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WO2025125600A1 - Process for preparing a cosmetic composition comprising a fatty phase - Google Patents

Process for preparing a cosmetic composition comprising a fatty phase Download PDF

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Publication number
WO2025125600A1
WO2025125600A1 PCT/EP2024/086284 EP2024086284W WO2025125600A1 WO 2025125600 A1 WO2025125600 A1 WO 2025125600A1 EP 2024086284 W EP2024086284 W EP 2024086284W WO 2025125600 A1 WO2025125600 A1 WO 2025125600A1
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WO
WIPO (PCT)
Prior art keywords
wax
oily phase
composition
waxes
melting point
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/EP2024/086284
Other languages
French (fr)
Inventor
Anne LIHARD
Anne ROHART
Karim BELLI
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LOreal SA
Original Assignee
LOreal SA
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Filing date
Publication date
Application filed by LOreal SA filed Critical LOreal SA
Publication of WO2025125600A1 publication Critical patent/WO2025125600A1/en
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • A61Q1/04Preparations containing skin colorants, e.g. pigments for lips
    • A61Q1/06Lipsticks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • A61K8/0229Sticks
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04Dispersions; Emulsions
    • A61K8/06Emulsions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/31Hydrocarbons
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8105Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • A61K8/8111Homopolymers or copolymers of aliphatic olefines, e.g. polyethylene, polyisobutene; Compositions of derivatives of such polymers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

Definitions

  • the present invention relates to a method for preparing a cosmetic composition comprising an oily phase, comprising specific steps.
  • Cosmetic compositions intended for care for example hygiene such as deodorant compositions
  • make-up in particular for the lips or the complexion
  • hair for example conditioners in paste form
  • viscous fluid type formulas such as glosses
  • solid compositions in stick form supported or not
  • compositions in pencil form or compositions stored in jars.
  • the routine strategy for varying hardness consists of modifying the formulation, for example by modifying the wax and/or oil type and/or concentration, which may result in an increase in the hardness of the composition, in particular lipstick, or may create composition stability problems at 4°C, at 25°C or at 40°C.
  • An object of the present invention is therefore to provide a solution to the above problems.
  • the invention relates to a novel method for producing a cosmetic composition for care and/or make-up and/or hair, preferably of lipstick type, which consists of applying specific stirring during the cooling of the mixture (or bulk product) for preparing the cosmetic composition before the filling step.
  • This specific stirring step results in a pre-crystallization of the bulk product before filling, and thus modifies the physicochemical and sensory properties of the product obtained.
  • combining stirring and cooling causes a rupture of the crystalline structure in formation, preventing the crystalline lattice from establishing correctly.
  • This phenomenon results in a substantial reduction in the hardness of the cosmetic composition obtained, which modifies its sensory properties.
  • the product obtained provides a specific smooth and soft sensory feeling.
  • the product obtained provides particular properties during withdrawal and/or application.
  • the invention thus relates to a method for preparing a cosmetic composition comprising an oily phase, comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the oily phase of step a) or into the heated oily step of step b), to obtain a cosmetic composition in emulsion form, it being understood that when step c) is present, then step b) is performed on the oily phase obtained in a) or on the composition obtained in c), d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in
  • steps a) and c) may only consist of a single step. Steps a) and c) are in this case simultaneous.
  • the following procedure may be carried out: an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats and mixtures thereof, may be contacted (steps a) and c)) prior to the heating step b) at a temperature greater than or equal to the temperature of the fat having the highest melting point.
  • the composition obtained after the heating step b) may then be stored, or be stirred directly after the heating step during the cooling step d) of the composition to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition
  • a heating step will be required again (so-called remelting step or step e)) to allow homogeneous mixing of the oily phase and the aqueous phase forming the composition.
  • the composition thus heated after remelting may then be stirred directly after the remelting step to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition.
  • the target temperature is preferably less than 90% of the value of the melting point of the fat having the highest melting point, but may be even much lower.
  • the method thus comprises the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, c) a step of adding an aqueous phase into the oily phase of step a), to obtain a cosmetic composition in emulsion form, steps a) and c) being simultaneous, b) a step of heating the oily phase obtained in c) to a temperature greater than or equal to the melting point(s) of the fat(s), d) a step of cooling the composition obtained in c), e) optionally, a step of remelting the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting
  • steps a) and c) may also be performed successively.
  • the method may comprise the following successive steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), an optional step c) of adding an aqueous phase into the heated oily phase of step b), to obtain a cosmetic composition in emulsion form.
  • composition obtained after the heating step b) or the optional step c) may then be stored, or be stirred during the cooling step d) of the composition to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition.
  • a heating step will be required again (so-called remelting step or step e)) to allow homogeneous mixing of the oily phase and the aqueous phase forming the composition.
  • the composition thus heated after remelting may then be stirred directly after the remelting step to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition.
  • the target temperature is preferably less than 90% of the value of the melting point of the fat having the highest melting point, but may be even much lower.
  • the method according to the invention comprises the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the heated oily phase of step b), to obtain a cosmetic composition in emulsion form, d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a
  • the method according to the invention relates to the preparation of a cosmetic composition comprising an oily phase.
  • a cosmetic composition is preferably solid or viscous at a temperature of 25°C.
  • Solid means that the composition does not flow under its own weight.
  • a composition according to the invention comprises at least one fat chosen from waxes, pasty fats and mixtures thereof.
  • the method according to the invention has less impact on fluid compositions at a temperature of 25°C; therefore, it is less adapted for compositions such as solutions, lotions or liquid compositions.
  • composition according to the invention may be anhydrous, a direct (O/W) emulsion or an indirect (W/O) emulsion.
  • O/W direct
  • W/O indirect
  • the cosmetic composition is a make-up or care composition, or a hair composition, for example a shampoo, a conditioner or an after-shampoo.
  • the cosmetic composition is a make-up composition, preferably a make-up composition for the lips or complexion, preferably a make-up composition for the lips, preferably a lipstick.
  • composition according to the invention includes at least one oily phase.
  • the oily phase of the composition prepared according to the invention comprises at least one fat chosen from waxes, pasty fats and mixtures thereof.
  • the fat in question is thus a fat which is solid at an ambient temperature of 25°C.
  • the oily phase according to the invention preferably comprises at least one wax or a wax mixture.
  • the oily phase according to the invention comprises at least two waxes.
  • the oily phase of the composition prepared according to the invention comprises at least two fats chosen from waxes, pasty fats and mixtures thereof.
  • a composition according to the invention comprises at least one wax and at least one pasty fat.
  • the first step of the method according to the invention is a step of introducing into a tank at least one, preferably at least two, fats chosen from waxes, pasty fats and mixtures thereof.
  • step a) is a step of introducing into a tank at least two fats chosen from waxes.
  • step a) is a step of introducing into a tank at least two waxes having different melting points (Tf).
  • the wax or waxes is/are in general a lipophilic compound, that is solid at ambient temperature (25°C), having a reversible solid/liquid change of state and a melting point greater than or equal to 30°C and up to 200°C and particularly up to 120°C.
  • the melting point is the temperature of the most endothermic peak observed in thermal analysis (DSC) as described in the standard ISO 11357-3; 1999.
  • the melting point of the wax can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the trade name "DSC Q2000" by TA Instruments.
  • the measurement protocol is as follows:
  • a sample of 5 mg of wax placed in a crucible is subjected to a first temperature rise from -20°C to 120°C, at the heating rate of 10°C I minute, then is cooled from 120°C to - 20°C at a cooling rate of 10°C I minute and finally subjected to a second temperature rise from -20°C to 120°C at a heating rate of 5°C I minute.
  • the following parameters are measured:
  • - AHf the enthalpy of fusion of the wax equivalent to the integral of the overall melting curve obtained. This enthalpy of fusion of the wax is the quantity of energy required to change the compound from the solid state to the liquid state. It is expressed in J/g.
  • the wax or waxes can be hydrocarbon, fluorinated and/or silicone and be of plant, mineral, animal, and/or synthetic origin.
  • a composition in accordance with the invention can comprise at least one wax chosen from the group comprising polar waxes, non-polar waxes and mixtures thereof.
  • the waxes are particularly as described in the document Ullmann’s Encyclopedia of Industrial Chemistry 2015, Wiley-VCH Verlag GmbH & Co. KgaA,
  • waxes can be natural, but also synthetic.
  • natural wax designates any pre-existing wax in nature or that can be transformed, extracted or purified using natural compounds that exist in nature.
  • synthetic wax designates waxes of which the synthesis requires one or several chemical reactions conducted by humans.
  • Natural waxes include natural waxes, mention can be made in particular of so-called fossil waxes of which those of petroleum origin such as ozokerite, pyropissite, macrocrystalline waxes also called paraffins - including raw or slack waxes, slack wax raffinates, de-oiled slack wax, soft waxes, semi-refined waxes, filtered waxes, refined waxes - and microcrystalline waxes called microwaxes including "bright stock” slack wax.
  • Fossil waxes further contain lignite also called montan wax, or peat wax.
  • plant waxes As examples of plant waxes, mention can be made of carnauba wax, candelilla wax, ouricuri wax, sugarcane wax, jojoba wax, T rithrinax campestris wax, raphia wax, alfalfa wax, wax extracted from the Douglas fir, sisal wax, linseed wax, cotton wax, Batavia dammar wax, cereal wax, tea wax, coffee wax, rice wax, palm wax, Japan wax, and mixtures thereof.
  • animal waxes mention can be made of beeswax, Ghedda wax, shellac, Chinese wax, lanolin also called wool wax, mixtures thereof and derivatives thereof.
  • ester waxes such as the waxes having the formula R1COOR2 wherein R1 and R2 are aliphatic linear, branched or cyclic chains of which the number of atoms varies from 10 to 50, that can contain a heteroatom in particular oxygen, and the melting point of which varies from 30 to 120°C, preferably from 30 to 100°C.
  • ester wax a C20-C40 (hydroxystearyloxy)alkyl stearate (with the alkyl group comprising from 20 to 40 carbon atoms), alone or in a mixture or a C20-C40 alkyl stearate.
  • Such waxes are particular sold under the trade names "Kester Wax K 82 P", “Hydroxypolyester K 82 P”, “Kester Wax K 80 P”, or “KESTER WAX K82H” by KOSTER KELINEN.
  • Mixtures of esters of C14-C18 carboxylic acid and of alcohols such as the products "Cetyl Ester Wax” from KOSTER KEUNEN, "SP Crodamol MS MBAL”, “Crodamol MS” from CRODA, "Miraceti” from LASERSON can also be used.
  • a montanate (octacosanoate) of glycol and of butylene glycol such as LICOWAX KPS FLAKES wax (INCI name: glycol montanate) sold by Clariant can also be used. Mention can also be made of hydrocarbon, polyoxyalkylene or polyglycerol waxes, natural or synthetic, of animal or plant origin; the number of oxyalkylene (C2-C4) units can vary from 2 to 100, the number of glycerol units can vary from 1 to 20.
  • polyoxyethylene beeswaxes such as PEG-6 beeswax, PEG-8 beeswax
  • polyoxyethylene carnauba waxes such as PEG- 12 carnauba
  • optionally hydrogenated polyoxyethylene or polyoxypropylene lanolin waxes such as PEG-30 lanolin, PEG-75 lanolin
  • PPG-5 lanolin wax glyceride polyglycerol beeswaxes, in particular polyglyceryl-3 Beewax
  • fatty alcohols that are solid at ambient temperature comprising from 14 to 22 carbon atoms, and more preferably from 16 to 18 carbon atoms.
  • ceotstearyl alcohol (or cetearyl alcohol) which is a mixture of stearyl and cetyl alcohols can be used.
  • the composition comprises at least one non-polar hydrocarbon wax.
  • non-polar hydrocarbon wax refers to a wax that comprises only carbon or hydrogen atoms in its structure.
  • such a wax is free of other atoms, in particular heteroatoms such as for example nitrogen, oxygen, silicon.
  • non-polar waxes suitable for the invention mention can in particular be made of hydrocarbon waxes such as microcrystalline waxes, paraffin waxes, ozokerite, polymethylene waxes, polyethylene waxes, waxes obtained by Fischer- Tropsch synthesis, microwaxes in particular of polyethylene.
  • hydrocarbon waxes such as microcrystalline waxes, paraffin waxes, ozokerite, polymethylene waxes, polyethylene waxes, waxes obtained by Fischer- Tropsch synthesis, microwaxes in particular of polyethylene.
  • the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 45°C.
  • the wax having a melting point greater than or equal to 45°C comprises at least one fatty alcohol.
  • the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 70°C.
  • the wax having a melting point greater than or equal to 70°C is chosen from paraffin waxes, ozokerite, polymethylene waxes and polyethylene waxes.
  • the oily phase of step a) comprises at least 0.1% by weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight with respect to the total weight of the mixture of at least one wax, preferably the melting point of which is greater than or equal to 45°C, preferably greater than or equal to 70°C.
  • the wax having a melting point greater than or equal to 70°C is a non-polar hydrocarbon wax, preferably a polyethylene wax, and said non-polar hydrocarbon wax represents at least 50% by weight with respect to the total weight of wax(es) of the mixture.
  • the liquid fraction by weight of the pasty compound at 23°C is more particularly equal to the ratio of the enthalpy of fusion consumed at 23°C to the enthalpy of fusion of the pasty compound.
  • the enthalpy of fusion of the pasty compound is the enthalpy consumed by the compound to change from the solid state to the liquid state.
  • the pasty compound is said to be in the solid state when the entire mass thereof is in solid crystalline form.
  • the pasty compound is said to be in the liquid state when the entire mass thereof is in liquid form.
  • the enthalpy of fusion of the pasty compound is in particular equal to the area under the curve of the thermogram obtained using a differential scanning calorimeter.
  • the enthalpy of fusion of the pasty compound is the quantity of energy required to change the compound from the solid state to the liquid state. It is expressed in J/g.
  • the enthalpy of fusion consumed at 23°C is the quantity of energy required by the sample to change from the solid state to the state present at 23°C consisting of a liquid fraction and a solid fraction.
  • the pasty compound(s) can be in particular chosen from synthetic pasty compounds and fats of plant origin.
  • the pasty compound(s) can be hydrocarbon or silicone.
  • the pasty compound(s) can be in particular chosen from:
  • lanolin and its derivatives such as lanolin alcohol, oxyethylenated lanolins, acetylated lanolin, lanolin esters such as isopropyl lanolate, oxypropylenated lanolins;
  • polyol ethers chosen from C2-C4 pentaerythritol and polyalkylene glycol ethers, fatty alcohol and sugar ethers, and mixtures thereof.
