61Q1/02—Preparations containing skin colorants, e.g. pigments
  • A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
  • A61K2800/59—Mixtures
  • A61K2800/591—Mixtures of compounds not provided for by any of the codes A61K2800/592 - A61K2800/596
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
  • A61K2800/88—Two- or multipart kits

Definitions

• the invention relates to a cosmetic method for making up and/or caring for keratinous substances, in particular the skin, comprising the application to said keratinous substances of a cosmetic composition comprising a siloxane resin and an inorganic filler.
• a cosmetic composition comprising a siloxane resin and an inorganic filler.
• the invention relates in particular to compositions for caring for or making up said keratinous substances.
• a makeup product must also be comfortable. Comfortable is understood to mean a product which glides over the skin, without a rubbing feeling, when the product is applied to the skin, but also a product which confers a soft touch on said skin.
• the aim of the present invention is thus to provide a makeup method which makes it possible to obtain satisfactory properties of hold of the makeup while at the same time retaining the comfort during and after application.
• R 3 groups of the siloxane resin are propyl groups
• the combination used according to the invention makes it possible to obtain a soft finish on the skin and cosmetic properties which are stable over time, in particular throughout the day.
• the product also glides over the skin, during application, without a rubbing feeling and confers a soft touch on said skin.
• composition according to the invention can be provided in various forms, in particular in the form of powders (loose or compact), of an anhydrous dispersion, of a water/oil, water/wax, oil/water, multiple (such as a water/oil/water or oil/water/oil) or wax/water emulsion or in the form of a gel.
• the composition according to the invention is provided in the form of powders (loose or compact), of anhydrous dispersions or of emulsions, preferably an inverse emulsion (i.e., water/oil emulsion).
• composition according to the invention is intended in particular for making up and/or caring for the skin.
• siloxane resins which can be used according to the invention can be obtained by a process comprising the reaction of:
• the A/B ratio is less than or equal to 70:30.
• the A/B ratio is equal to 30:70 or 50:50.
• the resins which can be used according to the invention are in particular those described in application WO 2005/075542.
• the MQ-propyl T resin according to the invention comprises units:
• the amount of each unit present in the MQ-propyl T resin can be expressed as a molar fraction (i.e. a, b, c or d) of the total number of moles of all the M, D, T and Q units present in the MQ-propyl T resin.
• the value of a (molar fraction of M units) is between 0.05 and 0.5, or alternatively between 0.15 and 0.4.
• the value of b (molar fraction of D units) is between 0 and 0.3, or alternatively between 0 and 0.1, or alternatively between 0 and 0.05.
• the MQ-propyl T resin according to the invention can be devoid of D units or alternatively can comprise up to 0.3 molar fraction of D units.
• the MQ-propyl T resin according to the invention is devoid of D units.
• c (molar fraction of T units) is greater than 0, or alternatively between 0.05 and 0.65, or alternatively between 0.4 and 0.65.
• d (molar fraction of Q units) is between 0.05 and 0.6, or alternatively between 0.2 and 0.6, or alternatively between 0.2 and 0.55.
• the MQ-propyl T resin according to the invention is characterized in that at least 40 mol %, preferably at least 50 mol %, preferably at least 90 mol % of R 3 alkyl groups of the T units are propyl groups.
• the R 1 , R 2 and R 3 radicals of the units of the MQ-propyl T resin independently represent an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group.
• the alkyl groups can in particular be chosen from the methyl, ethyl, propyl, butyl, pentyl, hexyl and octyl groups.
• the alkyl group is a methyl group or a propyl group.
• the aryl groups can be chosen from the phenyl, naphthyl, benzyl, tolyl, xylyl, xenyl, methylphenyl, 2-phenylethyl, 2-phenyl-2-methylethyl, chlorophenyl, bromophenyl and fluorophenyl groups, the aryl group preferably being a phenyl group.
• carbinol group is understood to mean any group comprising at least one hydroxyl radical bonded to a carbon (COH).
• the carbinol groups can thus comprise more than one COH radical, such as, for example:
• carbinol group is devoid of aryl groups, it comprises at least 3 carbon atoms. If the carbinol group comprises at least one aryl group, it comprises at least 6 carbon atoms.
• R 4 group of alkylene radicals, such as —(CH 2 ) x —, the value of x being between 3 and 10, —CH 2 CH(CH 3 )—, —CH 2 CH(CH 3 )CH 2 —, —CH 2 CH 2 CH(CH 2 CH 3 )CH 2 CH 2 CH 2 — and —OCH(CH 3 )(CH 2 ) x —, the value of x being between 1 and 10.
• alkylene radicals such as —(CH 2 ) x —, the value of x being between 3 and 10, —CH 2 CH(CH 3 )—, —CH 2 CH(CH 3 )CH 2 —, —CH 2 CH 2 CH(CH 2 CH 3 )CH 2 CH 2 CH 2 — and —OCH(CH 3 )(CH 2 ) x —, the value of x being between 1 and 10.
• carbinol group comprising aryl groups exhibiting at least 6 carbon atoms of the groups of formula R 5 OH in which R 5 represents an arylene radical such as —(CH 2 ) x C 6 H 4 —, x having a value of between 0 and 10, —CH 2 CH(CH 3 )(CH 2 ) x C 6 H 4 —, x having a value of between 0 and 10, —(CH 2 ) x C 6 H 4 (CH 2 ) x —, x having a value of between 1 and 10.
• the carbinol groups comprising aryl groups generally comprise from 6 to 14 atoms.
• Amino group according to the invention is understood to mean in particular groups of formula —R 6 NH 2 or —R 6 NHR 7 NH 2 , R 6 representing a divalent hydrocarbon radical having at least 2 carbon atoms and R 7 representing a divalent hydrocarbon radical having at least 2 carbon atoms.
• the R 6 group generally represents an alkylene radical having from 2 to 20 carbon atoms. Mention may be made, as examples of R 6 group, of the ethylene, propylene, —CH 2 CHCH 3 —, butylene, —CH 2 CH(CH 3 )CH 2 —, pentamethylene, hexamethylene, 3-ethylhexamethylene, octamethylene and decamethylene groups.
• the R 7 group generally represents an alkylene radical having 2 to 20 carbon atoms. Mention may be made, as examples of R 7 group, of the ethylene, propylene, —CH 2 CHCH 3 —, butylene, —CH 2 CH(CH 3 )CH 2 —, pentamethylene, hexamethylene, 3-ethylhexamethylene, octamethylene and decamethylene groups.
• the amino groups are generally —CH 2 CH 2 CH 2 NH 2 , —CH 2 (CH 3 )CHCH 2 (H)NCH 3 , —CH 2 CH 2 NHCH 2 CH 2 NH 2 , —CH 2 CH 2 NH 2 , —CH 2 CH 2 NHCH 3 , —CH 2 CH 2 CH 2 CH 2 NH 2 , —(CH 2 CH 2 NH) 3 H and —CH 2 CH 2 NHCH 2 CH 2 NHC 4 H 9 .
• R 1 represents a methyl group
• R 2 represents a methyl group or a phenyl group
• R 3 represents a propyl group
• the MQ-propyl T resin according to the invention is devoid of D units, and R 1 represents a methyl group, and R 3 represents a propyl group.
• the D, T or Q siloxane units of the MQ-propyl T resin according to the invention can comprise hydroxyl (—OH) groups and/or alkoxy groups.
• Such siloxane units comprising hydroxyl and/or alkoxy groups are commonly present in siloxane resins having the general formula R n SiO (4-n)/2 .
• hydroxyl groups typically result from the reaction of a hydrolyzable group on the siloxane unit with water; the alkoxy groups result from an incomplete hydrolysis when alkoxysilane precursors are used or result from the exchange of alcohol with hydrolyzable groups.
• the total amount by weight of —OH groups present in the MQ-propyl T resin is approximately 3%, preferably 2%, preferably 1.5%.
• the total amount by weight of alkoxy groups present in the MQ-propyl T resin is less than or equal to 20% by weight, preferably less than or equal to 10% by weight.
• the siloxane resin present in said composition comprises the units:
• R 3 groups of the siloxane resin are propyl groups.
• M N the number-average molecular weight
• the MQ-propyl T resins which can be used according to the invention can be prepared according to the processes known in the state of the art for preparing siloxane resins of general formula R n SiO (4-n)/2 , where R is an alkyl group and n is less than 1.8.
• the MQ-propyl T resins can be prepared according to the methods described below.
• MQ-propyl T resins according to the invention are illustrated by the MQ-propyl T resins comprising the following units:
• siloxane resins which can be used according to the invention can be obtained by a process comprising the reaction between:
• the component A) is an MQ resin comprising at least 80 mol % of (R 1 3 SiO 1/2 ) a and (SiO 4/2 ) d units, where R 1 is as defined above, i.e. represents an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group, a and d are greater than zero and the ratio aid is between 0.5 and 1.5.
• MQ resins which can be used as component A) and their method of preparation are known from the prior art.
• U.S. Pat. No. 2,814,601 belonging to Currie and al., dated Nov. 26, 1957 describes a process for manufacturing MQ resins by conversion of a water-soluble silicate into a silicic acid monomer or a silicic acid oligomer by using an acid. Once the appropriate polymerization has been carried out, trimethylchlorosilane ends are introduced in order to obtain the MQ resin.
• Another process of preparation of MQ resins is described in U.S. Pat. No. 2,857,356, belonging to Goodwin, dated Oct. 21, 1958.
• the MQ resins suitable as component A) in the present invention can comprise D and T units, provided that at least 80 mol %, indeed even 90 mol %, of the total siloxane units are M and Q units.
• the MQ resins can also comprise hydroxyl groups.
• the MQ resins can thus comprise hydroxyl groups in a total amount by weight of between 2 and 10%, preferably between 2 and 5%.
• the MQ resins can also comprise additional ends, residual hydroxyl groups being for this reacted with the M groups.
• the component B) is a propyl T resin comprising at least 80 mol % of (R 3 SiO 3/2 ) c units, R 3 being as defined above, i.e. representing an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group, c being greater than 0, provided that at least 40 mol % of the R 3 groups are propyl groups.
• the propyl T resin according to the invention is a silsesquioxane resin. Silsesquioxane resins are well known in the state of the art and are generally obtained by hydrolysis of an organosilane comprising three hydrolyzable groups, such as halogen or alkoxy groups, present in the molecule.
• the component B) can thus be obtained by hydrolysis of propyltrimethoxysilane, propyltriethoxysilane or propyltripropoxysilane or by cohydrolysis of the abovementioned propylalkoxysilanes with various alkoxysilanes. Mention may be made, as examples of these alkoxysilanes, of methyltrimethoxysilane, methyltriethoxysilane, methyltriisopropoxysilane, dimethyldimethoxysilane and phenyltrimethoxysilane. Propyltrichlorosilane can also be hydrolyzed, alone or in the presence of alcohol.
• the cohydrolysis can be carried out by adding methyltrichlorosilane, dimethyldichlorosilane, phenyltrichlorosilane or similar chlorosilanes and methyltrimethoxysilane, methyltriethoxysilane, methyltriisopropoxysilane or similar methylalkoxysilanes.
• Mention may be made, as alcohols suitable for this purpose, of methanol, ethanol, n-propyl alcohol, isopropyl alcohol, butanol, methoxyethanol, ethoxyethanol or similar alcohols.
• solvents of hydrocarbon type which can be used, of toluene, xylene or similar aromatic hydrocarbons; hexane, heptane, isooctane or similar saturated and linear or partially branched hydrocarbons; and cyclohexane or similar aliphatic hydrocarbons.
• the propyl T resins as component B) according to the invention can comprise M, D and Q units, provided that at least 80 mol %, indeed even 90 mol % of the total siloxane units are T units.
• the propyl T resins can also comprise hydroxyl groups.
• the propyl T resins comprise between 3 and 8% by weight of hydroxyl groups.
• a polyorganosiloxane can also be added to the process according to the invention as component C).
• the polyorganosiloxanes of use as component C) according to the invention comprise R 2 2 SiO 2/2 or R 3 SiO 3/2 units.
• the polyorganosiloxane can be added in order to introduce various D and T units into the MQ-propyl T resins, in order to modify the properties of the resulting resins.
• the structure or the formula of the polyorganosiloxane is not limiting, provided that said polyorganosiloxane comprises a measurable amount of R 2 2 SiO 2/2 or R 3 SiO 3/2 units and that the total amount of polyorganosiloxane added to the reaction between A) and B) does not result in more than 50 mol % of D or T units in the reaction mixture.
• the polyorganosiloxane can comprise combinations of M, D, T and Q units, provided that at least the D or T units are present.
• the polyorganosiloxane can be chosen from silicone fluids, gums or resins known from the prior art and comprising D or T units, or their mixtures.
• the D units typically comprise methyl or phenyl groups or their mixtures as R 2 groups.
• the T units typically comprise methyl or phenyl groups or their mixtures as R 3 groups.
• the polyorganosiloxane can be a fluid linear polydiorganosiloxane having a viscosity of between 10 and 1000 cS (mm 2 /s).
• the fluid polydiorganosiloxane can be a polydimethylsiloxane or a polymethylphenylsiloxane.
• the polyorganosiloxane can also be an organosilsesquioxane resin.
• the organosilsesquioxane resin is typically a methylsilsesquioxane resin or a phenylsilsesquioxane resin.
• the components A), B) and optionally C) can react by any method known from the prior art for acting on M, D, T and Q units. However, preferably, the components A), B) and optionally C) react by a condensation reaction in the presence of a catalyst.
• the MQ resin is typically present in an aromatic hydrocarbon or siloxane solvent.
• Condensation reaction catalysts which can be used are in particular metal hydroxides, such as potassium hydroxide or sodium hydroxide; metal salts, such as silanolates, carboxylates and carbonates; amines; titanates, such as tetrabutyl titanate; and their mixtures.
• the reaction between the components A), B) and optionally C) is carried out by heating the reaction mixture to temperatures ranging from 50 to 140° C., preferably ranging from 100 to 140° C.
• the reaction can take place in a semicontinuous, continuous or batch process.
• said siloxane resin is obtained by a process comprising the reaction between:
• the A/B ratio by weight in the reaction is between 95:5 and 15:85, preferably between 95:5 and 20:80, preferably between 90:10 and 20:80.
• the A/B ratio by weight is equal to 85:15 or 50:50 or 30:70 or 95:5.
• the A/B ratio by weight is equal to 30:70.
• the amount of component C) can vary but provided that it results in a content of additional D or T units of less than 30 mol %, with respect to the total molar amount of siloxane units of the reaction mixture.
• composition according to the invention comprises an amount of siloxane resin, by weight of active material (dry matter), ranging from 0.5 to 60% by weight, with respect to the total weight of the composition, preferably from 3 to 60% by weight and better still from 4 to 60% by weight, with respect to the total weight of said composition.
• the amount of siloxane resin, by weight of active material (dry matter) will advantageously range from 3 to 60% by weight and better still from 6 to 60% by weight, with respect to the total weight of said composition.
• active material dry matter
• these contents are in particular suitable for the compositions in anhydrous form and especially for the compositions in the stick form, such as lipsticks.
• the amount of siloxane resin, by weight of active material (dry matter) will advantageously range from 3 to 30% by weight and better still from 4 to 20% by weight, with respect to the total weight of said composition.
• These contents are in particular suitable for compositions in the form of emulsions and especially for compositions in the form of W/O emulsions, such as liquid foundations.
• composition according to the invention comprises one or more fillers, in particular at least one inorganic filler.
• inorganic fillers should be understood as meaning colorless or white, lamellar or nonlamellar inorganic particles.
• the inorganic particles can be of any shape, such as in particular potatoid, lamellar, platelet, spherical or oblong. They can be of any crystallographic form (for example sheet, cubic, hexagonal, orthorhombic, and the like).
• silica powder of:
• the inorganic filler is silica, talc or their mixture.
• the composition comprises at least one inorganic filler of potatoid form (that is to say, a form with a surface exhibiting an irregular outline which is pronounced of the longitudinal cross section of a potato), of lamellar form or their mixture.
• the inorganic fillers can be present in the composition in a content which can vary to a large extent according to the nature of the inorganic fillers and also according to the product desired and/or the effects desired; this amount is to be adjusted by a person skilled in the art.
• the inorganic filler(s) can be present in the composition in a content ranging from 0.01 to 50% by weight, in particular from 0.01 to 30% by weight, with respect to the total weight of the composition, preferably ranging from 0.01 to 20% by weight.
• the inorganic filler(s) can be present in the composition in a content ranging from 1 to 50% by weight, with respect to the total weight of the composition, and better still from 2 to 35% by weight.
• the composition according to the invention additionally comprises at least one other filler.
• Said at least one other filler can be inorganic or organic. It is thus possible for a mixture of inorganic or organic fillers to be involved.
• composition according to the invention can comprise an inorganic filler and another inorganic filler, said inorganic fillers being as defined above, and optionally at least one organic filler, as defined below.
• composition according to the invention can comprise an inorganic filler and an organic filler.
• organic fillers should be understood as meaning colorless or white, and lamellar or nonlamellar organic particles. Mention may in particular be made of powders formed of polyamide (Nylon® or Orgasol® from Arkema), powders formed of acrylic polymers, in particular powders formed of polymethyl methacrylate, of poly(methyl methacrylate/ethylene glycol dimethacrylate), of poly(allyl methacrylate/ethylene glycol dimethacrylate) or of ethylene glycol dimethacrylate/lauryl methacrylate copolymer, powders formed of cellulose, of poly- ⁇ -alanine and of polyethylene, powders formed of tetrafluoroethylene polymers (Teflon®), lauroyl lysine, starch, hollow polymeric microspheres, such as those of poly(vinylidene chloride/acrylonitrile), such as Expancel® (Nobel Industrie), or of acrylic acid copolymers (Polytrap® from Dow Corning),
• silicone elastomer powder of the powders sold under the names “Trefil® Powder E-505C” and “Trefil® Powder E-506C” by Dow Corning.