  • pentaerythritol and polyethylene glycol ether comprising 5 oxyethylene (5 OE) units C2-C4 pentaerythritol and polyalkylene glycol ethers, fatty alcohol and sugar ethers, and mixtures thereof.
  • OE oxyethylene
  • PPG-5 Pentaerythrityl Ether pentaerythritol and polypropylene glycol ether comprising 5 oxypropylene units (5 OP)
  • CTFA name: PPG-5 Pentaerythrityl Ether pentaerythrityl Ether
  • PPG-5 Pentaerythrityl Ether PPG-5 Pentaerythrityl Ether
  • soybean oil sold under the trade name "Lanolide” by VEVY, wherein the ratio of the constituents by weight is
  • - vinyl polymers in particular: oolefin homopolymers and copolymers; o hydrogenated diene homopolymers and copolymers; o branched oligomers, alkyl (meth)acrylate homo or copolymers preferably having a C8-C30 alkyl group, ovinyl ester homo and copolymer oligomers, having C8-C30 alkyl groups, and ovinylether homo and copolymer oligomers, having C8-C30 alkyl groups,
  • liposoluble polyethers derived from polyetherification between one or a several C2- C100, preferably C2-C50, diols.
  • liposoluble polyethers particular consideration is given to ethylene-oxide and/or propylene-oxide copolymers with C6-C30 long-chain alkylene-oxides, more preferably such that the weight ratio of ethylene-oxide and/or propylene-oxide with alkylene-oxides in the copolymer is 5:95 to 70:30.
  • copolymers such as long-chain alkylene-oxides arranged in blocks having a mean molecular weight of 1000 to 10,000, for example a polyoxyethylene/polydodecyl glycol block copolymer such as the dodecanediol (22 mol) and polyethylene glycol (45 OE) ethers sold under the brand ELFACOS ST9 by AKZO NOBEL.
  • esters particular consideration is given to: ooligomer glycerol esters, especially the esters of diglycerol, with monocarboxylic acids, optionally hydroxylated, linear or branched, saturated or not, preferably saturated, C6-C20, and/or dicarboxylic acids, linear or branched, saturated or not, preferably saturated, C6-C10, in particular condensates of adipic acid and diglycerol, for which a portion of the hydroxyl groups of the glycerols have reacted with a mixture of fatty acids, such as stearic acid, capric acid, stearic acid, isostearic acid and 12-hydroxystearic acid, such as for example bis-diglyceryl polyacyladipate-2 sold under the reference SOFTISAN® 649 by Sasol, o homopolymers of vinyl ester having C8-C30 alkyl groups, such as polyvinyl laurate (in particular sold under
  • the aliphatic carboxylic acid is C4-C30, preferably C8-C30. It is preferably chosen from hexanoic, heptanoic, octanoic, 2- ethylhexanoic, nonanoic, decanoic, undecanoic, dodecanoic, tridecanoic, tetradecanoic, pentadecanoic, hexadecanoic, hexyldecanoic, heptadecanoic, octadecanoic, isostearic, nonadecanoic, eicosanoic, isoarachidic, octyldodecanoic, heneicosanoic and docosanoic acids, and mixtures thereof.
  • the aliphatic carboxylic acid is preferably branched.
  • the hydroxycarboxylic acid ester is advantageously derived from a C2-C40 hydroxylated carboxylic acid, preferably C10 - C34, and more preferably C12 - C28; with the number of hydroxyl groups being between 1 and 20, more particularly between 1 and 10, preferably between 1 and 6.
  • Said hydroxycarboxylic acid esters are preferably chosen from: a) total or partial saturated, linear and monohydroxylated aliphatic monocarboxylic acid esters; b) total or partial saturated, monohydroxylated aliphatic monocarboxylic acid esters; c) total or partial saturated, monohydroxylated aliphatic polycarboxylic acid esters; d) total or partial saturated, polyhydroxylated aliphatic polycarboxylic acid esters; e) partial or total C2 -C16 aliphatic polyol esters with a mono or polyhydroxylated aliphatic mono or polycarboxylic acid f) mixtures thereof.
  • esters where applicable, esterified on their free alcohol or acid function(s) by acid or alcohol radicals, in particular dimer dilinoleate esters; such esters can particularly be chosen from esters having the following INCI classification: bis- behenyl/isostearyl/phytosteryl dimer dilinoleyl dimer dilinoleate (Plandool G), phytosteryl I isosteryl I cetyl I stearyl I behenyl dimer dilinoleate (Plandool H or Plandool S) and mixtures thereof, ohydrogenated rosin esters (Lusplan DD-DHR or DD-DHR from Nippon Fine Chemical)
  • - butters of plant origin such as mango butter, such as that sold under the reference Lipex 203 by AARHUSKARLSHAMN, shea butter, in particular that having the INCI name Butyrospermum Parkii Butter, such as that sold under the reference Sheasoft® by AARHUSKARLSHAMN, cupuacu butter (Rain forest RF3410 from Beraca Sahara), murumuru butter (RAIN FOREST RF3710 from Beraca Sahara), cocoa butter, babassu butter such as that sold under the name Cropure Babassu SS-(LK) by Croda, as well as orange wax such as, for example, that sold under the reference Orange Peel Wax by Koster Keunen,
  • hydrogenated castor oil esters such as dimer dilinoleate hydrogenated castor oil for example RISOCAST-DA-L sold by KOKYU ALCOHOL KOGYO, hydrogenated castor oil isostearate for example SALACOS HCIS (V-L) sold by NISSHIN OIL, - and mixtures thereof.
  • the pasty compound(s) are chosen from:
  • the letter "M” represents the Monofunctional unit having the formula R1 R2R3SiOi/2, the silicon atom being bound to a single oxygen atom in the polymer comprising this unit.
  • trimethylsiloxysilicate type MQ type solid silicone resins examples include those sold under the reference SR1000 by General Electric, under the reference TMS 803 by Wacker, under the trade name "KF-7312J” by Shin-Etsu, "DC 749", “DC 593” by Dow Corning.
  • silicone resins comprising MQ siloxysilicate units
  • phenylpropyldimethylsiloxysilicate sold by General Electric
  • the preparation of such resins is described in particular in patent US5817302.
  • polymethylsilsesquioxanes which are polysilsesquioxanes wherein none of the methyl radicals is substituted by another group.
  • polymethylsilsesquioxanes are described for example in document US 5,246,694.
  • polymethylsilsesquioxane resins can be used wherein R is a methyl group, such as for example those sold:
  • Resin MK such as Belsil PMS MK: polymer comprising CH3SiO3/2 repeat units (T units), that may also comprise up to 1% by weight of (CH 3 )2SiO 2 /2 units (D units) and having a mean molecular weight of approximately 10000 g/mol, or
  • MQT type resins are MQT-propyl resins (also called MQTPr).
  • MQTPr MQT-propyl resins
  • the MQ-T-propyl resin preferably comprises the units:
  • R1 , R2 and R3 independently are a hydrocarbon radical (in particular alkyl) having from 1 to 10 carbon atoms, a phenyl group, a phenylalkyl group or a hydroxyl group and preferably an alkyl radical having from 1 to 8 carbon atoms or a phenyl group,
  • R1 and R3 independently are an alkyl group having from 1 to 8 carbon atoms, R1 being preferably a methyl group and R3 preferably being a propyl group,
  • siloxane resins that can be used according to the invention can be obtained by a method comprising the reaction of: a) an MQ resin comprising at least 80% in moles of (Rl3SiOi/2)a and (SiC>4/2)d units
  • R3 being an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group,
  • the A/B mass ratio is between 95:5 and 15:85, preferably the A/B mass ratio is 30:70.
  • the A/B mass ratio is between 95:5 and 15:85.
  • the A/B ratio is less than or equal to 70:30. These preferred ratios have proven to allow comfortable deposits.
  • the composition according to the invention comprises, as a silicone resin, at least one MQ type resin as described hereinabove.
  • the silicone resin is a siloxysilicate resin, preferably a trimethylsiloxysilicate resin.
  • the silicone resin is present in a concentration of at least 5% by weight, preferably in a concentration ranging from 5 to 15% by weight with respect to the total weight of the composition, or preferably from 6 to 9% by weight, with respect to the total weight of the composition.
  • Hydrocarbon oil means an oil essentially formed, or consisting, of carbon and hydrogen atoms, and optionally oxygen, nitrogen atoms, and containing no silicon or fluorine atoms.
  • the hydrocarbon oil is therefore distinct from a silicone oil and from a fluorine oil.
  • the oil is present in a concentration of at least 5% by weight, preferably in a concentration ranging from 5 to 30% by weight with respect to the total weight of the composition, or preferably from 10 to 25% by weight, with respect to the total weight of the composition.
  • an oily phase comprising at least one, preferably at least two, fats chosen from waxes, pasty fats and mixtures thereof, is obtained in a tank.
  • step b) the oily phase obtained in a) is heated to a temperature greater than the melting point(s) of the fat(s) (chosen from waxes, pasty fats and mixtures thereof).
  • This step b) makes it possible to melt said fat(s) completely.
  • steps a) and c) are simultaneous, an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats and mixtures thereof, are mixed (steps a and c)) prior to the heating step b).
  • This step b) makes it possible to melt said fat(s) completely in the mixture.
  • this step b) is performed under stirring.
  • step b a homogeneous liquid oily phase is obtained.
  • step b) a homogeneous mixture of liquid oily phase and aqueous phase is in particular obtained.
  • Step c) is optional: indeed, it is possible to add an aqueous phase into the heated mixture of step b), to obtain a cosmetic composition in dispersion or emulsion form.
  • the aqueous phase added may be a dispersed aqueous phase.
  • Such an emulsion is then an invert (water-in-oil or W/O) emulsion.
  • the aqueous phase added can be a continuous aqueous phase; such an emulsion is then a direct (oil-in-water or O/W) emulsion.
  • the composition obtained is anhydrous (consists of the oily phase).
  • the aqueous phase can consist essentially of water; it can also comprise a mixture of water and water-miscible solvent (miscibility in water greater than 50% by weight at 25°C) such as lower monoalcohols having from 1 to 5 carbon atoms such as ethanol, isopropanol, glycols having from 2 to 8 carbon atoms such as propylene glycol, ethylene glycol, 1 ,3- butylene glycol, dipropylene glycol, and mixtures thereof.
  • water-miscible solvent miscibility in water greater than 50% by weight at 25°C
  • lower monoalcohols having from 1 to 5 carbon atoms
  • glycols having from 2 to 8 carbon atoms such as propylene glycol, ethylene glycol, 1 ,3- butylene glycol, dipropylene glycol, and mixtures thereof.
  • the composition preferably comprises a water concentration that represents at least 7% by weight, preferably a concentration ranging from 7% to 40% by weight, with respect to the total weight of the composition.
  • the water of the aqueous phase is present in a quantity between 7% and 30% by weight, preferably between 10% and 30% by weight, preferably between 15 and 30% by weight with respect to the total weight of the composition.
  • the surfactant(s) are chosen from silicone non-ionic surfactants, from hydrocarbon non-ionic surfactants, or from mixtures thereof.
  • silicone surfactants mention can be made of alkyl or alkoxy dimethicone copolyols with pendant alkyl or alkoxy chain or silicone backbone-end having for example from 6 to 22 carbon atoms; dimethicone copolyols, which are more particularly oxypropylene and/or oxyethylene polydimethyl methyl siloxanes, as well as crosslinked solid elastomeric organopolysiloxanes that comprise at least one oxyalkylene group, and mixtures thereof.
  • dimethicone copolyols such as for example those sold under the trade names KF- 6015 (PEG-3 dimethicone), KF-6016 (PEG-9 methyl ether dimethicone), KF-6017 (PEG-10 dimethicone), KF-6028 (PEG-9 polydimethylsiloxyethyl dimethicone), KF-6050 L (PEG/PPG 18/18 dimethicone in cyclopentasiloxane), by Shin-Etsu; dimethicone copolyols sold under the trade names Dow Corning 3225C (PEG/PPG-18/18 Dimethicone in a mixture of cyclotetrasiloxane and cyclopentasiloxane), DC 5225 C Formulation Aid (PEG/PPG- 18/18 Dimethicone in cyclopentasiloxane); or the product sold under the trade name SF 1528 GE
  • Alkyl-dimethicone copolyols can also be used such as Lauryl PEG/PPG- 18/18 Methicone (which is more particularly an alkoxyl derivative of Lauryl Methicone containing on average 18 moles of ethylene oxide and 18 moles of propylene oxide, sold under the trade name "Dow Corning 5200 Formulation Aid” by Dow Corning; cetyl PEG/PPG-10/1 Dimethicone (which is more particularly a copolymer of Cetyl Dimethicone and an alkoxyl derivative of dimethicone containing on average 10 moles of ethylene oxide and 1 mole of propylene oxide) such as the product sold under the trade name Abil EM 90 by Evonik Goldschmidt as well as the mixture of cetyl PEG/PPG-10/1 Dimethicone, polyglycerol isostearate (4 moles) and hexyl laurate sold under the trade name ABIL WE 09 by Evonik Goldschmidt.
  • the composition comprises as silicone surfactant(s), C8-C22 alkyl dimethicone copolyol such as cetyl dimethicone copolyol, in particular having the INCI name CETYL PEG/PPG-10/1 DIMETHICONE, dimethicone copolyols such as for example PEG- 10 dimethicone, PEG/PPG 18/18 dimethicone, as well as mixtures thereof.
  • C8-C22 alkyl dimethicone copolyol such as cetyl dimethicone copolyol, in particular having the INCI name CETYL PEG/PPG-10/1 DIMETHICONE
  • dimethicone copolyols such as for example PEG- 10 dimethicone, PEG/PPG 18/18 dimethicone, as well as mixtures thereof.
  • the dyes can be present, in the composition, at a concentration ranging from 0.01% to 25% by weight, with respect to the weight of the composition, preferably from 0.01% to 20% by weight.
  • water-soluble dye(s) that can be implemented within the scope of the present invention, mention can in particular be made of those of natural origin, such as extracts of carmine, cochineal, beet, grape, carrot, tomato, rocou, paprika, henna, caramel and curcumin.
  • nacres can also be mentioned.
  • the term "nacres" should be understood to mean iridescent or non-iridescent colored particles of any shape, which are in particular produced by certain mollusks in their shell or else are synthesized and which exhibit a color effect by optical interference.
  • the nacres can be selected from pearlescent pigments such as titanium mica coated with iron oxide, titanium mica coated with bismuth oxychloride, titanium mica coated with chromium oxide, titanium mica coated with an organic dye, and pearlescent pigments based on bismuth oxychloride. They can also consist of mica particles at the surface whereof are superposed at least two successive layers of metal oxides and/or of organic dyes.