• the organic filler corresponds to polyamide powders.
• the amount of fillers can vary to a large extent according to the nature of the filler and also according to the product desired and/or the effects desired; this amount is to be adjusted by a person skilled in the art.
• the filler(s) can be present in the composition in a content ranging from 0.01 to 50% by weight, in particular from 0.01 to 30% by weight, with respect to the total weight of the composition, preferably ranging from 0.01 to 20% by weight.
• the filler(s) can be present in the composition in a content ranging from 1 to 50% by weight, with respect to the total weight of the composition, and better still from 2 to 35% by weight.
• composition according to the invention comprises inorganic fillers and other fillers of organic type
• they will be in said composition in an inorganic fillers/organic fillers ratio by weight preferably of greater than or equal to 1.
• compositions capable of being employed in a method according to the invention comprising, in a physiologically acceptable medium, at least one siloxane resin as defined above and at least one inorganic filler as defined above, optionally additionally comprising at least one organic filler as defined above.
• composition according to the invention can comprise one or more other components and in particular oils, pasty compounds, hard or soft waxes, rheological additives, coloring materials, in particular pigments or pearlescent agents, which are or not surface-treated with a hydrophobic agent, polymers, in particular those comprising saccharide or carboxylate groups, or their mixture.
• compositions according to the invention can additionally comprise at least one polymer which may or may not be film-forming.
• the term “film-forming polymer” is understood to mean a polymer capable of forming, by itself alone or in the presence of an additional agent which is able to form a film, a film which is macroscopically continuous and which adheres to keratinous substances, and preferably a cohesive film, and better still a film having a cohesion and mechanical properties such that said film can be isolable and handleable in isolation, for example when said film is produced by casting on a nonstick surface, such as a Teflon- or silicone-treated surface.
• the composition can comprise an aqueous phase and the additional polymer can be present in this aqueous phase.
• the additional polymer will preferably be a polymer in dispersion or an amphiphilic or associative polymer.
• polymer in dispersion is understood to mean water-insoluble polymers present in the form of particles of variable size.
• the polymer may or may not be crosslinked.
• the mean particle size is typically between 25 and 500 nm, preferably between 50 and 200 nm.
• the following polymers in aqueous dispersion can be used: Ultrasol 2075 from Ganz Chemical, Daitosol 5000AD from Daito Kasei, Avalure UR 450 from Noveon, DynamX from National Starch, Syntran 5760 from Interpolymer, Acusol OP 301 from Röhm & Haas or Neocryl A 1090 from Avecia.
• Neocryl XK-90® The acrylic dispersions sold under the names Neocryl XK-90®, Neocryl A-1070®, Neocryl A-1090®, Neocryl BT-62®, Neocryl A-1079® and Neocryl A-523® by Avecia-Neoresins, Dow Latex 432® by Dow Chemical, Daitosol 5000 AD® or Daitosol 5000 SJ® by Daito Kasey Kogyo; Syntran 5760® by Interpolymer, Soltex OPT by Röhm & Haas, the aqueous dispersions of acrylic or styrene/acrylic polymers sold under the trade name Joncryl® by Johnson Polymer or also the aqueous polyurethane dispersions sold under the names Neorez R-981® and Neorez R-974® by Avecia-Neoresins, the names Avalure UR-405®, Avalure UR-410®, Avalure UR-425®, Avalure UR-
• amphiphilic or associative polymers is understood to mean polymers comprising one or more hydrophilic parts which render them partially soluble in water and one or more hydrophobic parts via which the polymers form an association or interact.
• the following associative polymers can be used: Nuvis FX1100 from Elementis, Aculyn 22, Aculyn 44, Aculyn 46 from Röhm & Haas or Viscophobe DB1000 from Amerchol.
• Diblock copolymers composed of a hydrophilic block (polyacrylate, polyethylene glycol) and of a hydrophobic block (polystyrene, polysiloxane) can also be used.
• Polymers soluble in an aqueous phase comprising monodisperse particles shall be avoided as they can bring about aggregation of the monodisperse particles.
• the film-forming polymer can thus be insoluble in such an aqueous phase.
• the composition can comprise an oily phase and the film-forming polymer can be present in this oily phase.
• the polymer can then be in dispersion or in solution.
• Polymers of NAD (nonaqueous dispersion) type or microgels (for example KSGs) can be used, and also polymers of the silicone-modified polyamide type or styrene-based copolymers (Kraton, Regalite).
• nonaqueous dispersions of fat-dispersible film-forming polymer in the form of nonaqueous dispersions of polymer particles in one or more silicone and/or hydrocarbon oils, which particles can be stabilized at their surface by at least one stabilizing agent, in particular a block, grafted or random polymer, of acrylic dispersions in isododecane, such as Mexomer PAP® from Chimex, or dispersions of particles of a grafted ethylenic polymer, preferably an acrylic polymer, in a liquid fatty phase, the ethylenic polymer advantageously being dispersed in the absence of additional stabilizer at the surface of the particles, such as described in particular in the document WO 04/055081.
• a stabilizing agent in particular a block, grafted or random polymer, of acrylic dispersions in isododecane, such as Mexomer PAP® from Chimex
• dispersions of particles of a grafted ethylenic polymer
• film-forming polymers which can be used in the composition of the present invention, of synthetic polymers of radical type or of polycondensate type, polymers of natural origin, and their blends.
• radical film-forming polymer is understood to mean a polymer obtained by polymerization of monomers possessing unsaturation, in particular ethylenic unsaturation, each monomer being capable of homopolymerizing.
• the film-forming polymers of radical type can in particular be vinyl polymers or copolymers, in particular acrylic polymers.
• the film-forming vinyl polymers can result from the polymerization of monomers possessing ethylenic unsaturation having at least one acid group and/or of the esters of these acidic monomers and/or of the amides of these acidic monomers.
• Use may be made, as monomer carrying an acid group, of unsaturated ⁇ , ⁇ -ethylenic carboxylic acids, such as acrylic acid, methacrylic acid, crotonic acid, maleic acid or itaconic acid.
• Use is preferably made of (meth)acrylic acid and crotonic acid and more preferentially of (meth)acrylic acid.
• esters of acidic monomers are advantageously chosen from esters of (meth)acrylic acid (also known as (meth)acrylates), in particular alkyl (meth)acrylates, especially C 1 -C 30 alkyl (meth)acrylates, preferably C 1 -C 20 alkyl (meth)acrylates, aryl (meth)acrylates, in particular C 6 -C 10 aryl (meth)acrylates, or hydroxyalkyl (meth)acrylates, in particular C 2 -C 6 hydroxyalkyl (meth)acrylates.
• esters of (meth)acrylic acid also known as (meth)acrylates
• alkyl (meth)acrylates especially C 1 -C 30 alkyl (meth)acrylates, preferably C 1 -C 20 alkyl (meth)acrylates, aryl (meth)acrylates, in particular C 6 -C 10 aryl (meth)acrylates, or hydroxyalkyl (meth)acrylates, in particular C 2
• alkyl (meth)acrylates of methyl methacrylate, ethyl methacrylate, butyl methacrylate, isobutyl methacrylate, 2-ethylhexyl methacrylate, lauryl methacrylate or cyclohexyl methacrylate.
• hydroxyalkyl (meth)acrylates of hydroxyethyl acrylate, 2-hydroxypropyl acrylate, hydroxyethyl methacrylate or 2-hydroxypropyl methacrylate.
• aryl (meth)acrylates of benzyl acrylate and phenyl acrylate.
• esters of (meth)acrylic acid which are particularly preferred are alkyl (meth)acrylates.
• the alkyl group of the esters can be either fluorinated or perfluorinated, that is to say that a portion or all of the hydrogen atoms of the alkyl group are substituted by fluorine atoms.
• amides of the acidic monomers for example, of (meth)acrylamides, in particular N-alkyl(meth)acrylamides, especially N—(C 2 -C 12 alkyl)(meth)acrylamides. Mention may be made, among N-alkyl(meth)acrylamides, of N-ethylacrylamide, N-(t-butyl)acrylamide, N-(t-octyl)acrylamide and N-undecylacrylamide.
• the film-forming vinyl polymers can also result from the homopolymerization or from the copolymerization of monomers chosen from vinyl esters and styrene monomers.
• these monomers can be polymerized with acidic monomers and/or their esters and/or their amides, such as those mentioned above.
• vinyl esters of vinyl acetate, vinyl neodecanoate, vinyl pivalate, vinyl benzoate and vinyl t-butylbenzoate.
• styrene monomers of styrene and ⁇ -methylstyrene.