  • stabilized means absence of an effect of variability of color with the angle of observation or in response to a temperature change.
  • this material may be selected from particles having a metallic glint, goniochromatic coloring agents, diffracting pigments, thermochromatic agents, optical brighteners, and also fibers, in particular of the interference type.
  • these various materials can be combined so as to provide the simultaneous manifestation of two effects, or even a new effect in accordance with the invention.
  • the composition according to the invention comprises at least one non-coated pigment.
  • the composition according to the invention comprises at least one pigment coated with at least one lipophilic or hydrophobic compound.
  • This type of pigment is particularly advantageous. Since they are treated by a hydrophobic compound, they manifest a preponderant affinity for an oily phase, which can then convey them.
  • the coating can also comprise at least one additional non-lipophilic compound.
  • the "coating" of a pigment according to the invention generally denotes the full or partial surface treatment of the pigment by a surface agent, absorbed, adsorbed or grafted onto said pigment.
  • the surface-treated pigments can be prepared using chemical, electronic, mechanochemical or mechanical surface treatment techniques well known to a person skilled in the art. Commercial products can also be used.
  • the surface agent can be absorbed, adsorbed or grafted onto the pigments by means of solvent evaporation, chemical reaction or creation of a covalent bond.
  • the surface treatment consists of a coating of the pigments.
  • the coating can represent 0.1% to 20% by weight and particularly 0.5% to 5% by weight of the total weight of the coated pigment.
  • the coating can be carried out for example by adsorbing a liquid surface agent on the surface of the solid particles merely by mixing while stirring the particles and said surface agent, optionally heated, before incorporating the particles in the other ingredients of the makeup or care composition.
  • the coating can be carried out for example by means of a chemical reaction of a surface agent with the surface of the solid pigment particles and the creation of a covalent bond between the surface agent and the particles. This method is particularly described in the patent US 4,578,266.
  • the chemical surface treatment can consist of diluting the surface agent in a volatile solvent, dispersing the pigments in this mixture, and then slowly evaporating the volatile solvent, such that the surface agent is deposited on the surface of the pigments.
  • the pigments can be coated according to the invention with at least one compound selected from silicone surfactants; fluorinated surfactants; fluorosilicone surfactants; metal soaps, n-acyl amino acids or salts thereof; lecithin and its derivatives; isopropyl triisostearyl titanate; isostearyl sebacate; plant or animal natural waxes; polar synthetic waxes; fatty esters; phospholipids; and mixtures thereof.
  • silicone surfactants selected from silicone surfactants; fluorinated surfactants; fluorosilicone surfactants; metal soaps, n-acyl amino acids or salts thereof; lecithin and its derivatives; isopropyl triisostearyl titanate; isostearyl sebacate; plant or animal natural waxes; polar synthetic waxes; fatty esters; phospholipids; and mixtures thereof.
  • the dye is an organic, synthetic, natural pigment or pigment of natural origin.
  • Organic pigment means any pigment that complies with the definition in Ullmann’s Encyclopedia in the Organic Pigment chapter.
  • the organic pigments can in particular be selected from the compounds nitroso, nitro, azo, xanthene, quinoline, anthraquinone, phthalocyanine, metal complex type, isoindolinone, isoindoline, quinacridone, perinone, perylene, diketopyrrolopyrrole, thioindigo, dioxazine, triphenylmethane, quinophthalone.
  • the organic pigment(s) can be selected for example from carmine, carbon black, aniline black, melanin, azo yellow, quinacridone, phthalocyanine blue, sorghum red, the blue pigments codified in the Color Index under the references Cl 42090, 69800, 69825, 73000, 74100, 74160, the yellow pigments codified in the Color Index under the references Cl 11680, 11710, 15985, 19140, 20040, 21100, 21108, 47000, 47005, the green pigments codified in the Color Index under the references Cl 61565, 61570, 74260, the orange pigments codified the Color Index under the references Cl 11725, 15510, 45370, 71105, the red pigments codified in the Color Index under the references Cl 12085, 12120, 12370, 12420, 12490, 14700, 15525, 15580, 15620, 15630, 15800, 15850, 15865, 15880, 17200, 26100, 45380,
  • the pigments can also be in the form of composite pigments as described in patent EP 1 184 426.
  • These composite pigments can be composed in particular of particles including an inorganic core covered at least partially with an organic pigment and at least one binder for fixing the organic pigments to the core.
  • the pigment can also be a lacquer.
  • lacquer means insoluble dyes adsorbed on insoluble particles, the assembly thus obtained remaining insoluble during use.
  • the inorganic substrates onto which the dyes are adsorbed are for example alumina, silica, borosilicate, calcium and sodium or calcium aluminum borosilicate, and aluminum.
  • the cosmetic mixture obtained in step b) or c) comprises at least one active agent.
  • Active agent means any active agent that can be used for a topical application on the skin and/or hair.
  • Step d) is a step of cooling the heated oily phase obtained in b) or the composition obtained in c).
  • the content of these buckets is transferred to a tank equipped with a stirrer according to the invention (the tank does not contain an impeller or a scraper).
  • the composition is heated to a temperature greater than or equal to the highest melting point of the waxes (in this case 85°C due to the presence of polyethylene wax) (remelting step e) of the method), then, to pre-crystallize the waxes, the temperature is lowered again to a target temperature of 70-75°C, thus creating a higher viscosity of the mixture which is stirred by the stirrer according to the invention (stirring applied according to the invention at the end of the remelting step e)).

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Abstract

The present invention relates to a method for preparing a cosmetic composition comprising an oily phase, comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the oily phase of step a) or into the heated oily step of step b), to obtain a cosmetic composition in emulsion form, it being understood that when step c) is present, then step b) is performed on the oily phase obtained in a) or on the composition obtained in c), d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the stirred oily phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one receptacle.

Description

Process for preparing a cosmetic composition comprising a fatty phase
The present invention relates to a method for preparing a cosmetic composition comprising an oily phase, comprising specific steps.
Cosmetic compositions intended for care (for example hygiene such as deodorant compositions) and/or make-up, in particular for the lips or the complexion, and/or for hair (for example conditioners in paste form), have been known for very long time and come in more and more varied forms, ranging from viscous fluid type formulas such as glosses, to solid compositions in stick form, supported or not, compositions in pencil form, or compositions stored in jars.
However, there are very few commercial cosmetic compositions for care and/or makeup and/or hair, in particular lipsticks, which are supple or smooth; this is on account of the difficulty adapting the texture or hardness in a controlled manner.
The routine strategy for varying hardness consists of modifying the formulation, for example by modifying the wax and/or oil type and/or concentration, which may result in an increase in the hardness of the composition, in particular lipstick, or may create composition stability problems at 4°C, at 25°C or at 40°C.
There is therefore a need for cosmetic compositions for care and/or make-up and/or hair which can be used on the skin, for example the cheeks, the face and/or the lips, and/or the hair, with novel textures and/or novel sensory properties, for example which are supple and easy to apply.
An object of the present invention is therefore to provide a solution to the above problems.
The invention relates to a novel method for producing a cosmetic composition for care and/or make-up and/or hair, preferably of lipstick type, which consists of applying specific stirring during the cooling of the mixture (or bulk product) for preparing the cosmetic composition before the filling step. This specific stirring step results in a pre-crystallization of the bulk product before filling, and thus modifies the physicochemical and sensory properties of the product obtained. Indeed, combining stirring and cooling causes a rupture of the crystalline structure in formation, preventing the crystalline lattice from establishing correctly. This phenomenon results in a substantial reduction in the hardness of the cosmetic composition obtained, which modifies its sensory properties. In particular, in the case of a lipstick type cosmetic composition, the product obtained provides a specific smooth and soft sensory feeling. In the case of a hair composition, the product obtained provides particular properties during withdrawal and/or application.
The invention thus relates to a method for preparing a cosmetic composition comprising an oily phase, comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the oily phase of step a) or into the heated oily step of step b), to obtain a cosmetic composition in emulsion form, it being understood that when step c) is present, then step b) is performed on the oily phase obtained in a) or on the composition obtained in c), d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the oily phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one receptacle.
It should be noted that steps a) and c) may only consist of a single step. Steps a) and c) are in this case simultaneous. In other words, in the case where it is sought to obtain a cosmetic composition comprising an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats, and mixtures thereof, the following procedure may be carried out: an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats and mixtures thereof, may be contacted (steps a) and c)) prior to the heating step b) at a temperature greater than or equal to the temperature of the fat having the highest melting point. The composition obtained after the heating step b) may then be stored, or be stirred directly after the heating step during the cooling step d) of the composition to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition.
If this composition is stored after the heating step b), then a heating step will be required again (so-called remelting step or step e)) to allow homogeneous mixing of the oily phase and the aqueous phase forming the composition. Similarly, the composition thus heated after remelting (step e)) may then be stirred directly after the remelting step to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition. The target temperature is preferably less than 90% of the value of the melting point of the fat having the highest melting point, but may be even much lower.
According to this embodiment, the method thus comprises the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, c) a step of adding an aqueous phase into the oily phase of step a), to obtain a cosmetic composition in emulsion form, steps a) and c) being simultaneous, b) a step of heating the oily phase obtained in c) to a temperature greater than or equal to the melting point(s) of the fat(s), d) a step of cooling the composition obtained in c), e) optionally, a step of remelting the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the stirred composition obtained at the end of step d) or e) into at least one receptacle.
According to the invention, it should be noted that steps a) and c) may also be performed successively. In other words, in the case where it is sought to obtain a cosmetic composition comprising an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats, and mixtures thereof, the method may comprise the following successive steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), an optional step c) of adding an aqueous phase into the heated oily phase of step b), to obtain a cosmetic composition in emulsion form.
The composition obtained after the heating step b) or the optional step c) may then be stored, or be stirred during the cooling step d) of the composition to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition.
If this composition is stored after the heating step b) or the optional step c), then a heating step will be required again (so-called remelting step or step e)) to allow homogeneous mixing of the oily phase and the aqueous phase forming the composition. Similarly, the composition thus heated after remelting (step e)) may then be stirred directly after the remelting step to a target temperature less than the value of the melting point of the fat having the highest melting point present in said composition. The target temperature is preferably less than 90% of the value of the melting point of the fat having the highest melting point, but may be even much lower.
Preferably, in the case where the cosmetic composition comprises an oily phase (in particular continuous), the method according to the invention comprises the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the heated oily phase of step b), to obtain a cosmetic composition in emulsion form, d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the oily phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one receptacle. The invention also relates to a cosmetic composition obtained directly with a preparation method according to the invention.
The method according to the invention relates to the preparation of a cosmetic composition comprising an oily phase. Such a cosmetic composition is preferably solid or viscous at a temperature of 25°C.
"Solid" means that the composition does not flow under its own weight.
"Viscous" means that the composition flows slightly under its own weight.
In other words, the method according to the invention is adapted to cosmetic compositions provided at a temperature 25°C in stick, bullet, hot-cast form, in paste or thick composition form, in order to impart novel cosmetic properties and/or novel sensory properties to these compositions. Typically, a composition according to the invention comprises at least one fat chosen from waxes, pasty fats and mixtures thereof.
The method according to the invention has less impact on fluid compositions at a temperature of 25°C; therefore, it is less adapted for compositions such as solutions, lotions or liquid compositions.
The composition according to the invention may be anhydrous, a direct (O/W) emulsion or an indirect (W/O) emulsion. When the composition according to the invention is anhydrous or in indirect emulsion form, it has a continuous oily phase.
Preferably, the cosmetic composition is a make-up or care composition, or a hair composition, for example a shampoo, a conditioner or an after-shampoo. Preferably, the cosmetic composition is a make-up composition, preferably a make-up composition for the lips or complexion, preferably a make-up composition for the lips, preferably a lipstick.
Step a)
The composition according to the invention includes at least one oily phase.
The oily phase of the composition prepared according to the invention comprises at least one fat chosen from waxes, pasty fats and mixtures thereof.
The fat in question is thus a fat which is solid at an ambient temperature of 25°C.
The oily phase according to the invention preferably comprises at least one wax or a wax mixture. Preferably, the oily phase according to the invention comprises at least two waxes.
Preferably, the oily phase of the composition prepared according to the invention comprises at least two fats chosen from waxes, pasty fats and mixtures thereof.
According to one particular embodiment, a composition according to the invention comprises at least one wax and at least one pasty fat. The first step of the method according to the invention, i.e. step a), is a step of introducing into a tank at least one, preferably at least two, fats chosen from waxes, pasty fats and mixtures thereof.
Preferably, step a) is a step of introducing into a tank at least two fats chosen from waxes. Preferably, step a) is a step of introducing into a tank at least two waxes having different melting points (Tf).
Wax(es)
The wax or waxes is/are in general a lipophilic compound, that is solid at ambient temperature (25°C), having a reversible solid/liquid change of state and a melting point greater than or equal to 30°C and up to 200°C and particularly up to 120°C.
For the purposes of the invention, the melting point is the temperature of the most endothermic peak observed in thermal analysis (DSC) as described in the standard ISO 11357-3; 1999. The melting point of the wax can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the trade name "DSC Q2000" by TA Instruments.
The measurement protocol is as follows:
A sample of 5 mg of wax placed in a crucible is subjected to a first temperature rise from -20°C to 120°C, at the heating rate of 10°C I minute, then is cooled from 120°C to - 20°C at a cooling rate of 10°C I minute and finally subjected to a second temperature rise from -20°C to 120°C at a heating rate of 5°C I minute. During the second temperature rise, the following parameters are measured:
- the melting point (Tf) of the wax, as mentioned above equivalent to the temperature of the most endothermic peak of the melting curve observed, representing the variation in the difference in power absorbed as a function of the temperature,
- AHf: the enthalpy of fusion of the wax equivalent to the integral of the overall melting curve obtained. This enthalpy of fusion of the wax is the quantity of energy required to change the compound from the solid state to the liquid state. It is expressed in J/g.
The wax or waxes can be hydrocarbon, fluorinated and/or silicone and be of plant, mineral, animal, and/or synthetic origin.
A composition in accordance with the invention can comprise at least one wax chosen from the group comprising polar waxes, non-polar waxes and mixtures thereof. The waxes are particularly as described in the document Ullmann’s Encyclopedia of Industrial Chemistry 2015, Wiley-VCH Verlag GmbH & Co. KgaA,
In particular, such waxes can be natural, but also synthetic.
The term "natural" wax designates any pre-existing wax in nature or that can be transformed, extracted or purified using natural compounds that exist in nature.
The term "synthetic" wax designates waxes of which the synthesis requires one or several chemical reactions conducted by humans.