• the polyurethanes can be chosen from anionic, cationic, nonionic or amphoteric polyurethanes, polyurethane-acrylics, polyurethane-polyvinylpyrrolidones, polyester-polyurethanes, polyether-polyurethanes, polyureas, polyurea-polyurethanes, and their blends.
• polyesters can be obtained in a known way by polycondensation of dicarboxylic acids with polyols, in particular diols.
• the dicarboxylic acid can be aliphatic, alicyclic or aromatic. Mention may be made, as examples of such acids, of: oxalic acid, malonic acid, dimethylmalonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, 2,2-dimethylglutaric acid, azelaic acid, suberic acid, sebacic acid, fumaric acid, maleic acid, itaconic acid, phthalic acid, dodecanedioic acid, 1,3-cyclohexanedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid, isophthalic acid, terephthalic acid, 2,5-norbornanedicarboxylic acid, diglycolic acid, thiodipropionic acid, 2,5-naphthalenedicarboxylic acid or 2,6-naphthalenedicarboxylic acid. These dicarboxylic acid monomers can be used alone or as a combination of at
• the diol can be chosen from aliphatic, alicyclic or aromatic diols. Use is preferably made of a diol chosen from: ethylene glycol, diethylene glycol, triethylene glycol, 1,3-propanediol, cyclohexanedimethanol or 4-butanediol. Use may be made, as other polyols, of glycerol, pentaerythritol, sorbitol or trimethylolpropane.
• Polyesteramides can be obtained analogously to the polyesters by polycondensation of diacids with diamines or amino alcohols. Use may be made, as diamines, of ethylenediamine, hexamethylenediamine, meta-phenylenediamine or para-phenylenediamine. Use may be made, as amino alcohol, of monoethanolamine.
• the polyester can additionally comprise at least one monomer carrying at least one —SO 3 M group, with M representing a hydrogen atom, an ammonium ion NH 4 + or a metal ion, such as, for example, an Na + , Li + , K + , Mg 2+ , Ca 2+ , Cu 2+ , Fe 2+ or Fe 3+ ion.
• M representing a hydrogen atom, an ammonium ion NH 4 + or a metal ion, such as, for example, an Na + , Li + , K + , Mg 2+ , Ca 2+ , Cu 2+ , Fe 2+ or Fe 3+ ion.
• Use may in particular be made of a bifunctional aromatic monomer comprising such an —SO 3 M group.
• the aromatic ring system of the bifunctional aromatic monomer additionally carrying an —SO 3 M group as described above can be chosen, for example, from the benzene, naphthalene, anthracene, biphenyl, oxydiphenyl, sulfonyldiphenyl or methylenediphenyl ring systems. Mention may be made, as example of bifunctional aromatic monomer additionally carrying an —SO 3 M group, of: sulfoisophthalic acid, sulfoterephthalic acid, sulfophthalic acid or 4-sulfonaphthalene-2,7-dicarboxylic acid.
• the film-forming polymer can be a polymer dissolved in a liquid fatty phase comprising oils or organic solvents (the film-forming polymer is then described as a fat-soluble polymer).
• the liquid fatty phase comprises a volatile oil, optionally as a mixture with a nonvolatile oil.
• fat-soluble polymer of copolymers of vinyl ester (the vinyl group being directly connected to the oxygen atom of the ester group and the vinyl ester having a saturated, linear or branched, hydrocarbon radical of 1 to 19 carbon atoms bonded to the carbonyl of the ester group) and of at least one other monomer which can be a vinyl ester (other than the vinyl ester already present), an ⁇ -olefin (having from 8 to 28 carbon atoms), an alkyl vinyl ether (the alkyl group of which comprises from 2 to 18 carbon atoms) or an allyl or methallyl ester (having a saturated, linear or branched, hydrocarbon radical of 1 to 19 carbon atoms bonded to the carbonyl of the ester group).
• vinyl ester the vinyl group being directly connected to the oxygen atom of the ester group and the vinyl ester having a saturated, linear or branched, hydrocarbon radical of 1 to 19 carbon atoms bonded to the carbonyl of the ester group
• copolymers can be crosslinked using crosslinking agents which can be either of the vinyl type or of the allyl or methallyl type, such as tetraallyloxyethane, divinylbenzene, divinyl octanedioate, divinyl dodecanedioate and divinyl octadecanedioate.
• crosslinking agents which can be either of the vinyl type or of the allyl or methallyl type, such as tetraallyloxyethane, divinylbenzene, divinyl octanedioate, divinyl dodecanedioate and divinyl octadecanedioate.
• fat-soluble film-forming polymers of copolymers of a vinyl ester and of at least one other monomer which can be a vinyl ester, in particular vinyl neodecanoate, vinyl benzoate and vinyl t-butylbenzoate, an ⁇ -olefin, an alkyl vinyl ether or an allyl or methallyl ester.
• fat-soluble film-forming polymers of fat-soluble copolymers and in particular those resulting from the copolymerization of vinyl esters having from 9 to 22 carbon atoms or of alkyl acrylates or methacrylates, the alkyl radicals having from 10 to 20 carbon atoms.
• Such fat-soluble copolymers can be chosen from copolymers of poly(vinyl stearate), of poly(vinyl stearate) crosslinked using divinylbenzene, diallyl ether or diallyl phthalate, copolymers of poly(stearyl (meth)acrylate), of poly(vinyl laurate), of poly(lauryl (meth)acrylate), it being possible for these poly(meth)acrylates to be crosslinked using ethylene glycol dimethacrylate or tetraethylene glycol dimethacrylate.
• the fat-soluble copolymers defined above are known and are described in particular in application FR-A-2 232 303; they can have a weight-average molecular weight ranging from 2000 to 500 000 and preferably from 4000 to 200 000.
• fat-soluble film-forming polymers which can be used in the invention, of polyalkylenes and in particular copolymers of C 2 -C 20 alkenes, such as polybutene, alkylcelluloses with a saturated or unsaturated and linear or branched C 1 to C 8 alkyl radical, such as ethylcellulose and propylcellulose, copolymers of vinylpyrrolidone (VP) and in particular copolymers of vinylpyrrolidone and of C 2 to C 40 alkene and better still C 3 to C 20 alkene.
• polyalkylenes and in particular copolymers of C 2 -C 20 alkenes such as polybutene
• alkylcelluloses with a saturated or unsaturated and linear or branched C 1 to C 8 alkyl radical such as ethylcellulose and propylcellulose
• VP copolymer which can be used in the invention, of the VP/vinyl acetate, VP/ethyl methacrylate, butylated polyvinylpyrrolidone (PVP), VP/ethyl methacrylate/methacrylic acid, VP/eicosene, VP/hexadecene, VP/triacontene, VP/styrene or VP/acrylic acid/lauryl methacrylate copolymer.
• PVP polyvinylpyrrolidone
• silicone resins generally soluble or swellable in silicone oils, which are crosslinked polyorganosiloxane polymers.
• the nomenclature of silicone resins is known under the name of “MDTQ”, the resin being described according to the various siloxane monomer units which it comprises, each of the letters “MDTQ” characterizing one type of unit.
• TMS trimethylsiloxysilicate
• Mention may be made, as siloxysilicate resins, of trimethylsiloxysilicate (TMS) resins, such as those sold under the reference SR1000 by General Electric or under the reference TMS 803 by Wacker. Mention may also be made of trimethylsiloxysilicate resins sold in a solvent, such as cyclomethicone, sold under the names KF-7312J by Shin-Etsu or “DC 749” or “DC 593” by Dow Corning.
• TMS trimethylsiloxysilicate
• silicone resins such as those mentioned above with polydimethylsiloxanes
• the pressure-sensitive adhesive copolymers sold by Dow Corning under the reference BIO-PSA and described in the document U.S. Pat. No. 5,162,410 or the silicone copolymers resulting from the reaction of a silicone resin, such as those described above, and of a diorganosiloxane, such as are described in the document WO 2004/073626.
• the film-forming polymer can be a film-forming linear ethylenic block polymer which preferably comprises at least one first block and at least one second block having different glass transition temperatures (Tg), said first and second blocks being connected to one another via an intermediate block comprising at least one constituent monomer of the first block and at least one constituent monomer of the second block.
• Tg glass transition temperatures
• the first and second blocks of the block polymer are incompatible with one another.
• Such polymers are described, for example, in the documents EP 1 411 069 and WO 04/028488.
• the film-forming polymer can be chosen from polymers and/or block or random copolymers comprising in particular polyurethanes, polyacrylics, silicones, fluoropolymers, butyl rubbers, ethylene copolymers, natural gums and polyvinyl alcohols and their blends.
• the monomers of the block or random copolymers comprising at least one combination of monomers, the polymer of which results in a glass transition temperature below ambient temperature (25° C.), can be chosen in particular from butadiene, ethylene, propylene, acrylic, methacrylic, isoprene, isobutene, a silicone and their mixtures.
• the film-forming polymer can also be present in the composition in the form of particles in dispersion in an aqueous phase or in a nonaqueous solvent phase, generally known under the name of latex or pseudolatex.