Among natural waxes, mention can be made in particular of so-called fossil waxes of which those of petroleum origin such as ozokerite, pyropissite, macrocrystalline waxes also called paraffins - including raw or slack waxes, slack wax raffinates, de-oiled slack wax, soft waxes, semi-refined waxes, filtered waxes, refined waxes - and microcrystalline waxes called microwaxes including "bright stock" slack wax. Fossil waxes further contain lignite also called montan wax, or peat wax.
As natural waxes other than fossil waxes mention can be made of animal and plant waxes.
As examples of plant waxes, mention can be made of carnauba wax, candelilla wax, ouricuri wax, sugarcane wax, jojoba wax, T rithrinax campestris wax, raphia wax, alfalfa wax, wax extracted from the Douglas fir, sisal wax, linseed wax, cotton wax, Batavia dammar wax, cereal wax, tea wax, coffee wax, rice wax, palm wax, Japan wax, and mixtures thereof.
As examples of animal waxes, mention can be made of beeswax, Ghedda wax, shellac, Chinese wax, lanolin also called wool wax, mixtures thereof and derivatives thereof.
Mention can also be made of ester waxes such as the waxes having the formula R1COOR2 wherein R1 and R2 are aliphatic linear, branched or cyclic chains of which the number of atoms varies from 10 to 50, that can contain a heteroatom in particular oxygen, and the melting point of which varies from 30 to 120°C, preferably from 30 to 100°C. In particular, it is possible to use as ester wax a C20-C40 (hydroxystearyloxy)alkyl stearate (with the alkyl group comprising from 20 to 40 carbon atoms), alone or in a mixture or a C20-C40 alkyl stearate. Such waxes are particular sold under the trade names "Kester Wax K 82 P", "Hydroxypolyester K 82 P", "Kester Wax K 80 P", or "KESTER WAX K82H" by KOSTER KELINEN. Mixtures of esters of C14-C18 carboxylic acid and of alcohols such as the products "Cetyl Ester Wax" from KOSTER KEUNEN, "SP Crodamol MS MBAL", "Crodamol MS" from CRODA, "Miraceti" from LASERSON can also be used. A montanate (octacosanoate) of glycol and of butylene glycol such as LICOWAX KPS FLAKES wax (INCI name: glycol montanate) sold by Clariant can also be used. Mention can also be made of hydrocarbon, polyoxyalkylene or polyglycerol waxes, natural or synthetic, of animal or plant origin; the number of oxyalkylene (C2-C4) units can vary from 2 to 100, the number of glycerol units can vary from 1 to 20. By way of examples, mention can be made of polyoxyethylene beeswaxes, such as PEG-6 beeswax, PEG-8 beeswax; polyoxyethylene carnauba waxes, such as PEG- 12 carnauba; optionally hydrogenated polyoxyethylene or polyoxypropylene lanolin waxes, such as PEG-30 lanolin, PEG-75 lanolin; PPG-5 lanolin wax glyceride; polyglycerol beeswaxes, in particular polyglyceryl-3 Beewax; wax-derived esters obtained from reacting plant waxes and a polyglycerol, preferably derived esters obtained from reacting a mixture of jojoba, mimosa (Acacia Decurrens) and sunflower waxes and polyglycerol-3, for example the Acacia Decurrens (Mimosa)/Jojoba/Sunflower Seed Wax Polyglyceryl-3 Esters mixture sold under the trade name Hydracire S by Gattefosse, or the Acacia Decurrens Flower Wax, Jojoba esters, Sunflower Seed Wax and Polyglycerin-3 mixture particularly sold under the trade name Acticire MB by Gattefosse, and mixtures thereof.
As waxes, mention can also be made of fatty alcohols that are solid at ambient temperature comprising from 14 to 22 carbon atoms, and more preferably from 16 to 18 carbon atoms. As particular examples of fatty alcohols that can be used, particular mention can be made of stearyl alcohol, cetyl alcohol, myristyl alcohol and mixtures thereof. Preferably, ceotstearyl alcohol (or cetearyl alcohol), which is a mixture of stearyl and cetyl alcohols can be used.
Preferably, the composition comprises at least one non-polar hydrocarbon wax.
For the purposes of the invention, "non-polar hydrocarbon wax" refers to a wax that comprises only carbon or hydrogen atoms in its structure. In other words, such a wax is free of other atoms, in particular heteroatoms such as for example nitrogen, oxygen, silicon.
For the purposes of illustration of non-polar waxes suitable for the invention, mention can in particular be made of hydrocarbon waxes such as microcrystalline waxes, paraffin waxes, ozokerite, polymethylene waxes, polyethylene waxes, waxes obtained by Fischer- Tropsch synthesis, microwaxes in particular of polyethylene.
Preferably, the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 45°C. Preferably, the wax having a melting point greater than or equal to 45°C comprises at least one fatty alcohol.
Preferably, the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 70°C. Preferably, the wax having a melting point greater than or equal to 70°C is chosen from paraffin waxes, ozokerite, polymethylene waxes and polyethylene waxes.
Preferably, the oily phase of step a) comprises at least 0.1% by weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight with respect to the total weight of the mixture of at least one wax, preferably the melting point of which is greater than or equal to 45°C, preferably greater than or equal to 70°C.
Preferably, the wax having a melting point greater than or equal to 70°C is a non-polar hydrocarbon wax, preferably a polyethylene wax, and said non-polar hydrocarbon wax represents at least 50% by weight with respect to the total weight of wax(es) of the mixture.
Pasty fat(s)
For the purposes of the invention, the term "pasty fat" denotes a lipophilic fatty compound having a reversible solid/liquid change of state, having an anisotropic crystalline organization in the solid state, and including a liquid fraction and a solid fraction at a temperature of 23°C.
In other words, the initial melting point of the pasty compound can be less than 23°C. The liquid fraction of the pasty compound measured at 23°C can represent 9 to 97% by weight of the compound. This liquid fraction at 23°C preferably represents between 15 and 85%, more preferably between 40 and 85% by weight.
The melting point of a solid fat can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the trade name "DSC Q100" by TA Instruments with "TA Universal Analysis" software, according to the protocol defined hereinabove.
The liquid fraction by weight of the pasty compound at 23°C is more particularly equal to the ratio of the enthalpy of fusion consumed at 23°C to the enthalpy of fusion of the pasty compound.
The enthalpy of fusion of the pasty compound is the enthalpy consumed by the compound to change from the solid state to the liquid state. The pasty compound is said to be in the solid state when the entire mass thereof is in solid crystalline form. The pasty compound is said to be in the liquid state when the entire mass thereof is in liquid form.
The enthalpy of fusion of the pasty compound is in particular equal to the area under the curve of the thermogram obtained using a differential scanning calorimeter. The enthalpy of fusion of the pasty compound is the quantity of energy required to change the compound from the solid state to the liquid state. It is expressed in J/g.
The enthalpy of fusion consumed at 23°C is the quantity of energy required by the sample to change from the solid state to the state present at 23°C consisting of a liquid fraction and a solid fraction.
The pasty compound(s) can be in particular chosen from synthetic pasty compounds and fats of plant origin. The pasty compound(s) can be hydrocarbon or silicone.
The pasty compound(s) can be in particular chosen from:
- lanolin and its derivatives, such as lanolin alcohol, oxyethylenated lanolins, acetylated lanolin, lanolin esters such as isopropyl lanolate, oxypropylenated lanolins;
- petroleum jelly (also called petrolatum),
- polyol ethers chosen from C2-C4 pentaerythritol and polyalkylene glycol ethers, fatty alcohol and sugar ethers, and mixtures thereof. For example, mention can be made of pentaerythritol and polyethylene glycol ether comprising 5 oxyethylene (5 OE) units (CTFA name: PEG-5 Pentaerythrityl Ether), pentaerythritol and polypropylene glycol ether comprising 5 oxypropylene units (5 OP) (CTFA name: PPG-5 Pentaerythrityl Ether), and mixtures thereof and more specifically the mixture of PEG-5 Pentaerythrityl Ether, PPG-5 Pentaerythrityl Ether and soybean oil, sold under the trade name "Lanolide" by VEVY, wherein the ratio of the constituents by weight is 46:46:8: 46% PEG-5 Pentaerythrityl Ether, 46% PPG-5 Pentaerythrityl Ether and 8% soybean oil,
- optionally polymeric silicone compounds,
- optionally polymeric fluorinated compounds,
- vinyl polymers, in particular: oolefin homopolymers and copolymers; o hydrogenated diene homopolymers and copolymers; o branched oligomers, alkyl (meth)acrylate homo or copolymers preferably having a C8-C30 alkyl group, ovinyl ester homo and copolymer oligomers, having C8-C30 alkyl groups, and ovinylether homo and copolymer oligomers, having C8-C30 alkyl groups,
- liposoluble polyethers derived from polyetherification between one or a several C2- C100, preferably C2-C50, diols. Of the liposoluble polyethers, particular consideration is given to ethylene-oxide and/or propylene-oxide copolymers with C6-C30 long-chain alkylene-oxides, more preferably such that the weight ratio of ethylene-oxide and/or propylene-oxide with alkylene-oxides in the copolymer is 5:95 to 70:30. In this family, particular mention can be made of copolymers such as long-chain alkylene-oxides arranged in blocks having a mean molecular weight of 1000 to 10,000, for example a polyoxyethylene/polydodecyl glycol block copolymer such as the dodecanediol (22 mol) and polyethylene glycol (45 OE) ethers sold under the brand ELFACOS ST9 by AKZO NOBEL.
- esters and polyesters. Among esters, particular consideration is given to: ooligomer glycerol esters, especially the esters of diglycerol, with monocarboxylic acids, optionally hydroxylated, linear or branched, saturated or not, preferably saturated, C6-C20, and/or dicarboxylic acids, linear or branched, saturated or not, preferably saturated, C6-C10, in particular condensates of adipic acid and diglycerol, for which a portion of the hydroxyl groups of the glycerols have reacted with a mixture of fatty acids, such as stearic acid, capric acid, stearic acid, isostearic acid and 12-hydroxystearic acid, such as for example bis-diglyceryl polyacyladipate-2 sold under the reference SOFTISAN® 649 by Sasol, o homopolymers of vinyl ester having C8-C30 alkyl groups, such as polyvinyl laurate (in particular sold under the reference Mexomere PP by Chimex), oarachidyl propionate sold under the brand Waxenol 801 by ALZO, o phytosterol esters, otriglycerides of fatty acids and their derivatives, in particular triglycerides of fatty acids, saturated or not, linear or branched, optionally mono or poly hydroxylated, C6-C30, more particularly C8-C18, optionally hydrogenated (totally or partially); with for example Softisan 100® sold by Sasol, o pentaerythritol esters, oaliphatic esters derived from esterification of an aliphatic hydroxycarboxylic acid with an aliphatic carboxylic acid. More particularly, the aliphatic carboxylic acid is C4-C30, preferably C8-C30. It is preferably chosen from hexanoic, heptanoic, octanoic, 2- ethylhexanoic, nonanoic, decanoic, undecanoic, dodecanoic, tridecanoic, tetradecanoic, pentadecanoic, hexadecanoic, hexyldecanoic, heptadecanoic, octadecanoic, isostearic, nonadecanoic, eicosanoic, isoarachidic, octyldodecanoic, heneicosanoic and docosanoic acids, and mixtures thereof. The aliphatic carboxylic acid is preferably branched. The hydroxycarboxylic acid ester is advantageously derived from a C2-C40 hydroxylated carboxylic acid, preferably C10 - C34, and more preferably C12 - C28; with the number of hydroxyl groups being between 1 and 20, more particularly between 1 and 10, preferably between 1 and 6.
Said hydroxycarboxylic acid esters are preferably chosen from: a) total or partial saturated, linear and monohydroxylated aliphatic monocarboxylic acid esters; b) total or partial saturated, monohydroxylated aliphatic monocarboxylic acid esters; c) total or partial saturated, monohydroxylated aliphatic polycarboxylic acid esters; d) total or partial saturated, polyhydroxylated aliphatic polycarboxylic acid esters; e) partial or total C2 -C16 aliphatic polyol esters with a mono or polyhydroxylated aliphatic mono or polycarboxylic acid f) mixtures thereof. odimer diol and dimer diacid esters, where applicable, esterified on their free alcohol or acid function(s) by acid or alcohol radicals, in particular dimer dilinoleate esters; such esters can particularly be chosen from esters having the following INCI classification: bis- behenyl/isostearyl/phytosteryl dimer dilinoleyl dimer dilinoleate (Plandool G), phytosteryl I isosteryl I cetyl I stearyl I behenyl dimer dilinoleate (Plandool H or Plandool S) and mixtures thereof, ohydrogenated rosin esters (Lusplan DD-DHR or DD-DHR from Nippon Fine Chemical)
- butters of plant origin, such as mango butter, such as that sold under the reference Lipex 203 by AARHUSKARLSHAMN, shea butter, in particular that having the INCI name Butyrospermum Parkii Butter, such as that sold under the reference Sheasoft® by AARHUSKARLSHAMN, cupuacu butter (Rain forest RF3410 from Beraca Sahara), murumuru butter (RAIN FOREST RF3710 from Beraca Sahara), cocoa butter, babassu butter such as that sold under the name Cropure Babassu SS-(LK) by Croda, as well as orange wax such as, for example, that sold under the reference Orange Peel Wax by Koster Keunen,
- totally or partially hydrogenated plant oils, such as for example hydrogenated soybean oil, hydrogenated coconut oil, hydrogenated rapeseed oil, mixtures of hydrogenated plant oils such as the mixture of hydrogenated plant oils of soybean, coconut, palm and rapeseed, for example the mixture sold under the reference Akogel® by AARHUSKARLSHAMN (INCI name Hydrogenated Vegetable Oil), trans isomerized partially hydrogenated jojoba oil manufactured or sold by Desert Whale under the commercial reference I so- Jojoba-50®, partially hydrogenated olive oil such as, for example, the compound sold under the reference Beurrolive by Soliance,
- hydrogenated castor oil esters, such as dimer dilinoleate hydrogenated castor oil for example RISOCAST-DA-L sold by KOKYU ALCOHOL KOGYO, hydrogenated castor oil isostearate for example SALACOS HCIS (V-L) sold by NISSHIN OIL, - and mixtures thereof.