• the techniques for the preparation of these dispersions are well known to a person skilled in the art.
• composition according to the invention can comprise a plasticizing agent which promotes the formation of a film with the film-forming polymer.
• a plasticizing agent can be chosen from all the compounds known to a person skilled in the art as being capable of performing the desired role.
• a film-forming system which can be used in the compositions according to the invention, of the systems in which the film is formed in situ during the application of the composition or of a mixture of compositions comprising two silicone compounds which react when they are brought into contact with one another.
• Such systems are described in particular in application WO 2007/071706, the content of which is incorporated here by way of reference.
• Systems of this type are also described in applications US 2007/142575 or US 2007/142599, the contents of which are also incorporated here by way of reference.
• compositions according to the invention can comprise an elastomer, in particular a polyglycerolated silicone elastomer.
• an elastomer in particular a polyglycerolated silicone elastomer.
• a crosslinked organopolysiloxane elastomer which can be obtained by a crosslinking addition reaction of a diorganopolysiloxane comprising at least one hydrogen bonded to the silicon and of polyglycerolated compounds having groups possessing ethylenic unsaturation, in particular in the presence of a platinum catalyst.
• compositions according to the invention can in addition comprise an additional emulsifying silicone elastomer.
• polyoxyalkylenated silicone elastomer of those sold under the names “KSG-21”, “KSG-20”, “KSG-30”, “KSG-31”, KSG-32′′, “KSG-33”, “KSG-210”, “KSG-310”, “KSG-320”, “KSG-330”, “KSG-340” and “X-226146” by Shin-Etsu and “DC9010” and “DC9011” by Dow Corning.
• compositions according to the invention can additionally comprise a nonemulsifying elastomer.
• the spherical nonemulsifying silicone elastomer can also be provided in the form of a crosslinked organopolysiloxane elastomer powder coated with silicone resin, in particular with silsesquioxane resin, as described, for example, in U.S. Pat. No. 5,538,793, the content of which is incorporated by way of reference.
• Such elastomers are sold under the names “KSP-100”, “KSP-101”, “KSP-102”, “KSP-103”, “KSP-104” and “KSP-105” by Shin-Etsu.
• crosslinked organopolysiloxane elastomers in the form of spherical powders can be powders formed of hybrid silicone functionalized by fluoroalkyl groups, sold in particular under the name “KSP-200” by Shin-Etsu; or powders formed of hybrid silicone functionalized by phenyl groups, sold in particular under the name “KSP-300” by Shin-Etsu.
• silicone elastomers with an MQ group such as those sold by Wacker under the names Belsil RG100, Belsil RPG33 and, preferably, Belsil RG80.
• MQ group such as those sold by Wacker under the names Belsil RG100, Belsil RPG33 and, preferably, Belsil RG80.
• composition according to the invention can comprise at least one structuring agent.
• structuring agent is understood to mean a compound capable of increasing the viscosity of the composition.
• the structuring agent makes it possible in particular to obtain a composition which can exhibit a texture ranging from fluid textures to solid textures.
• the structuring agent can be present in the composition in a content ranging from 0.05% to 40% by weight, with respect to the total weight of the composition, preferably ranging from 0.1% to 30% by weight and preferentially ranging from 0.1% to 25% by weight.
• the structuring agent can be chosen in particular from thickeners (thickeners for an oily medium; thickeners for an aqueous medium), organic gelling agents, waxes, pasty compounds or gums.
• the thickening agent for an aqueous medium can be chosen from:
• the thickening agent for an oily medium can be chosen from:
• organic gelling agents can be chosen from those described in application WO-A-03/105788, the content of which is incorporated by way of reference.
• the structuring agents can be composed of waxes.
• wax is understood to mean, within the meaning of the present invention, a lipophilic compound which is solid at ambient temperature (25° C.), which exhibits a reversible solid/liquid change in state and which has a melting point of greater than or equal to 30° C. which can range up to 120° C.
• the melting point of the wax can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name DSC 30 by Mettler.
• DSC differential scanning calorimeter
• the wax can also exhibit a hardness ranging from 0.05 MPa to 15 MPa and preferably ranging from 6 MPa to 15 MPa.
• the hardness is determined by the measurement of the compressive force measured at 20° C. using the texture analyzer sold under the name TA-TX21 by Rheo, equipped with a stainless steel cylinder with a diameter of 2 mm which is displaced at the measuring rate of 0.1 mm/s and which penetrates the wax to a penetration depth of 0.3 mm.
• the waxes can be hydrocarbon, fluorinated and/or silicone waxes and can be of vegetable, mineral, animal and/or synthetic origin.
• the waxes exhibit a melting point of greater than 30° C. and better still of greater than 45° C.
• wax which can be used in the composition of the invention, of beeswax, carnauba wax, candelilla wax, paraffin wax, microcrystalline waxes, rice bran wax, olive waxes (photowax olive 14L48, photowax olive 18L57), ceresin or ozokerite; synthetic waxes, such as polyethylene waxes or Fischer-Tropsch waxes, or silicone waxes, such as alkyl or alkoxy dimethicones having from 16 to 45 carbon atoms.
• wax which can be used in the composition of the invention, of beeswax, carnauba wax, candelilla wax, paraffin wax, microcrystalline waxes, rice bran wax, olive waxes (photowax olive 14L48, photowax olive 18L57), ceresin or ozokerite; synthetic waxes, such as polyethylene waxes or Fischer-Tropsch waxes, or silicone waxes, such as alkyl or alkoxy dimethicones
• the composition can comprise from 0.1 to 50% by weight of waxes, with respect to the total weight of the composition, and better still from 1 to 30% by weight.
• the gums are generally high molecular weight polydimethylsiloxanes (PDMSs) or cellulose gums or polysaccharides.
• composition according to the invention can comprise at least one surfactant.
• the surfactant can be lipophilic and/or hydrophilic, and used alone or as a blend.
• the surfactant can be chosen from nonionic, anionic, cationic or amphoteric surfactants.
• the nonionic surfactant can be chosen from:
• the C 8 -C 22 alkyl dimethicone copolyol is advantageously a compound of following formula (VI):
• C 8 -C 22 alkyl dimethicone copolyol of cetyl dimethicone copolyol, such as the product sold under the name Abil EM-90 by Goldschmidt.
• R 1 , R 2 and R 3 represent, independently of one another, a C 1 -C 6 alkyl radical or a —(CH 2 ) x —(OCH 2 CH 2 ) y —(OCH 2 CH 2 CH 2 ) z —OR 4 radical, at least one R 1 , R 2 or R 3 radical not being an alkyl radical; R 4 being a hydrogen, a C 1 -C 3 alkyl radical or a C 2 -C 4 acyl radical; A is an integer ranging from 0 to 200; B is an integer ranging from 0 to 50; provided that A and B are not simultaneously equal to zero; x is an integer ranging from 1 to 6; y is an integer ranging from 1 to 30; z is an integer ranging from 0 to 5.
• R 1 ⁇ R 3 methyl radical
• x is an integer ranging from 2 to 6
• y is an integer ranging from 4 to 30.
• R 4 is in particular a hydrogen.
• A is an integer ranging from 20 to 105
• B is an integer ranging from 2 to 10
• y is an integer ranging from 10 to 20.
• A′ and y are integers ranging from 10 to 20.
• Use may be made, as dimethicone copolyol, of those sold under the names DC 5329, DC 7439-146, DC2-5695 and Q4-3667 by Dow Corning and KF-6013, KF-6015, KF-6016 and KF-6017 by Shin-Etsu.
• the compounds DC 5329, DC 7439-146 and DC 2 -5695 are compounds of formula (VIII) where, respectively, A is 22, B is 2 and y is 12, A is 103, B is 10 and y is 12, and A is 27, B is 3 and y is 12.
• polyol fatty acid esters such as sorbitol mono-, di-, tri- or sesqui-oleates or -stearates, glycerol mono-, di-, tri- or sesqui-oleates or -stearates, or glycerol or polyethylene glycol laurates; polyethylene glycol fatty acid esters (polyethylene glycol monostearate or monolaurate); polyoxyethylenated sorbitol fatty acid esters (stearate, oleate); or polyoxyethylenated alkyl (lauryl, cetyl, stearyl, octyl)ethers.
• polyol fatty acid esters such as sorbitol mono-, di-, tri- or sesqui-oleates or -stearates, glycerol mono-, di-, tri- or sesqui-oleates or -stearates, or glycerol or polyethylene glycol laurates; poly
• carboxylates sodium 2-(2-hydroxyalkyloxy)acetate
• amino acid derivatives N-acylglutamates, N-acyl
• amphoteric and zwitterionic surfactant of betaines, N-alkyl amido betaines and their derivatives, glycine derivatives, sultaines, alkyl polyaminocarboxylates, alkyl amphoacetates, and their mixtures.
• the surfactant can be present in the composition according to the invention in a content ranging from 0.1% to 10% by weight, with respect to the total weight of the composition, preferably ranging from 0.5% to 8% by weight and preferentially ranging from 0.5% to 7% by weight.
• composition according to the invention can additionally comprise at least one coloring material.
• the coloring material can be chosen from pulverulent coloring materials (in particular pigments and pearlescent agents) or water-soluble or fat-soluble coloring materials.
• the pigments can be white or colored and inorganic and/or organic. Mention may be made, among inorganic pigments, of titanium dioxide, zirconium or cerium oxides, and also zinc, iron (black, yellow or red) or chromium oxides, manganese violet, ultramarine blue, chromium hydrate and ferric blue, or metal powders, such as aluminum powder or copper powder.
• effect pigments such as particles comprising an organic or inorganic and natural or synthetic substrate, for example glass, acrylic resins, polyester, polyurethane, polyethylene terephthalate, ceramics or aluminas, said substrate being covered or not being covered with metal substances, such as aluminum, gold, silver, platinum, copper or bronze, or with metal oxides, such as titanium dioxide, iron oxide or chromium oxide, and their mixtures.
• the pearlescent pigments can be chosen from white pearlescent pigments, such as mica covered with titanium oxide or with bismuth oxychloride, colored pearlescent pigments, such as titanium oxide-coated mica covered with iron oxides, titanium oxide-coated mica covered with in particular ferric blue or chromium oxide, or titanium oxide-coated mica covered with an organic pigment of the abovementioned type, and pearlescent pigments based on bismuth oxychloride. Use may also be made of interferential pigments, in particular liquid crystal or multilayer pigments.
• the water-soluble dyes are, for example, beetroot juice or methylene blue.
• the synthetic or natural fat-soluble dyes are, for example, DC Red 17, DC Red 21, DC Red 27, DC Green 6, DC Yellow 11, DC Violet 2, DC Orange 5, Sudan red, carotenes ( ⁇ -carotene, lycopene), xanthophylls (capsanthin, capsorubin, lutein), palm oil, Sudan brown, quinoline yellow, annatto or curcumin.
• the solid particles such as pulverulent coloring materials (pigments and pearlescent agents), can be completely or partially surface-treated with a compound of silicone nature, a compound of fluorinated nature, a compound of fluorinated/silicone nature, a fatty acid or amino acid or one of their mixtures.
• compositions in particular the compositions for making up or caring for the skin and in particular foundations, can comprise at least one solid particle (more specifically pigments and/or pearlescent agents) completely or partially surface-treated with a compound of fluorinated nature, in particular in order to improve the persistence of the color and mattness.
• solid particle more specifically pigments and/or pearlescent agents
• the hydrophobic treatment agent can be chosen from silicones, such as methicones, dimethicones, perfluoroalkylsilanes, perfluoroalkylsilazanes, triethoxycapryloylsilane or triethoxysilylethyl polydimethylsiloxyethyl hexyl dimethicone; fatty acids such as stearic acid; metal soaps, such as aluminum dimyristate or the aluminum salt of hydrogenated tallow glutamate; perfluoroalkyl phosphates, polyhexafluoropropylene oxides, polyorganosiloxanes comprising perfluoroalkyl perfluoropolyether groups or silicone-grafted acrylic polymers (described in particular in application JP-A-05-339125, the content of which is incorporated by way of reference); amino acids; N-acylated amino acids or their salts; lecithin, isopropyl triisostearoyltitan
• the N-acylated amino acids can comprise an acyl group having from 8 to 22 carbon atoms, such as, for example, a 2-ethylhexanoyl, caproyl, lauroyl, myristoyl, palmitoyl, stearoyl or cocoyl group.
• the salts of these compounds can be aluminum, magnesium, calcium, zirconium, zinc, sodium or potassium salts.
• the amino acid can be, for example, lysine, glutamic acid or alanine.
• the fluorinated surface-active agents can be chosen from perfluoroalkyl phosphates, perfluoropolyethers, polytetrafluoroethylenes (PTFEs) and perfluoroalkanes.
• Perfluoroalkyl phosphates are described in particular in application JP H05-86984.
• the diethanolamine perfluoroalkyl phosphates sold by Asahi Glass under the reference AsahiGuard AG530 can be used.
• perfluoroalkanes of the series of the linear alkanes, such as perfluorooctane, perfluorononane or perfluorodecane.
• perfluorocycloalkanes and perfluoro(alkylcycloalkanes) of perfluorodecalin, sold under the name of “Flutec PP5 GMP” by Rhodia, perfluoro(methyldecalin) or perfluoro(C 3 -C 5 alkylcyclohexanes), such as perfluoro(butylcyclohexane).
• perfluoropolycycloalkanes of bicyclo[3.3.1]nonane derivatives, such as perfluorotrimethylbicyclo[3.3.1]nonane, adamantane derivatives, such as perfluorodimethyladamantane, and perfluorinated derivatives of hydrogenated phenanthrene, such as tetracosafluorotetradecahydrophenanthrene.
• bicyclo[3.3.1]nonane derivatives such as perfluorotrimethylbicyclo[3.3.1]nonane
• adamantane derivatives such as perfluorodimethyladamantane
• perfluorinated derivatives of hydrogenated phenanthrene such as tetracosafluorotetradecahydrophenanthrene.
• the coloring materials in particular the pigments, can be present in the composition in a content ranging from 0.1% to 30% by weight, with respect to the total weight of the composition, preferably ranging from 0.5% to 20% by weight and preferentially ranging from 1% to 10% by weight.
• composition can additionally comprise fibers.
• fiber should be understood as meaning an object with a length L and a diameter D such that L is greater than D, D being the diameter of the circle in which the cross section of the fiber is framed.
• L/D ratio or aspect ratio
• the L/D ratio is chosen within the range from 3.5 to 2500, preferably from 5 to 500 and better still from 5 to 150.
• the fibers which can be used in the composition of the invention can be fibers of synthetic or natural and inorganic or organic origin. They can be short or long, individual or organized, for example braided, and hollow or solid. They can have any shape and can in particular be circular or polygonal (square, hexagonal or octagonal) in cross section, according to the specific application envisaged. In particular, their ends are blunted and/or polished to prevent injury.
• the fibers have a length ranging from 1 ⁇ m to 10 mm, preferably from 0.1 mm to 5 mm and better still from 0.3 mm to 3 mm.
• Their cross section can be included within a circle with a diameter ranging from 2 nm to 500 ⁇ m, preferably ranging from 100 nm to 100 ⁇ m and better still from 1 ⁇ m to 50 ⁇ m.
• the weight or count of the fibers is often given in denier or decitex and represents the weight in grams per 9 km of yarn.
• the fibers according to the invention have a count chosen within the range from 0.01 to 10 denier, preferably from 0.1 to 2 denier and better still from 0.3 to 0.7 denier.
• the fibers can be present in the composition in a content ranging from 0.1% to 30% by weight, with respect to the total weight of the composition, preferably ranging from 0.1% to 20% by weight and preferentially ranging from 0.1% to 10% by weight.
• physiologically acceptable medium is intended to denote a medium suitable in particular for the application of a composition of the invention to the skin or its superficial body growths.
• the physiologically acceptable medium is generally suited to the nature of the support on which the composition has to be applied and to the appearance under which the composition has to be packaged.
• composition according to the invention can be provided in various forms, in particular in the form of powders (loose or compact), of an anhydrous composition, of a dispersion, of an emulsion, such as in particular a water/oil, water/wax, oil/water, multiple or wax/water emulsion, or else in the form of a gel.
• a composition of the invention is preferably an emulsion, in particular a direct or inverse emulsion, or an anhydrous composition.
• a dispersion can be produced in an aqueous phase or in an oily phase.
• An emulsion can have an oily or aqueous continuous phase.
• Such an emulsion can, for example, be an inverse (W/O) or direct (0/W) emulsion, or a multiple (W/O/W or O/W/O) emulsion.
• the inverse (W/O) emulsions are preferred.
• An anhydrous composition is a composition comprising less than 2% by weight of water, indeed even less than 0.5% of water, and is in particular devoid of water. If appropriate, amounts of water which are as low can in particular be introduced by ingredients of the composition which may comprise residual amounts thereof.
• composition according to the invention can be provided in the form of a fluid, for example a pasty or liquid fluid. It can also be provided in the form of a loose or compact powder, of a soft paste or of a cream. For example, it can be an oil-in-water, water-in-oil or multiple emulsion, a solid emulsion, in particular of water-in-oil type, a solid or soft gel which is in particular anhydrous, in the loose or compact powder form and even in a two-phase form.
• composition under consideration according to the invention is generally provided in the form of a composition for making up and/or caring for keratinous substances, for example of a foundation, in particular to be applied to the face or the neck, of a concealer, of a complexion corrector, of a tinted cream, of a face powder or of a makeup composition for the body.
• composition according to the invention can comprise at least one aqueous phase.
• the aqueous phase comprises water.
• a water suitable for the invention can be a floral water, such as cornflower water, and/or a mineral water, such as water from Vittel, water from Lucas or water from La Roche Posay, and/or a thermal water.