Preferably, the pasty compound(s) are chosen from:
- petroleum jelly;
- C2-C4 pentaerythritol and polyalkylene glycol ethers;
- fatty alcohol and sugar ethers;
- ethylene-oxide and/or propylene-oxide copolymers with C6-C30 long-chain alkylene-oxides;
- oligomer glycerol esters, particularly the esters of diglycerol, with monocarboxylic acids, optionally hydroxylated, linear or branched, saturated or not, preferably saturated, C6-C20, and/or dicarboxylic acids, linear or branched, saturated or not, preferably saturated, C6-C10; in particular BIS-DIGLYCERYL POLYACYLADI PATE-2 (INCI name),
- vinyl ester homopolymers having C8-C30 alkyl groups;
- arachidyl propionate;
- triglycerides of fatty acids, saturated or not, linear or branched, possibly mono or poly hydroxylated, C6-C30, more particularly C8-C18, optionally hydrogenated;
- pentaerythritol esters;
- non-crosslinked esters obtained by condensation of a C4-C50 linear or branched di- or poly-carboxylic acid and of a C2-C50 diol or polyol, aliphatic esters obtained by reacting a hydroxycarboxylic acid ester and of an aliphatic carboxylic acid; advantageously the carboxylic acid is C4-C30,
- dimer diol and dimer diacid esters, such as dilinoleic dimer esters;
- butters of plant origin,
- partially hydrogenated plant oils,
- and mixtures thereof.
According to an embodiment, the composition comprises from 1 to 20% by weight of pasty fat, with respect to the total weight of the composition, preferably from 5 to 15% by weight, preferably from 10 to 15% by weight.
Other ingredient(s) of the oily phase
The oily phase of the composition prepared according to the invention can also comprise at least one additional fat chosen from at least one hydrophobic film-forming hydrocarbon resin, at least one silicone resin, at least one non-volatile hydrocarbon (polar or non-polar) oil, and mixtures thereof. The oily phase of the composition prepared according to the invention preferably comprises at least one oil, preferably non-volatile, preferably hydrocarbon.
Preferably, the oily phase of step a) further comprises at least one, preferably at least two fat(s) chosen from waxes and pasty fats, at least one hydrophobic film-forming hydrocarbon resin, at least one silicone resin and at least one non-volatile polar or nonpolar hydrocarbon oil.
Hydrophobic film-forming hydrocarbon resin
The hydrophobic film-forming hydrocarbon resin is preferably an indenic resin. The term "resin" refers to a compound the structure of which is three-dimensional.
The composition may comprise one or several indenic hydrocarbon resins at a total concentration ranging preferably from 0.1 to 20% by weight, preferably from 0.5 to 15% by weight, more preferably from 1 to 10% by weight, even more preferably from 1.5 to 8% by weight, with respect to the total weight of the composition.
The indenic hydrocarbon resin(s) are chosen preferably from resins obtained from polymerizing a majority proportion of indene monomer and a minority proportion of monomer chosen from styrene, methylindene, methylstyrene and mixtures thereof; these resins optionally being hydrogenated. These resins can have a molecular weight ranging from 290 to 1150 g/mol.
As examples of indenic resins, mention can be made of those sold under the reference ESCOREZ 7105 by Exxon Chem., NEVCHEM 100 and NEVEX 100 by Neville Chem., NORSOLENE S105 by Sartomer, PICCO 6100 by Hercules and RESINALL by Resinall Corp., or indene/methylstyrene/hydrogenated styrene copolymers sold under the trade name "REGALITE" by Eastman Chemical, in particular REGALITE R 1100, REGALITE R 1090, REGALITE R-7100, REGALITE R1010 HYDROCARBON RESIN, REGALITE R1125 HYDROCARBON RESIN.
Preferably, the composition comprises at least one hydrocarbon resin solid at ambient temperature (20°C).
Preferably, the composition comprises one or several resins chosen from indene/methylstyrene/hydrogenated styrene copolymers. In particular, the indene/methylstyrene/hydrogenated styrene copolymers sold under the trade name "REGALITE" by Eastman Chemical, such as REGALITE R 1100 CG HYDROCARBON RESIN, REGALITE R 1100, REGALITE R 1090, REGALITE R-7100, REGALITE R1010 HYDROCARBON RESIN, REGALITE R1125 HYDROCARBON RESIN can be used. Silicone resin
The composition according to the invention can comprise at least one silicone resin. The term "resin" refers to a compound the structure of which is three-dimensional. As such, for the purposes of the present invention, a polydimethylsiloxane is not a silicone resin.
The classification of silicone resins (also called siloxane resins) is known under the name "MDTQ", the resin being described according to the various siloxane monomeric units comprised therein, each of the letters "MDTQ" characterizing a type of unit.
The letter "M" represents the Monofunctional unit having the formula R1 R2R3SiOi/2, the silicon atom being bound to a single oxygen atom in the polymer comprising this unit.
The letter "D" denotes a Difunctional unit R1 R2SiO2/2 wherein the silicon atom is bound to two oxygen atoms.
The letter "T" represents a Trifunctional unit having the formula R1SiO3/2.
Such resins are described for example in "Encyclopedia of Polymer Science and Engineering, vol. 15, John and Wiley and Sons, New York, (1989), p. 265-270, and US 2,676,182, US 3,627,851 , US 3,772,247, US 5,248,739 or US 5,082,706, US 5,319,040, US 5,302, 685 and US 4,935,484.
In the M, D, T structural units defined above, Ri, namely R1 , R2 and R3, identical or different, represent a hydrocarbon radical (in particular alkyl) having from 1 to 10 carbon atoms, a phenyl group, a phenylalkyl group or a hydroxyl group.
Finally, the letter "Q" denotes a Tetrafunctional unit SiO4/2 wherein the silicon atom is bound to four oxygen atoms in turn bound to the remainder of the polymer.
Various silicone resins having different properties can be obtained from these various units, the properties of these polymers varying according to the type of monomers (or units), the type and number of the Ri radical(s), the polymer chain length, the degree of branching and the pendant chain size.
As silicon resins that can be used in the compositions according to the invention use can be made for example of MQ type, T type or MQT type silicone resins.
MQ resins:
As examples of MQ type silicone resins, mention can be made of alkylsiloxysilicates having formula [(R1)3SiOi/2]x(SiO4/2)y (MQ units) wherein x and y are integers ranging from 50 to 80, and such that the group R1 represents a radical as defined hereinabove, and preferably is an alkyl group having from 1 to 8 carbon atoms, or a hydroxyl group, preferably, a methyl group.
As examples of trimethylsiloxysilicate type MQ type solid silicone resins, mention can be made of those sold under the reference SR1000 by General Electric, under the reference TMS 803 by Wacker, under the trade name "KF-7312J" by Shin-Etsu, "DC 749", "DC 593" by Dow Corning.
Like the silicone resins comprising MQ siloxysilicate units, mention can also be made of phenylalkylesiloxysilicate resins, such as phenylpropyldimethylsiloxysilicate (Silshine 151 sold by General Electric). The preparation of such resins is described in particular in patent US5817302.
T resins:
As examples of T type silicone resins, mention can be made of polysilsesquioxanes having formula (RSiOs/2)x (T units) wherein x is greater than 100 and such that the R group is an alkyl group having from 1 to 10 carbon atoms, said polysilsesquioxanes can furthermore include Si-OH terminal groups.
Mention can also be made of polymethylsilsesquioxanes which are polysilsesquioxanes wherein none of the methyl radicals is substituted by another group. Such polymethylsilsesquioxanes are described for example in document US 5,246,694.
Preferably, polymethylsilsesquioxane resins can be used wherein R is a methyl group, such as for example those sold:
- - by Wacker under the reference Resin MK such as Belsil PMS MK: polymer comprising CH3SiO3/2 repeat units (T units), that may also comprise up to 1% by weight of (CH3)2SiO2/2 units (D units) and having a mean molecular weight of approximately 10000 g/mol, or
- - by SHIN-ETSU under the references KR-220L consisting of T units having formula CH3SiC>3/2 and having Si-OH (silanol) terminal groups, under the reference KR-242A comprising 98% T units and 2% dimethyl units and having Si-OH terminal groups of under the reference KR-251 comprising 88% units and 12% D dimethyl units and having Si-OH terminal groups.
MQT resins:
As a resin comprising MQT units, those mentioned in document US 5 110 890 are known.
A preferred form of MQT type resins are MQT-propyl resins (also called MQTPr). Such resins that can be used in the compositions according to the invention are in particular those described and prepared in application WO 2005/075542, the content of which is incorporated here by reference.
The MQ-T-propyl resin preferably comprises the units:
- (i) (R13SiOi/2)a - (ii) (R22SiO2/2)b
- (iii) (RSSiC c and
- (iv) (SiO4/2)d where
- R1 , R2 and R3 independently are a hydrocarbon radical (in particular alkyl) having from 1 to 10 carbon atoms, a phenyl group, a phenylalkyl group or a hydroxyl group and preferably an alkyl radical having from 1 to 8 carbon atoms or a phenyl group,
- a, b, c and d are molar fractions,
- a is between 0.05 and 0.5,
- b is between zero and 0.3,
- c being greater than zero,
- d is between 0.05 and 0.6,
- a + b + c + d = 1 ,
- with the condition that more than 40% in moles of the R3 groups of the siloxane resin are propyl groups.
Preferably, the siloxane resin comprises the units:
- (i) (R13SiOi/2)a
- (iii) (RSSiC c and
- (iv) (SiO4/2)d where
- R1 and R3 independently are an alkyl group having from 1 to 8 carbon atoms, R1 being preferably a methyl group and R3 preferably being a propyl group,
- a is between 0.05 and 0.5, preferably between 0.15 and 0.4,
- c is greater than zero, preferably between 0.15 and 0.4,
- d is between 0.05 and 0.6, preferably between 0.2 and 0.6, or between 0.2 and 0.55, - a + b + c + d = 1 , and a, b, c and d being molar fractions,
- with the condition that more than 40% in moles of the R3 groups of the siloxane resin are propyl groups.
The siloxane resins that can be used according to the invention can be obtained by a method comprising the reaction of: a) an MQ resin comprising at least 80% in moles of (Rl3SiOi/2)a and (SiC>4/2)d units
- R1 being an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group,
- a and d being greater than zero, - the a/d ratio being between 0.5 and 1.5; and of b) a T propyl resin comprising at least 80% in moles of (R3SiC>3/2)c units,
- R3 being an alkyl group having from 1 to 8 carbon atoms, an aryl group, a carbinol group or an amino group,
- c being greater than zero,
- with the condition that at least 40% in moles of the R3 groups are propyl groups,
- where the A/B mass ratio is between 95:5 and 15:85, preferably the A/B mass ratio is 30:70.
Advantageously, the A/B mass ratio is between 95:5 and 15:85. Preferably, the A/B ratio is less than or equal to 70:30. These preferred ratios have proven to allow comfortable deposits.
Preferably, the composition according to the invention comprises, as a silicone resin, at least one MQ type resin as described hereinabove.
In particular, the silicone resin is a siloxysilicate resin, preferably a trimethylsiloxysilicate resin.
Advantageously, the silicone resin is present in a concentration of at least 5% by weight, preferably in a concentration ranging from 5 to 15% by weight with respect to the total weight of the composition, or preferably from 6 to 9% by weight, with respect to the total weight of the composition.
Polar or non-polar oil
"Oil" means a non-aqueous compound, liquid at 25°C and at atmospheric pressure (1.013.105 Pa), non-miscible in water.
"Non-miscible" means that the mixture of the same quantity of water and oil, after stirring, does not lead to a stable solution that comprises only a single phase, under the aforementioned temperature and pressure conditions. The observation is made with the naked eye or using a phase contrast microscope if necessary, on 100g of mixture obtained after Rayneri stirring sufficient to cause a vortex to appear within the mixture (for the purposes of information 200 to 1000 rpm); the resulting mixture being left to sit, in a closed bottle, for 24 hours at ambient temperature before observation. "Non-volatile oil" means an oil, the vapor pressure of which at 25°C and atmospheric pressure, is not zero and is less than 2.66 Pa, more particularly less than or equal to 0.13 Pa. By way of example, the vapor pressure can be measured in accordance with the static method or by the isothermal thermogravimetry effusion method, according to the vapor pressure (OCDE 104).
"Hydrocarbon oil" means an oil essentially formed, or consisting, of carbon and hydrogen atoms, and optionally oxygen, nitrogen atoms, and containing no silicon or fluorine atoms. The hydrocarbon oil is therefore distinct from a silicone oil and from a fluorine oil.
It may contain alcohol, ester, ether, carboxylic acid, amine and/or amide groups.
Preferably, the oil is a hydrocarbon oil, i.e. it is free of heteroatoms such as nitrogen, sulfur and phosphorus.
When the hydrocarbon oil is non-volatile and polar, it comprises at least one oxygen atom. In particular, this non-volatile polar hydrocarbon oil comprises at least one alcohol function (it is then an "alcohol oil") or at least one ester function (it is then an "ester oil"). The ester oils that can be used in the compositions according to the invention can in particular be hydroxylated. The composition can comprise one or several non-volatile hydrocarbon oils, in particular chosen from C10-C26 alcohols, preferably monoalcohols; monoesters, diesters, triesters, optionally hydroxylated, of a C2-C8 mono or polycarboxylic acid and a C2-C8 alcohol; esters of a C2-C8 polyol and one or several C2-C8 carboxylic acids, in particular having between 17 and 70 carbon atoms; vinylpyrrolidone/1 -hexadecene copolymers; dialkyl carbonates and mixtures thereof. Preferably, the non-volatile polar hydrocarbon oil(s) are chosen from C10-C26 monoalcohols, ester oils, and in particular monoesters comprising at least 17 carbon atoms in total, diesters, hydroxylated or not, comprising at least 18 carbon atoms in total, triesters, in particular having at least 35 carbon atoms, tetraesters, in particular having at least 35 carbon atoms, as well as mixtures thereof.
When the hydrocarbon oil is non-volatile and non-polar, it is chosen from compounds only comprising carbon and hydrogen atoms. Said oils, linear or branched, can be of mineral or synthetic origin such as for example:
- paraffin oil,
- squalane, in particular of plant origin,
- isoeicosane,
- saturated linear hydrocarbon mixtures, more particularly the mixtures for which the INCI names are for example as follows: C18-21 Alkane, C21-28 Alkane, such as for example the products Gemseal 60, Gemseal 120 sold by Total, - polybutenes, hydrogenated polybutenes, such as for example products of the Indopol range sold by Ineos Oligomers,
- polyisobutenes, hydrogenated polyisobutenes such as for example Parleam® sold by NIPPON OIL FATS, PANALANE H-300 E sold by INEOS OLIGOMERS, REWOPAL PIB 1000 sold by EVON IK,
- decene/butene copolymers, polybutene/polyisobutene copolymers particularly Indopol L-14,
- polydecenes and hydrogenated polydecenes such as for example PURESYN 10, PURESYN 150 or PURESYN 6 sold by EXXONMOBIL CHEMICAL), Silkflo 366, Silkflo 364 sold by INEOS OLIGOMERS, Dekanex 2008 by IMCD,
- and mixtures thereof.