• the aqueous phase can also comprise water-miscible (at ambient temperature ⁇ 25° C.) organic solvents, such as, for example, monoalcohols having from 2 to 6 carbon atoms, such as ethanol or isopropanol; polyols having in particular from 2 to 20 carbon atoms, preferably having from 2 to 10 carbon atoms, and preferentially having from 2 to 6 carbon atoms, such as glycerol, propylene glycol, butylene glycol, pentylene glycol, hexylene glycol, dipropylene glycol or diethylene glycol; glycol ethers (having in particular from 3 to 16 carbon atoms), such as mono-, di- or tripropylene glycol (C 1 -C 4 )alkyl ethers or mono-, di- or triethylene glycol (C 1 -C 4 )alkyl ethers, and their mixtures.
• organic solvents such as, for example, monoalcohols having from 2 to 6 carbon
• the aqueous phase can additionally comprise stabilizing agents, for example sodium chloride, magnesium dichloride and magnesium sulfate.
• the aqueous phase can also comprise any water-soluble or water-dispersible compound compatible with an aqueous phase, such as gelling agents, film-forming polymers, thickeners, surfactants and their mixtures.
• a composition of the invention can comprise an aqueous phase in a content varying from 1% to 80% by weight, in particular from 5% to 50% by weight and more particularly from 10% to 45% by weight, with respect to the total weight of the composition.
• a composition of the invention can be anhydrous.
• An anhydrous composition can comprise less than 5% by weight of water, with respect to the total weight of the composition, and in particular less than 3% by weight of water, especially less than 2% by weight of water and more particularly less than 1% by weight of water, with respect to the total weight of the composition.
• an anhydrous composition can be devoid of water.
• a cosmetic composition in accordance with the present invention can comprise at least one liquid and/or solid fatty phase.
• composition of the invention can comprise at least one liquid fatty phase, in particular at least one oil, as mentioned below.
• oil is understood to mean any fatty substance in the liquid form at ambient temperature (20-25° C.) and at atmospheric pressure.
• a composition of the invention can comprise a liquid fatty phase in a content varying from 1 to 90% by weight, in particular from 5 to 80% by weight, in particular from 10 to 70% by weight and more particularly from 20 to 50% by weight, with respect to the total weight of the composition.
• the oily phase suitable for the preparation of the cosmetic compositions according to the invention can comprise oils which may or may not be hydrocarbon, silicone or fluorinated oils, or their mixtures.
• the oils can be volatile or nonvolatile.
• They can be of animal, vegetable, mineral or synthetic origin.
• volatile oil is understood to mean an oil (or nonaqueous medium) capable of evaporating on contact with the skin in less than one hour at ambient temperature and at atmospheric pressure.
• the volatile oil is a volatile cosmetic oil which is liquid at ambient temperature and which has in particular a nonzero vapor pressure at ambient temperature and at atmospheric pressure, especially which has a vapor pressure ranging from 0.13 Pa to 40 000 Pa (10 ⁇ 3 to 300 mmHg), preferably ranging from 1.3 Pa to 13 000 Pa (0.01 to 100 mmHg) and preferentially ranging from 1.3 Pa to 1300 Pa (0.01 to 10 mmHg).
• nonvolatile oil is understood to mean an oil having a vapor pressure of less than 0.13 Pa.
• silicon oil is understood to mean an oil comprising at least one silicon atom and in particular at least one Si—O group.
• fluorinated oil is understood to mean an oil comprising at least one fluorine atom.
• hydrocarbon oil is understood to mean an oil comprising mainly hydrogen and carbon atoms.
• the oils can optionally comprise oxygen, nitrogen, sulfur and/or phosphorus atoms, for example in the form of hydroxyl or acid radicals.
• the volatile oils can be chosen from hydrocarbon oils having from 8 to 16 carbon atoms and in particular branched C 3 -C 16 alkanes (also known as isoparaffins), such as isododecane (also known as 2,2,4,4,6-pentamethylheptane), isodecane, isohexadecane and, for example, the oils sold under the Isopars® or Permethyl® trade names.
• hydrocarbon oils having from 8 to 16 carbon atoms and in particular branched C 3 -C 16 alkanes (also known as isoparaffins), such as isododecane (also known as 2,2,4,4,6-pentamethylheptane), isodecane, isohexadecane and, for example, the oils sold under the Isopars® or Permethyl® trade names.
• volatile oils of volatile silicones, such as, for example, volatile linear or cyclic silicone oils, in particular those having a viscosity ⁇ 8 centistokes (cSt) (8 ⁇ 10 ⁇ 6 m 2 /s), and having in particular from 2 to 10 silicon atoms and especially from 2 to 7 silicon atoms, these silicones optionally comprising alkyl or alkoxy groups having from 1 to 10 carbon atoms.
• volatile silicones such as, for example, volatile linear or cyclic silicone oils, in particular those having a viscosity ⁇ 8 centistokes (cSt) (8 ⁇ 10 ⁇ 6 m 2 /s), and having in particular from 2 to 10 silicon atoms and especially from 2 to 7 silicon atoms, these silicones optionally comprising alkyl or alkoxy groups having from 1 to 10 carbon atoms.
• volatile silicone oil which can be used in the invention, of dimethicones with viscosities of 5 and 6 cSt, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, heptamethylhexyltrisiloxane, heptamethyloctyltrisiloxane, hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane, dodecamethylpentasiloxane, and their mixtures.
• Use may also be made of volatile fluorinated oils, such as nonafluoromethoxybutane or perfluoromethylcyclopentane, and their mixtures.
• a composition of the invention can comprise from 1% to 80% by weight, indeed even from 5% to 70% by weight, indeed even from 10% to 60% by weight and in particular from 15% to 50% by weight of volatile oil, with respect to the total weight of the composition.
• the nonvolatile oils can be chosen in particular from nonvolatile fluorinated hydrocarbon oils and/or nonvolatile silicone oils.
• nonvolatile hydrocarbon oil of:
• the fatty phase of the composition according to the invention can comprise only volatile compounds.
• composition according to the invention can comprise at least one pasty compound.
• Such a compound can advantageously be chosen from lanolin and its derivatives; polymeric or nonpolymeric silicone compounds; polymeric or nonpolymeric fluorinated compounds; vinyl polymers, in particular olefin homopolymers; olefin copolymers; homopolymers and copolymers of hydrogenated dienes; linear or branched oligomers which are homo- or copolymers of alkyl (meth)acrylates preferably having a C 8 -C 30 alkyl group; oligomers which are homo- and copolymers of vinyl esters having C 8 -C 30 alkyl groups; oligomers which are homo- and copolymers of vinyl ethers having C 8 -C 30 alkyl groups; fat-soluble polyethers resulting from the polyetherification between one or more C 2 -C 100 , in particular C 2 -C 50 diols; fatty alcohol or acid esters; and their mixtures.
• esters of:
• the pasty compound or compounds can be present in a composition of the invention in a content ranging from 0.1 to 30% by weight of agents, more preferably from 0.5 to 20% by weight, with respect to the total weight of the composition.
• composition according to the invention can also comprise ingredients commonly used in cosmetics, such as vitamins, thickeners, trace elements, softeners, sequestering agents, fragrances, basifying or acidifying agents, preservatives, sunscreens, surfactants, antioxidants, agents for combating hair loss, antidandruff agents, propellants, or their mixtures.
• ingredients commonly used in cosmetics such as vitamins, thickeners, trace elements, softeners, sequestering agents, fragrances, basifying or acidifying agents, preservatives, sunscreens, surfactants, antioxidants, agents for combating hair loss, antidandruff agents, propellants, or their mixtures.
• a composition according to the invention can in particular be provided in the form of a composition for making up and/or caring for the skin, in particular a foundation.
• the invention also relates to a cosmetic combination comprising:
• the container can have any appropriate form. It can in particular be in the form of a bottle, a tube, a pot, a box, a tin, a bag or a case.
• the closing element can be in the form of a removable stopper, of a lid, of a seal, of a tear-off strip or of a capsule, in particular of the type comprising a body fixed to the container and a cap articulated over the body. It can also be in the form of an element providing the selective closure of the container, in particular a pump, a valve or a flap.
• the container can be used in combination with an applicator, in particular in the form of a brush comprising an arrangement of hairs held by a twisted wire.
• a twisted brush is described in particular in U.S. Pat. No. 4,887,622.
• It can also be in the form of a comb comprising a plurality of application elements, obtained in particular from molding. Such combs are described, for example, in patent FR 2 796 529.
• the applicator can be in the form of a fine brush, such as described, for example, in patent FR 2 722 380.
• the applicator can be in the form of a pad of foam or elastomer, of a felt-tipped pen or of a spatula.
• the applicator can be free (powder puff or sponge) or integrally attached to a rod carried by the closing element, such as described, for example, in U.S. Pat. No. 5,492,426.
• the applicator can be integrally attached to the container, such as described, for example, in patent FR 2 761 959.