Advantageously, the oil is present in a concentration of at least 5% by weight, preferably in a concentration ranging from 5 to 30% by weight with respect to the total weight of the composition, or preferably from 10 to 25% by weight, with respect to the total weight of the composition.
At the end of step a), an oily phase comprising at least one, preferably at least two, fats chosen from waxes, pasty fats and mixtures thereof, is obtained in a tank.
Step b)
According to step b), the oily phase obtained in a) is heated to a temperature greater than the melting point(s) of the fat(s) (chosen from waxes, pasty fats and mixtures thereof).
This step b) makes it possible to melt said fat(s) completely.
In the case where steps a) and c) are simultaneous, an aqueous phase and an oily phase comprising at least one fat at least partly solid at a temperature of 25°C chosen from waxes, pasty fats and mixtures thereof, are mixed (steps a and c)) prior to the heating step b). This step b) makes it possible to melt said fat(s) completely in the mixture.
Typically, this step b) is performed under stirring.
At the end of step b), a homogeneous liquid oily phase is obtained.
In the case where steps a) and c) are simultaneous, at the end of step b), a homogeneous mixture of liquid oily phase and aqueous phase is in particular obtained. Step (c)
Step c) is optional: indeed, it is possible to add an aqueous phase into the heated mixture of step b), to obtain a cosmetic composition in dispersion or emulsion form. The aqueous phase added may be a dispersed aqueous phase. Such an emulsion is then an invert (water-in-oil or W/O) emulsion. The aqueous phase added can be a continuous aqueous phase; such an emulsion is then a direct (oil-in-water or O/W) emulsion.
If this step c) is not present, then the composition obtained is anhydrous (consists of the oily phase).
The aqueous phase can consist essentially of water; it can also comprise a mixture of water and water-miscible solvent (miscibility in water greater than 50% by weight at 25°C) such as lower monoalcohols having from 1 to 5 carbon atoms such as ethanol, isopropanol, glycols having from 2 to 8 carbon atoms such as propylene glycol, ethylene glycol, 1 ,3- butylene glycol, dipropylene glycol, and mixtures thereof.
The composition preferably comprises a water concentration that represents at least 7% by weight, preferably a concentration ranging from 7% to 40% by weight, with respect to the total weight of the composition. Advantageously, the water of the aqueous phase is present in a quantity between 7% and 30% by weight, preferably between 10% and 30% by weight, preferably between 15 and 30% by weight with respect to the total weight of the composition.
The composition according to the invention can comprise, in addition to the compounds described hereinabove, water-in-oil surfactants, volatile oils, aqueous phase thickeners or any of the mixtures thereof. It is understood that the quantity of these ancillary compounds can be adjusted by those skilled in the art in such a way as to not bear prejudice to the effect sought within the scope of the present invention.
The compositions of the invention can comprise surfactant agents of the water-in-oil type. Preferably, the surfactant has an HLB (hydrophilic/lipophilic balance) less than or equal to 8, more particularly less than or equal to 7, preferably between 1 and 6. Preferably, it is non-ionic. The HLB value as per GRIFFIN is defined in J. Soc. Cosm. Chem. 1954 (volume 5), pages 249-256.
Preferably, the surfactant(s) are chosen from silicone non-ionic surfactants, from hydrocarbon non-ionic surfactants, or from mixtures thereof. With regards to silicone surfactants, mention can be made of alkyl or alkoxy dimethicone copolyols with pendant alkyl or alkoxy chain or silicone backbone-end having for example from 6 to 22 carbon atoms; dimethicone copolyols, which are more particularly oxypropylene and/or oxyethylene polydimethyl methyl siloxanes, as well as crosslinked solid elastomeric organopolysiloxanes that comprise at least one oxyalkylene group, and mixtures thereof. Among the particularly preferred silicone surfactants, mention can be made of dimethicone copolyols such as for example those sold under the trade names KF- 6015 (PEG-3 dimethicone), KF-6016 (PEG-9 methyl ether dimethicone), KF-6017 (PEG-10 dimethicone), KF-6028 (PEG-9 polydimethylsiloxyethyl dimethicone), KF-6050 L (PEG/PPG 18/18 dimethicone in cyclopentasiloxane), by Shin-Etsu; dimethicone copolyols sold under the trade names Dow Corning 3225C (PEG/PPG-18/18 Dimethicone in a mixture of cyclotetrasiloxane and cyclopentasiloxane), DC 5225 C Formulation Aid (PEG/PPG- 18/18 Dimethicone in cyclopentasiloxane); or the product sold under the trade name SF 1528 GE (mixture of PEG/PPG-20/15 Dimethicone and cyclopentasiloxane) by Momentive Performance Materials. Alkyl-dimethicone copolyols can also be used such as Lauryl PEG/PPG- 18/18 Methicone (which is more particularly an alkoxyl derivative of Lauryl Methicone containing on average 18 moles of ethylene oxide and 18 moles of propylene oxide, sold under the trade name "Dow Corning 5200 Formulation Aid" by Dow Corning; cetyl PEG/PPG-10/1 Dimethicone (which is more particularly a copolymer of Cetyl Dimethicone and an alkoxyl derivative of dimethicone containing on average 10 moles of ethylene oxide and 1 mole of propylene oxide) such as the product sold under the trade name Abil EM 90 by Evonik Goldschmidt as well as the mixture of cetyl PEG/PPG-10/1 Dimethicone, polyglycerol isostearate (4 moles) and hexyl laurate sold under the trade name ABIL WE 09 by Evonik Goldschmidt.
Preferably, the composition comprises as silicone surfactant(s), C8-C22 alkyl dimethicone copolyol such as cetyl dimethicone copolyol, in particular having the INCI name CETYL PEG/PPG-10/1 DIMETHICONE, dimethicone copolyols such as for example PEG- 10 dimethicone, PEG/PPG 18/18 dimethicone, as well as mixtures thereof. A mixture of cetyl dimethicone copolyol with polyglyceryl-4-isostearate and hexylaurate can also be used, such as the product sold under the name Abil WE-09 by Evonik Goldschmidt (the INCI name is polyglyceryl-4-isostearate (and) hexylaurate (and) cetyl PEG/PPG-10/1 dimethicone).
Non-ionic surfactants can also be chosen in particular from polyoxyethylenated C8- C30 alcohols, (poly)oxyethylenated and/or (poly)oxypropylenated polyalkyl(Cs-C3o)- and polyalkyl(Cs-C3o)- esters; fatty acid polyesters, preferably polyhydroxylated, C12-C20, polyoxyethylenated, having from 4 to 50 moles of ethylene oxide; alkyl- and polyalkyl- esters of sorbitan; alkyl- and polyalkyl- esters of (poly)glycerol and mixtures thereof. As alkyl(Cs- C30)- and polyalkyl(Cs-C3o)- esters of (poly)glycerol, those having a number of glycerol units ranging from 1 to 4 are preferably used. Mention can be made for example of polyglyceryl- 4 isostearate (Isolan Gl 34 sold by Evonik Goldschmidt); polyglyceryl-3 diisostearate (Lameform TGI sold by Cognis), glyceryl stearate, glyceryl laurate, alone or in mixtures.
According to a particularly preferred embodiment, the composition comprises at least one silicone non-ionic surfactant. Advantageously, the silicone surfactant or surfactants are chosen from dimethicone copolyols, alkyl dimethicone copolyols described hereinabove, in particular alkyl C8-C22 dimethicone copolyols in particular having formula (I), alone or in mixtures. According to a particular embodiment of the invention, the composition also comprises at least one hydrocarbon non-ionic surfactant, very particularly alkyl- and polyalkyl- esters of (poly)glycerol and/or of sorbitan, and preferably polyglyceryl-3 diisostearate, polyglyceryl-4 isostearate, sorbitan isostearate or sorbitan and glycerol isostearate.
The surfactant(s) can be present in the composition in a concentration ranging from 0.1 to 20% by weight, and preferably from 0.5 to 15%, preferably from 1 to 10% by weight, with respect to the total weight of the composition.
The aqueous phase can also comprise at least one hydrophilic thickening polymer (also called aqueous phase thickening polymer).
Typically, step c), like step b), is performed under stirring.
Dyes and/or active agents
Preferably, the cosmetic mixture obtained in step b) or c) (i.e. the oily phase or the composition obtained in step b) or c)) comprises at least one dye and/or at least one active agent.
The dye is typically chosen from water-soluble or liposoluble colorants, pigments, nacres and mixtures thereof. The dye can also be a pigmentary paste.
The dyes can be present, in the composition, at a concentration ranging from 0.01% to 25% by weight, with respect to the weight of the composition, preferably from 0.01% to 20% by weight.
The term "colorants" refers to generally organic compounds soluble in fats such as oils or in an aqueous or hydroalcoholic phase. The water-soluble dyes used according to the invention are more particularly water- soluble colorants. The term "water-soluble colorant" refers, for the purposes of the invention, to any generally organic, natural or synthetic compound, soluble in an aqueous phase or water-miscible solvents and able to dye. In particular, the term water-soluble is intended to characterize the ability of a compound to be solubilized in water, measured at 25°C, at a concentration at least equal to 0.1 g/l (obtaining a macroscopically isotropic and transparent solution, colored or not). This solubility is in particular greater than or equal to 1 g/l. As water-soluble colorants that are suitable for the invention, mention can in particular be made of synthetic or natural water-soluble colorants such as for example DC Red 6 (Lithol Rubine Na; Cl: 15850), DC Red 22 (Cl: 45380), DC Red 28 (Cl: 45410, Na salt), DC Red 30 (Cl: 73360), DC Red 33 (Cl: 17200), DC Red 40 (Cl: 16035), FDC Yellow 5 (Cl: 19140), FDC Yellow 6 (Cl: 15985), DC Yellow 8 (Cl: 45350 Na salt), FDC Green 3 (Cl: 42053), DC Green 5 (Cl: 61570), FDC Blue 1 (Cl: 42090). Given by way of illustration and not limiting examples of sources of water-soluble dye(s) that can be implemented within the scope of the present invention, mention can in particular be made of those of natural origin, such as extracts of carmine, cochineal, beet, grape, carrot, tomato, rocou, paprika, henna, caramel and curcumin. As such, the water-soluble dyes that are suitable for the invention are in particular carminic acid, betanin, anthocyanins, enocyanins, lycopene, bixin, norbixin, capsanthyn, capsorubin, flovoxanthin, lutein, cryptoxanthin, rubixanthin, violaxanthin, riboflavin, roudoxanthin, cantaxanthin, chlorophyll, and mixtures thereof. They can also consist of copper sulfate, iron, water-soluble sulfopolyesters, rhodamine, betaine, methylene blue, disodium tartrazine salt and fuchsin disodium salt. Some of these water- soluble dyes are in particular approved from a food standpoint. By way of example of these colorants, more particular mention can be made of the colorants in the carotenoid family, referenced under food codes E120, E162, E163, E160a-g, E150a, E101 , E100, E140 and E141. According to a particularly preferred embodiment, the water-soluble dye(s) are chosen from the sodium salts of Yellow 6, Yellow 5, Red 6, Red 33, Red 40.
The term "liposoluble colorant" refers, for the purposes of the invention, to any generally organic, natural or synthetic compound, soluble in an oily phase or solvents miscible in the oily phase and able to dye. By way of liposoluble colorants suitable for the invention, mention can particularly be made of liposoluble colorants such as 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, Sudan brown. By way of illustration of natural liposoluble colorants, mention can particularly be made of carotenes such as p-carotene, a-carotene, lycopene; quinoline yellow; xanthophylls such as astaxanthin, antheraxanthin, citranaxanthin, cryptoxanthin, canthaxanthin, diatomoxanthin, flavoxanthin, fucoxanthin, lutein, rhodoxanthin, rubixanthin, siphonaxanthin, violaxanthin, zeaxanthin; annatto; curcumin; quinizarin (Ceres Green BB, D&C Green No. 6, Cl 61565, 1 ,4-Di-p-Toluidinoanthraquinone, Green No. 202, Quinzaine Green SS) and chlorophylls.
The term "pigments" should be understood to mean white or colored, mineral or organic particles, which are insoluble in an aqueous solution and are intended for coloring and/or opacifying the resulting deposit. The pigments can be present in a proportion of 0.01 % to 25% by weight, in particular from 0.01 % to 20% by weight, with respect to the total weight of the cosmetic composition. The pigments can be chosen from mineral pigments, organic pigments, and composite pigments (i.e. pigments with a mineral and/or organic material base). The pigments can be chosen from monochrome pigments, lacquers, nacres, optical-effect pigments, such as reflective pigments and goniochromatic pigments.
According to a particular embodiment, the pigments used according to the invention are chosen from mineral pigments.
"Mineral pigment" means any pigment that complies with the definition in Ullmann’s Encyclopedia in the Inorganic Pigment chapter. Mention can be made, among the mineral pigments that can be used in the present invention, of zirconium or cerium oxides, along with zinc, iron (black, yellow or red) or chromium oxides, manganese violet, ultramarine blue, chromium hydrate and iron blue, titanium dioxide, metallic powders such as aluminum powder and copper powder. The following mineral pigments can also be used: Ta2O5, Ti3O5, Ti2O3, TiO, ZrO2 in a mixture with TiO2, ZrO2, Nb2O5, CeO2, ZnS.
The size of the pigment that can be used within the scope of the present invention is in general greater than 100 nm and can range up to 10 pm, preferably from 200 nm to 5 pm, and more preferably from 300 nm to 1 pm. According to a particular embodiment of the invention, the pigments have a size characterized by a D[50] greater than 100 nm and can range up to 10 pm, preferably from 200 nm to 5pm, and more preferably from 300 nm to 1 pm. The sizes are measured by laser diffraction by means of a commercial MasterSizer 3000® granulometer from Malvern, making it possible to ascertain the granulometric distribution of all the particles over a wide range that can range from 0.01 pm to 1000 pm. The data are processed on the basis of the classic Mie scattering theory. This theory is the most adapted for size distributions ranging from submicron to multi-micron, and makes it possible to determine an "effective" diameter of particles. This theory is described particularly in the book by Van de Hulst, H.C., "Light Scattering by Small Particles", Chapters 9 and 10, Wiley, New York, 1957. D[50] represents the maximum size of 50% by volume of the particles.
Within the scope of the present invention, the mineral pigments are more particularly iron oxide and/or titanium dioxide. By way of example, mention can be made more particularly of titanium dioxide and iron oxide, coated with aluminum stearoyl glutamate for example marketed under the reference NAI® by Miyoshi Kasei.
As mineral pigments that can be used in the invention, nacres can also be mentioned. The term "nacres" should be understood to mean iridescent or non-iridescent colored particles of any shape, which are in particular produced by certain mollusks in their shell or else are synthesized and which exhibit a color effect by optical interference. The nacres can be selected from pearlescent pigments such as titanium mica coated with iron oxide, titanium mica coated with bismuth oxychloride, titanium mica coated with chromium oxide, titanium mica coated with an organic dye, and pearlescent pigments based on bismuth oxychloride. They can also consist of mica particles at the surface whereof are superposed at least two successive layers of metal oxides and/or of organic dyes.
By way of example of nacres, mention can also be made of natural mica coated with titanium oxide, with iron oxide, with natural pigment or with bismuth oxychloride.
The nacres can more particularly possess a yellow, pink, red, bronze, orange, brown and/or copper color or glint.
Among the pigments that can be used according to the invention, mention can also be made of those that have an optical effect that differs from a simple conventional hue effect, i.e. a unified and stabilized effect of the kind produced by conventional dyes, such as, for example, monochromatic pigments.
For the purposes of the invention, "stabilized" means absence of an effect of variability of color with the angle of observation or in response to a temperature change. For example, this material may be selected from particles having a metallic glint, goniochromatic coloring agents, diffracting pigments, thermochromatic agents, optical brighteners, and also fibers, in particular of the interference type. Of course, these various materials can be combined so as to provide the simultaneous manifestation of two effects, or even a new effect in accordance with the invention.
According to a particular embodiment, the composition according to the invention comprises at least one non-coated pigment.
According to another particular embodiment, the composition according to the invention comprises at least one pigment coated with at least one lipophilic or hydrophobic compound. This type of pigment is particularly advantageous. Since they are treated by a hydrophobic compound, they manifest a preponderant affinity for an oily phase, which can then convey them. The coating can also comprise at least one additional non-lipophilic compound.
According to the invention, the "coating" of a pigment according to the invention generally denotes the full or partial surface treatment of the pigment by a surface agent, absorbed, adsorbed or grafted onto said pigment.
The surface-treated pigments can be prepared using chemical, electronic, mechanochemical or mechanical surface treatment techniques well known to a person skilled in the art. Commercial products can also be used.
The surface agent can be absorbed, adsorbed or grafted onto the pigments by means of solvent evaporation, chemical reaction or creation of a covalent bond. According to a variant, the surface treatment consists of a coating of the pigments. The coating can represent 0.1% to 20% by weight and particularly 0.5% to 5% by weight of the total weight of the coated pigment.
The coating can be carried out for example by adsorbing a liquid surface agent on the surface of the solid particles merely by mixing while stirring the particles and said surface agent, optionally heated, before incorporating the particles in the other ingredients of the makeup or care composition.
The coating can be carried out for example by means of a chemical reaction of a surface agent with the surface of the solid pigment particles and the creation of a covalent bond between the surface agent and the particles. This method is particularly described in the patent US 4,578,266.
The chemical surface treatment can consist of diluting the surface agent in a volatile solvent, dispersing the pigments in this mixture, and then slowly evaporating the volatile solvent, such that the surface agent is deposited on the surface of the pigments.
According to a particular embodiment of the invention, the pigments can be coated according to the invention with at least one compound selected from silicone surfactants; fluorinated surfactants; fluorosilicone surfactants; metal soaps, n-acyl amino acids or salts thereof; lecithin and its derivatives; isopropyl triisostearyl titanate; isostearyl sebacate; plant or animal natural waxes; polar synthetic waxes; fatty esters; phospholipids; and mixtures thereof.
According to a particular embodiment, the dye is an organic, synthetic, natural pigment or pigment of natural origin.
"Organic pigment" means any pigment that complies with the definition in Ullmann’s Encyclopedia in the Organic Pigment chapter. The organic pigments can in particular be selected from the compounds nitroso, nitro, azo, xanthene, quinoline, anthraquinone, phthalocyanine, metal complex type, isoindolinone, isoindoline, quinacridone, perinone, perylene, diketopyrrolopyrrole, thioindigo, dioxazine, triphenylmethane, quinophthalone.
The organic pigment(s) can be selected for example from carmine, carbon black, aniline black, melanin, azo yellow, quinacridone, phthalocyanine blue, sorghum red, the blue pigments codified in the Color Index under the references Cl 42090, 69800, 69825, 73000, 74100, 74160, the yellow pigments codified in the Color Index under the references Cl 11680, 11710, 15985, 19140, 20040, 21100, 21108, 47000, 47005, the green pigments codified in the Color Index under the references Cl 61565, 61570, 74260, the orange pigments codified the Color Index under the references Cl 11725, 15510, 45370, 71105, the red pigments codified in the Color Index under the references Cl 12085, 12120, 12370, 12420, 12490, 14700, 15525, 15580, 15620, 15630, 15800, 15850, 15865, 15880, 17200, 26100, 45380, 45410, 58000, 73360, 73915, 75470, and the pigments obtained by oxidative polymerization of indole or phenolic derivatives as described in patent FR 2 679 771.
The pigments can also be in the form of composite pigments as described in patent EP 1 184 426. These composite pigments can be composed in particular of particles including an inorganic core covered at least partially with an organic pigment and at least one binder for fixing the organic pigments to the core.
The pigment can also be a lacquer. The term lacquer means insoluble dyes adsorbed on insoluble particles, the assembly thus obtained remaining insoluble during use.
The inorganic substrates onto which the dyes are adsorbed are for example alumina, silica, borosilicate, calcium and sodium or calcium aluminum borosilicate, and aluminum.
Among the organic dyes, mention can be made of cochineal carmine. The products known under the following names can also be cited: D&C Red 21 (Cl 45 380), D&C Orange 5 (Cl 45 370), D&C Red 27 (Cl 45 410), D&C Orange 10 (Cl 45 425), D&C Red 3 (Cl 45 430), D&C Red 4 (Cl 15 510), D&C Red 33 (Cl 17 200), D&C Yellow 5 (Cl 19 140), D&C Yellow 6 (Cl 15 985), D&C Green (Cl 61 570), D&C Yellow 1 O (Cl 77 002), D&C Green 3 (Cl 42053), D&C Blue 1 (Cl 42 090). By way of examples of lacquers, mention can be made of the product known under the trade name D&C Red 7 (Cl 15 850:1).
Preferably, the cosmetic mixture obtained in step b) or c) comprises at least one active agent.
Active agent means any active agent that can be used for a topical application on the skin and/or hair.
The active agent, in particular for a topical application on the skin, can particularly be chosen from emollients, deodorant active agents, antiperspirant active agents, hydrating agents, anti-seborrheic agents, anti-acne agents, hair growth promoting agents, keratolytic and/or exfoliating agents, anti-wrinkle agents, tightening agents, anti-irritant and/or soothing agents, vitamins, UV filters, depigmenting agents, odor absorbers and mixtures thereof.
The active agent, in particular for a topical application on the hair, can in particular be chosen from coloring agents, conditioners, hair volumizing and/or gloss agents, and mixtures thereof.
The active agent can be present, in the composition, at a concentration ranging from 0.001 % to 25% by weight, with respect to the weight of the composition, preferably from 0.01% to 20% by weight.
Preferably, the cosmetic composition obtained with the method according to the invention comprises at least one dye and/or at least one active agent.
Step d)
Step d) is a step of cooling the heated oily phase obtained in b) or the composition obtained in c).
When the composition sought is anhydrous, then the heated oily phase obtained in b) is cooled.
When the composition sought is an emulsion, then the composition obtained in c) is cooled.
Step e)
Step e) is optional: it comprises remelting the cooled oily phase obtained in d) or the cooled composition obtained in d). This melting typically comprises heating the cooled oily phase obtained in d) or the cooled composition obtained in d) to a temperature greater than the melting point of the oily phase or the composition.
Preferably, this melting comprises heating the cooled oily phase obtained in d) or the cooled composition obtained in d) to a temperature greater than the highest melting point of the fat of the oily phase or the composition.
Typically, the melting comprises heating the cooled oily phase obtained in d) or the cooled composition obtained in d) to a temperature greater than or equal to 85°C.
Step f)
Step f) comprises casting the oily phase obtained at the end of step d) (after cooling) or e) (after remelting) or the stirred composition obtained at the end of step d) or e) into at least one receptacle. In any case, the stirred composition obtained at the end of step d) or e) is stirred before being cast into the receptacle.
The receptacle can be in any suitable form. It is in particular in the form of a jar, a case, a box or a casing. Preferably, the receptacle is sealed.
Preferably, the receptacle delimits a compartment containing the mixture, and it is closed by a closing element. The closing element can be in the form of a removable cap, a lid, a seal, in particular of the type comprising a body secured to the receptacle and a cap hinged on the body.
Stirring step
In the method according to the invention, stirring is applied either during the cooling step d), or at the end of the remelting step e).
Moreover, said stirring is performed until a target temperature is obtained, in the mixture, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point. The stirring applied during the cooling step d) or at the end of the remelting step e) makes it possible to obtain, in the mixture during cooling (i.e. during step d) or at the end of remelting (i.e. at the end of step e), the target temperature.
The stirring applied allows the mixture to reach a target temperature. This target temperature is less than 90% of the value of the melting point of the fat having the highest melting point. Preferably, this target temperature is less than or equal to 89% of the value of the melting point of the fat having the highest melting point, preferably less than or equal to 88%.
For example, if the cosmetic composition comprises at least one polyethylene wax having a melting point around 85°C, and this wax is the fat having the highest melting point in the composition, then the target temperature is less than 76.5°C.
Typically, this stirring step prevents the normal crystallization of the wax(es) and/or pasty fat(s) in the mixture. This step makes it possible to obtain effects, particularly sensory, hitherto not obtained in the field of solid or viscous compositions (for example such as sticks or thick creams).
According to the size and geometry of the tank used, the stirring can vary. Preferably, the stirring is constant: it is homogeneous throughout the tank, and there is no unstirred dead zone of mixture.
Preferably, according to a first embodiment, the stirring is carried out in a standard tank equipped with a stirring system.
Preferably, according to a second embodiment, the stirring is carried out in a tank, which defines a volume and has a central axis, as follows:
Preferably, the stirring is performed thanks to a stirrer having an axis of rotation and being capable of rotating about the axis of rotation in the tank about the central axis, the tank comprising a bottom and at least one lateral wall, the stirrer comprising a base and at least one blade, the base extending facing the bottom of the tank, the at least one blade having a radial edge extending facing the lateral wall, the radial distance between the radial edge of the lateral wall being constant and non-zero all along the length of the radial edge during the stirring step, the at least one blade having a height measured parallel with the axis of rotation greater than or equal to 80% of the height of the tank measured along the central axis.
Preferably, the stirrer ensures good homogeneity of the temperature of the bulk product inside the tank. The specific geometric design of the stirrer makes it possible to lessen the insufficient mixing of standard stirrers used in tanks. Thus, the temperature of the bulk product is homogeneous regardless of the point in the tank, and therefore also the bulk product crystallization state.
Preferably, the radial distance between the radial edge and the lateral wall is less than or equal to 3 cm, preferably less than or equal to 2 cm, preferably less than or equal to 1 cm.
Preferably, the or each blade has a helix shape, the helix having a helix angle measured with respect to the direction of the angle of rotation, the helix angle being preferably between 20° and 60°, more particularly between 20° and 30°.
Preferably, the or each blade has a width measured along the radial direction with respect to the axis of rotation between 10% and 20% of the width of the tank measured perpendicularly to the central axis. Preferably, the base and the bottom are spaced apart, at any point of the base, by a dimension less than or equal to 40mm, preferably between 5mm and 15mm.
Preferably, the base comprises a plurality of radial arms, each radial arm having a radial scraping surface. Preferably, each radial arm has a height measured parallel with the axis of rotation greater than or equal to 10% of the height of the tank measured along the central axis. Preferably, each arm has a height measured parallel with the axis of rotation greater than twice its thickness measured perpendicularly to the radial scraping surface.
In the method according to the invention, the stirring is applied either during the cooling step d), or at the end of the remelting step e). In any case, preferably, it is stopped before reaching the solidification point of the mixture obtained in step d) or e) (first preferred embodiment); or it is performed at a temperature less by 5°C or less than the solidification point of the fats (second preferred embodiment); or it is performed at a temperature less by more than 5°C than the solidification point of the fats (third preferred embodiment).
Preferably, according to a first embodiment, the stirring is stopped before reaching the solidification point of the mixture of step d) or e).
The solidification point of the mixture of step d) or e) is different from the melting point of the wax(es) and/or pasty fat(s) used to make the oily phase of step a). This solidification point can be determined using a differential scanning calorimeter (DSC), for example the calorimeter sold under the trade name "DSC Q2000" by TA Instruments:
The solidification point of the mixture of step d) is determined as follows: a sample of mixture obtained in b) or in c) is cooled in step d), and during the cooling of this sample, the crystallization temperature interval is measured, i.e. said interval being defined by a crystallization start temperature T 1 and a crystallization end temperature T2, where T1>T2. The solidification point of the oily phase or the composition of step d) is included in the interval [T2; T1 ], and it is generally close to the value of T1. patesThe solidification point of the mixture of step e) is determined as follows: a sample of oily phase or of composition remelted in step e) is cooled, and during the cooling of this sample, the crystallization temperature interval is measured, i.e. said interval being defined by a crystallization start temperature T’1 and a crystallization end temperature T’2, where T’1 >T’2. The solidification point of the oily phase or the composition of step r) is included in the interval [T’2; T’1], and it is generally close to the value of T’1 .
The target temperature, which is less than 90% of the value of the melting point of the fat having the highest melting point, is preferably included in the interval [T2; T1] or [T’2; T’1], Indeed, over this range, the oily phase of the composition of step d) or step e) is homogeneous at this temperature. Taking the example cited hereinabove, if the cosmetic composition comprises at least one polyethylene wax having a melting point around 85°C, and this wax is the fat having the highest melting point in the composition, then the target temperature is less than 76.5°C, and preferably the target temperature is between 70 and 75°C (i.e. interval [T2; T 1] or [T’2; T’1],
Thus, according to a first embodiment, the stirring is stopped before reaching the solidification point of the oily phase or the composition obtained in step d) or e).
Preferably, according to a second embodiment, the stirring is performed at a temperature less by 5°C or less, preferably by 4°C or less, preferably by 3°C or less, preferably by 2°C or less than the solidification point of the fats. Preferably, the stirring is performed at a temperature less by 2°C to 3°C than the solidification point of the fats.
The solidification point of the fats corresponds to the fat(s) used to make the oily phase of step a) solidify.
Preferably, according to a third embodiment, the stirring is performed at a temperature less by more than 5°C than the solidification point of the fat(s).