• the product may be contained directly in the container or indirectly.
• the product can be positioned on an impregnated support, particularly in the form of a wipe or of a wad, and can be positioned (singly or severally) in a tin or in a bag.
• an impregnated support particularly in the form of a wipe or of a wad
• Such a support incorporating the product is described, for example, in application WO 01/03538.
• the closing element can be coupled to the container by screwing.
• the coupling between the closing element and the container is carried out other than by screwing, in particular via a bayonet mechanism, by snapping, clamping, welding or adhesive bonding, or by magnetic attraction.
• the term “snapping” is understood to mean in particular any system involving the crossing of a row or strip of material by elastic deformation of a portion, in particular of the closing element, and then by elastically returning said portion to the unstressed position after the row or strip has been crossed.
• the container can be at least partially made of thermoplastic material. Mention may be made, as examples of thermoplastic materials, of polypropylene or polyethylene.
• the container is made of non-thermoplastic material, in particular of glass or of metal (or alloy).
• the container can have rigid walls or deformable walls, in particular in the form of a tube or of a tube bottle.
• the container can comprise means intended to bring about or facilitate the distribution of the composition.
• the container can have deformable walls, so as to bring about the departure of the composition in response to excess pressurization inside the container, which excess pressurization is brought about by the elastic (or non-elastic) crushing of the walls of the container.
• the container can comprise a mechanism, in particular a rack-and-pinion mechanism or a mechanism with a screw rod or a mechanism with a helical groove, capable of moving a stick in the direction of said opening.
• a mechanism is described, for example, in patent FR 2 806 273 or in patent FR 2 775 566.
• Such a mechanism for a liquid product is described in patent FR 2 727 609.
• the container can be composed of a case with a bottom delimiting at least one receptacle comprising the composition and a lid, in particular articulated over the bottom, capable of at least partially covering said bottom.
• a case is described, for example, in application WO 03/018423 or in patent FR 2 791 042.
• the container can be equipped with a drainer positioned in the vicinity of the opening of the container.
• a drainer makes it possible to wipe the applicator and optionally the rod to which it may be integrally attached.
• a drainer is described, for example, in patent FR 2 792 618.
• the composition can be at atmospheric pressure inside the container (at ambient temperature) or pressurized, in particular using a propellent gas (aerosol).
• a propellent gas in particular using a propellent gas (aerosol).
• the container is equipped with a valve (of the type of those used for aerosols).
• composition of the invention can be provided in the form of a product for caring for or preferably making up, in particular in colored form, the skin, more specifically the face, such as a foundation, a face powder, an eyeshadow, a concealer, a blush, or a loose or compact powder, or alternatively a product for making up the body, such as a semi-permanent tattooing product.
• composition according to the invention can be manufactured by known processes used generally in the cosmetics field.
• the present invention also relates to a method, more specifically a cosmetic method, for caring for or in particular making up the skin and/or superficial body growths (in particular hair or nails) comprising the application of a composition according to the invention described above to the skin and/or its superficial body growths.
• the MQ resin was manufactured according to the techniques described by Daudt in patent U.S. Pat. No. 2,676,182.
• Propyl T resin a propyl silsesquioxane resin at 74.8% by weight in toluene.
• the propyl silsesquioxane resin was obtained by hydrolysis of propyltrichlorosilane.
• An MQ resin, a propyl T resin, xylene and 1M KOH in water, in the proportions shown in table 1, are introduced into a three-necked flask equipped with a stirrer, with a temperature probe and Dean and Stark apparatus equipped with a condenser at the top.
• Xylene is preintroduced into the Dean and Stark apparatus in order to ensure that a level of solids at 50% is maintained in the reactor.
• the mixture in the reactor is maintained at a reflux temperature (between 100 and 140° C.) for at least 3 hours. Any water which is formed in the reaction mixture is continuously removed, if appropriate, and trapped in the form of an azeotrope in the Dean and Stark apparatus.
• Example 3 Example 4 % by % by weight weight Example 2 (according (according Example 5 % by weight to the to the % by weight (comparative) invention) invention) (comparative) A1 Bis-PEG/PPG-14/14 Dimethicone & Cyclopentasiloxane 1.8 1.8 1.8 1.8 (Abil EM97 from Goldschmidt) Isostearyl Diglyceryl Succinate (Inwitor 780K from Sasol) 0.6 0.6 0.6 0.6 PEG-10 Dimethicone 0.5 0.5 0.5 0.5 0.5 Isododecane 13.32 13.32 13.32 13.32 Disteardimonium Hectorite & Propylene Carbonate 5 5 5 5 (bentone gel ISD V from Elementis) Dicaprylyl carbonate (Cetiol CC from Cognis) 6 6 6 6 6 MQ/Propyl T resin 30:70, as prepared according to example 11.38 11.38 11.38 11.38 1-c described above,
• Examples 3 and 4 correspond to compositions according to the invention.
• Examples 2 and 5 are comparative examples.
• phase A2 The constituents of phase A2 are weighed out.
• the mixture is passed through a triple roll mill.
• the constituents of phase A1 are subsequently weighed out into the main beaker and the latter is placed in a water bath (75-80° C.). When the mixture is homogeneous, it is cooled to ambient temperature.
• phase A2 is incorporated in phase A1 with stirring with a Moritz stirrer at 1500 revolutions/min.
• the constituents of phase A3 are then successively added while retaining the same stirring.
• phase B The constituents of phase B are weighed out. Phase B is brought to boiling, until the constituents have completely dissolved. Phase B is cooled to 50° C.
• Phase B is subsequently trickled into phase A1+A2+A3 while stirring with a Moritz stirrer at 3200 rev/min.
• the mattness and the persistence of the mattness can be measured using the protocol described below.
• the mattness of a region of the skin is measured using a polarimetric camera, which is a black and white polarimetric imaging system, with which images are acquired in parallel (P) and crossed (C) polarized light.
• a polarimetric camera which is a black and white polarimetric imaging system, with which images are acquired in parallel (P) and crossed (C) polarized light.
• the shine is quantified by measuring the mean level of gray of the 5% of shiniest pixels corresponding to the regions of shine.
• the measurements are carried out on a panel of individuals who are kept in an air-conditioned (22° C.+/ ⁇ 2° C.) waiting room for 15 min before the beginning of the test. They remove their makeup and an image of one of their cheeks is acquired with the polarimetric camera. This image makes it possible to measure the shine at T0 before applying makeup. Approximately 100 mg of each cosmetic composition as prepared above are then weighed out into a watch glass and are applied with the bare fingers to the half of the face on which the T0 measurement was carried out.
• the results are expressed by calculating the difference (Timm ⁇ T0), which measures the effect of the makeup.
• a negative value means that the makeup reduces the shine of the skin and that it is thus mattifying.
• the difference (T3 h ⁇ Timm) measuring the persistence of this effect is subsequently calculated.
• the value obtained should be as low as possible, which means that the mattness of the makeup does not change over time.
• Each image obtained with the camera is made use of in color.
• the color is quantified by the red and yellow indices, the brightness and the color difference (respectively a*,b*, L* and deltaE).
• the deltaE, dE or ⁇ E is defined as a measurement of difference between two colors.
• the formula established in 1976 is shown below:
• L 1 , a 1 and b 1 are the coordinates in the colorimetric space of the first color to be compared and L 2 , a 2 and b 2 those of the second.
• examples 2, 3, 4 and 5 exhibit good persistence of the cosmetic properties (mattness and color):
• compositions were carried out on a panel of individuals who use foundation. After free application of each composition to the face, each individual evaluates the perception of said composition at the time of application and in terms of makeup result.
• application is easy without a “crunching” effect on the skin. The product glides perfectly under the fingers, which makes application pleasant.
• the makeup finish is soft to the touch and nontacky.
• formulations 2 and 5 which are comparative examples
• rubbing over the skin is felt, which makes application uncomfortable and bothersome.
• the makeup finish is much less soft to the touch.
• phase A1 The constituents of phase A1 are weighed out.
• phase A2 The constituents of phase A2 are weighed out. Phases A1 and A2 are added to a mixer of Lodige type over 10 minutes.
• phase B1 The constituents of phase B1 are successively added and then homogenized in the Lodige mixer for 10 minutes.
• phase B2 is added and homogenization is carried out with the mixer for 3 minutes.
• the composition is sieved using a 250 ⁇ m sieve.
• composition is passed through a mill of Alpine type.
• Example No. 6 A Pigments 10 Talc 64.7 Nylon powder 10 Preservative 0.3 B Parleam oil 8 Resin as described in 10 WO 2005/075542* *MQ/Propyl T resin 30:70, as prepared according to example 1-c described above, in isododecane
• phase A The starting materials of phase A are weighed out and homogenization is carried out with a mixer for 10 minutes.
• phase B The starting materials of phase B are weighed out, which phase is added to phase A.
• the mixture is homogenized with the mixer for 3 minutes.
• the mixture A+B is passed through an Alpine mill.

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