The solidification point of the fats corresponds to the melting point of the mixture of fats used to make the oily phase of step a).
Preferably, according to this third embodiment, the stirring is performed at ambient temperature (20-25°C).
Indeed, before casting (step f), if the temperature of the cosmetic composition preferably the lipstick, in bulk form decreases to a value close to the solidification point of the oily phase or the composition of step d) or e) or the solidification point of the fat, initial crystal formation occurs. The stirring applied during the formation of the crystalline structure breaks the lattice in formation. It is preferable to interrupt stirring just before the solidification point, otherwise a paste may be formed instead of a solid lattice.
The cosmetic composition obtained, preferably the lipstick, thus has a lower hardness on account of impeding the formation of the crystalline structure up to the casting temperature. Once the cosmetic composition has been cast, preferably the lipstick, the waxes having a lower solidification point than the casting temperature can function correctly and a solid and supple cosmetic composition, preferably a lipstick, is obtained. In particular, the application of a controlled stirring step during the cooling d) or at the end of the remelting step e), and before casting f), makes it possible to obtain more supple and softer lipsticks, having a hydrating effect and better comfort during application on the lips.
Without wishing to be bound by any theory, the texture and the appearance of a lipstick in bulk form develop when constant stirring is applied during cooling below the solidification point (for example below 70°C). When controlled stirring is applied below the solidification point, a paste can be obtained (from 70 to 50°C), then the consistency decreases substantially until a liquid texture is obtained (constant stirring applied up to 40 to 10°C). The application of controlled stirring while cooling the lipstick in bulk form makes it possible to obtain a wide range of textures:
1 . in solid state (when constant stirring is stopped before reaching the solidification point, which allows the waxes to solidify, giving a solid lipstick appearance): first preferred embodiment;
2. in paste form (when constant stirring is applied just below the solidification point, which allows some remaining crystals to crystallize, which gives an appearance of an intermediate firmness and a matte appearance): second preferred embodiment;
3. a liquid/fluid appearance (when constant stirring is applied well below the solidification point, completely preventing crystallization of the solid, giving a fluid appearance with a very low firmness and a gloss appearance): third preferred embodiment.
The invention also relates to a cosmetic composition obtained directly with a preparation method according to the invention.
The examples hereinafter are given by way of illustration and are not intended to restrict this invention. Unless specified otherwise, the percentages are percentages by weight with respect to the weight of the composition (% w/w).
Example 1 of lipstick according to the invention
The solid invert emulsion composition of example 1 according to the invention is obtained according to the following protocol:
1. Preparation of the hot oily phase (90°C): phases A1 , A2, B, hydrogenated polyisobutene and silica are mixed. Regalite, silicone resin and isohexadecane are then added (steps a) and b) of the method according invention), the whole is allowed to cool to 85°C,
2. Preparation of the hot aqueous phase (85°C): phases F and F1 are mixed,
3. Emulsification (intake of aqueous phase into oily phase) at 85°C for 20 minutes (step c) of the method),
4. Introduction of a portion of the pigments (phase D1), homogenization, then addition of the other pigments and fillers,
5. Introduction of isododecane,
6. Homogenization for 5min, then discharge into buckets and cooling (solidification to ambient temperature; step d) of the method):
Steps 1 to 6 hereinabove of manufacturing a composition according to the invention are carried out in a 30L KRIEGER MMD tank, equipped with a blade (rotating at 50 rpm), a scraper (rotating at 35 rpm) and an impeller, but also with a double jacket for thermal control and vacuum and pressure management, then the composition is discharged into buckets or containers for cooling at ambient temperature.
The content of these buckets is transferred to a tank equipped with a stirrer according to the invention (the tank does not contain an impeller or a scraper).
7. Remelting and casting (mold filling):
In this tank equipped with a stirrer according to the invention, the composition is heated to a temperature greater than or equal to the highest melting point of the waxes (in this case 85°C due to the presence of polyethylene wax) (remelting step e) of the method), then, to pre-crystallize the waxes, the temperature is lowered again to a target temperature of 70-75°C, thus creating a higher viscosity of the mixture which is stirred by the stirrer according to the invention (stirring applied according to the invention at the end of the remelting step e)).
Once the temperature of the composition in the tank is stable, the composition is cast into molds (step f) of the method) for forming lipsticks, which have the feature of being softer and more melting than if the latter had been cast as usual at 85°C (without this cooling step); the whole is allowed to cool at ambient temperature.
The solidification point for this composition (solidification of the mixture obtained in d) or e)) is around 68°C.
The stirring is stopped around 70-75°C.
[Table 1]
Figure imgf000037_0001
When the stirring is applied to a low temperature (stirring performed at a temperature less by more than 5°C than the solidification point of the fats, i.e. third preferred embodiment), the crystalline lattice cannot establish correctly. In this case, the hardness obtained is dependent on the waxes which can crystallize further under the casting temperature. In the specific case of the formula hereinabove, polyethylene wax has the highest drop point (83-92°C). Therefore, this wax may not be completely crystallized when the stirring is applied to a casting temperature less than 80°C, which results in lower crystalline lattice and therefore hardness formation.
Example 2 of preparing another composition according to the invention
A hair conditioner composition in cetearyl alcohol-based paste form is prepared with the method of the invention. Cetearyl alcohol is a mixture of cetyl and stearyl alcohols; cetyl alcohol has the highest melting point, i.e. around 50°C. The ingredients of the lipophilic phase are therefore mixed and heated to over 50°C (steps a) and b)).
The ingredients are mixed and then cooled (step d), and stirring is applied at a target temperature of 30°C (stirring step of the method), before casting (step f). Stirring allows a lessening of the viscosity of the composition, and therefore novel sensory properties during withdrawal and/or application.

Claims

1. Method for preparing a cosmetic composition comprising an oily phase, comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the oily phase of step a) or into the heated oily step of step b), to obtain a cosmetic composition in emulsion form, it being understood that when step c) is present, then step b) is performed on the oily phase obtained in a) or on the composition obtained in c), d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the oily phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one receptacle.
2. Preparation method according to claim 1 , comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, c) a step of adding an aqueous phase into the oily phase of step a), to obtain a cosmetic composition in emulsion form, steps a) and c) being simultaneous, b) a step of heating the oily phase obtained in c) to a temperature greater than or equal to the melting point(s) of the fat(s), d) a step of cooling the composition obtained in c), e) optionally, a step of remelting the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the stirred composition obtained at the end of step d) or e) into at least one receptacle.
3. Preparation method according to claim 1 , comprising the following steps: a) a step of introducing into a tank an oily phase comprising at least one fat, at least partly solid at 25°C, chosen from waxes, pasty fats, and mixtures thereof, b) a step of heating the oily phase obtained in a) to a temperature greater than or equal to the melting point(s) of the fat(s), c) optionally, a step of adding an aqueous phase into the heated oily phase of step b), to obtain a cosmetic composition in emulsion form, d) a step of cooling the heated oily phase obtained in b) or the composition obtained in c), e) optionally, a step of remelting the cooled oily phase obtained in d) or the cooled composition obtained in d), wherein stirring is applied either during the cooling step d), or at the end of the remelting step e), said stirring being performed until a target temperature is obtained, in the oily phase or the composition, said target temperature being less than 90% of the value of the melting point of the fat having the highest melting point, and f) a step of casting the oily phase obtained at the end of step d) or e) or the stirred composition obtained at the end of step d) or e) into at least one receptacle.
4. Preparation method according to one of the preceding claims, wherein step a) comprises mixing in a tank at least two fats solid at 25°C, chosen from waxes, pasty fats and mixtures thereof, preferably at least two waxes.
5. Preparation method according to one of the preceding claims, wherein the waxes are chosen from ozokerite, pyropissite, raw or slack waxes, slack wax raffinates, deoiled slack wax, soft waxes, semi-refined waxes, filtered waxes, refined waxes, microcrystalline waxes, montan wax, peat wax; carnauba wax, candelilla wax, ouricuri wax, sugarcane wax, jojoba wax, Trithrinax campestris wax, raphia wax, alfalfa wax, wax extracted from the Douglas fir, sisal wax, linseed wax, cotton wax, Batavia dammar wax, cereal wax, tea wax, coffee wax, rice wax, palm wax, Japan wax, beeswax, Ghedda wax, shellac, Chinese wax, lanolin; ester waxes such as the waxes having the formula R1COOR2 wherein R1 et R2 are linear, branched or cyclic aliphatic chains of which the number of atoms varies from 10 to 50, that can contain a heteroatom in particular oxygen, and the melting point of which varies from 30 to 120°C, preferably from 30 to 100°C, preferably a C20-C40 (hydroxystearyloxy)alkyl stearate, a C20-C40 alkyl stearate, a mixture of esters of C14-C18 carboxylic acid esters and alcohols, a montanate of glycol and of butylene glycol, polyoxyethylene beeswaxes, such as PEG-6 beeswax, PEG-8 beeswax, polyoxyethylene carnauba waxes, such as PEG- 12 carnauba, optionally hydrogenated polyoxyethylene or polyoxypropylene lanolin waxes, such as PEG-30 lanolin, PEG-75 lanolin, PPG-5 lanolin wax glyceride, polyglycerol beeswaxes, in particular polyglyceryl-3 Beewax, wax-derived esters obtained from reacting plant waxes and a polyglycerol, preferably derived esters obtained from reacting a mixture of jojoba, mimosa (Acacia Decurrens) and sunflower waxes and polyglycerol-3, or the Acacia Decurrens Flower Wax, Jojoba esters, Sunflower Seed Wax and Polyglycerin-3 mixture; fatty alcohols that are solid at ambient temperature comprising from 14 to 22 carbon atoms, and more preferably from 16 to 18 carbon atoms, and in particularly stearyl alcohol, cetyl alcohol, cetostearyl alcohol, myristyl alcohol; paraffin waxes, polymethylene waxes, polyethylene waxes, waxes obtained by Fischer-Tropsch synthesis, microwaxes in particular of polyethylene and mixtures thereof.
6. Preparation method according to one of the preceding claims, wherein the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 45°C.
7. Preparation method according to one of the preceding claims, wherein the oily phase of step a) comprises at least one wax having a melting point greater than or equal to 70°C; preferably, the wax having a melting point greater than or equal to 70°C is chosen from paraffin waxes, ozokerite, polymethylene waxes and polyethylene waxes; preferably, the wax having a melting point greater than or equal to 70°C is a non-polar hydrocarbon wax, preferably a polyethylene wax, and said non-polar hydrocarbon wax represents at least 50% by weight with respect to the total weight of wax(es) of the oily phase.
8. Preparation method according to one of the preceding claims, wherein the oily phase of step a) comprises at least 0.1 % by weight, preferably at least 0.5% by weight, preferably at least 1% by weight, preferably at least 2% by weight, preferably at least 5% by weight, preferably at least 6% by weight, preferably at least 7% by weight with respect to the total weight of the composition of at least one wax, preferably the melting point of which is greater than or equal to 45°C, preferably greater than or equal to 70°C.
9. Preparation method according to one of the preceding claims, wherein the oily phase of step a) further comprises at least one oil, preferably non-volatile, preferably hydrocarbon, preferably polar or non-polar.
10. Preparation method according to one of the preceding claims, wherein the oily phase of step a) further comprises at least one hydrophobic film-forming hydrocarbon resin, and/or at least one silicone resin, and/or at least one preferably non-volatile, preferably hydrocarbon, polar or non-polar oil.
11. Preparation method according to any of the preceding claims, wherein the oily phase or the composition obtained in step b) or c) comprises at least one dye and/or at least one active agent.
12. Preparation method according to claim 11 , wherein the dye is chosen from water-soluble or liposoluble colorants, pigments, nacres, pigmentary pastes and mixtures thereof.
13. Preparation method according to claim 11 , wherein the active agent, is chosen from emollients, deodorant active agents, antiperspirant active agents, hydrating agents, anti-seborrheic agents, anti-acne agents, hair growth promoting agents, keratolytic and/or exfoliating agents, anti-wrinkle agents, tightening agents, anti-irritant and/or soothing agents, vitamins, UV filters, depigmenting agents, odor absorbers, coloring agents, conditioners, hair volumizing and/or gloss agents, and mixtures thereof.
14. Preparation method according to one of claims 11 to 13, wherein the dye is present at a concentration ranging from 0.001% to 25% by weight, with respect to the weight of the composition, preferably from 0.01 % to 20% by weight.
15. Preparation method according to one of the preceding claims, wherein step e), when it is present, comprises heating the cooled oily phase obtained in d) or the cooled composition obtained in d) to a temperature greater than the melting point of the oily phase or the composition; preferably, the remelting comprises heating the cooled oily phase obtained in d) or the cooled composition obtained in d) to a temperature greater than the highest melting point of the fat of the oily phase or the composition.
16. Preparation method according to one of the preceding claims, wherein the stirring is constant.
17. Preparation method according to one of the preceding claims, wherein the target temperature is less than or equal to 89% of the value of the melting point of the fat having the highest melting point, preferably less than or equal to 88%.
18. Preparation method according to one of the preceding claims, wherein the stirring is stopped before reaching the solidification point of the mixture of step d) or e), and the solidification point of the oily phase or the composition of step d) being determined as follows: a sample of oily phase of composition obtained in b) or in c) is cooled in step d), and during the cooling of this sample, the crystallization temperature interval is measured, i.e. said interval being defined by a crystallization start temperature T1 and a crystallization end temperature T2, where T1 >T2; the solidification point of the oily phase or the composition of step d) is included in the interval [T2; T1], and it is generally close to the value of T1; the solidification point of the oily phase or the composition of step e) being determined as follows: a sample of oily phase or of composition remelted in step e) is cooled, and during this cooling, the crystallization temperature interval is measured, i.e. said interval being defined by a crystallization start temperature T’1 and a crystallization end temperature T’2, where T’1 >T’2; the solidification point of the oily phase or the composition of step e) is included in the interval [T’2; T’1], and it is in general close to the value of T’1.
19. Preparation method according to one of claims 1 to 18, wherein the stirring is performed at a temperature less by 5°C or less, preferably by 4°C or less, preferably by 3°C or less, preferably by 2°C or less than the solidification point of the fats; preferably, the stirring is performed at a temperature less by 2°C to 3°C than the solidification point of the fats.
20. Preparation method according to one of claims 1 to 18, wherein the stirring is performed at a temperature less by more than 5°C than the solidification point of the fats; preferably, the stirring is performed at ambient temperature (20-25°C).
21. Cosmetic composition obtained directly with a preparation method according to any one of claims 1 to 20.
PCT/EP2024/086284 2023-12-15 2024-12-13 Process for preparing a cosmetic composition comprising a fatty phase Pending WO2025125600A1 (en)

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