Classifications

• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/04—Dispersions; Emulsions
  • A61K8/06—Emulsions
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/04—Dispersions; Emulsions
  • A61K8/06—Emulsions
  • A61K8/062—Oil-in-water emulsions
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
  • A61K8/04—Dispersions; Emulsions
  • A61K8/042—Gels
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
  • A61K8/37—Esters of carboxylic acids
  • A61K8/375—Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/73—Polysaccharides
  • A61K8/732—Starch; Amylose; Amylopectin; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q19/00—Preparations for care of the skin
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
  • A61Q5/00—Preparations for care of the hair
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
  • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
  • A61K2800/30—Characterized by the absence of a particular group of ingredients
  • A61K2800/33—Free of surfactant

Definitions

• the present invention relates to stable oil-in-water dispersions comprising an aqueous continuous phase and drops, in particular macroscopic, of a dispersed fatty phase comprising at least one lipophilic gelling agent. It also relates to compositions, in particular cosmetic compositions, containing said dispersions as well as their uses in the cosmetic field.
• dispersions in the form of direct emulsion such as for example described in US 2004/137020 and EP 2 189 081.
• the dispersed phases of these dispersions are not in the form of macroscopic drops and are endowed with 'a hardness such that the sensoriality and / or the comfort on application are not satisfactory, moreover in the presence of phases dispersed in the form of macroscopic drops.
• amodimethicone can sometimes lead to problems of compatibility with other raw materials and / or phenomena of aggregation of the drops between them, of adhesion of the drops to the packaging and / or. drop sphericity defects, which for obvious reasons is not desirable. Indeed, such drawbacks can impact the stability of the dispersion and / or the homogeneity of delivery of the different constituent phases of the dispersion and / or the visual and aesthetic rendering of the dispersion, or even its sensoriality on application to the skin. , and these drawbacks are exacerbated the larger the diameter of the drops increases. Without wishing to be bound by any theory, the Applicant believes that the aforementioned drop sphericity defect may be related to a decrease in the elasticity of the dispersed fatty phase due to the presence of amodimethicone.
• the present invention relates to an oil-in-water dispersion comprising, or even containing, a dispersed phase comprising drops and a continuous aqueous phase, preferably in gel form, in which the drops comprise a fatty phase comprising at least one agent.
• lipophilic gelling agent and optionally at least one oil in which:
• x a hardness (x) of between 2 and 14 N, preferably between 2.5 and 12 N, and better still between 3 and 9 N, and very particularly between 4 and 6 N;
• the fatty phase of a dispersion according to the invention also has a cohesion (z) less than or equal to 40, preferably less than or equal to 35, and better still less than or equal to 30.
• a dispersion according to the invention also allows more freedom as regards the compounds and / or their contents, in particular of active ingredients, which can be encapsulated.
• stable or “kinetic stability” is understood to denote, within the meaning of the present invention, at room temperature and atmospheric pressure, the absence of creaming or sedimentation of the drops of phase dispersed in the continuous phase, the absence of opacification of the continuous aqueous phase, the absence of aggregation of the drops between them, and in particular the absence of coalescence or Oswald ripening of the drops between them, the absence of adhesion of the drops to the packaging and the absence of material leakage from the dispersed phase to the continuous phase, or vice versa, for a dispersion according to the invention over a period of time greater than or equal to 1 month, preferably greater than or equal to 3 months, and better still greater than or equal at 6 months.
• the term “gelling agent” is intended to denote an agent making it possible to increase the viscosity of the phase devoid of said gelling agent, and preferably to achieve a final viscosity of the phase thus gelled of greater than 20. 000 mPa.s, preferably greater than 50,000 mPa.s, better still greater than 100,000 mPa.s, and most particularly greater than 200,000 mPa.s.
• a dispersion in a dispersion according to the invention:
• a dispersion according to the invention does not include glyceryl trioctanoate, glycerol tricaprylate / caprate, and their mixture. According to one embodiment, a dispersion according to the invention does not include:
• the drops advantageously have an apparent monodispersity (ie they are perceived by the eye as spheres identical in diameter).
• the drops are advantageously substantially spherical.
• R 2 and R 3 independently of each other, represent OH or CH 3 ;
• R 4 represents a -CH 2 - group or a -X-NH- group in which X is a divalent C3 or C4 alkylene radical;
• - y is an integer between 1 and 1000, in particular between 2 and 1000, preferably between 4 and 100, and better still between 5 and 20;
• the sample is then subjected to the following protocol by being first of all brought to temperature at 20 ° C, then subjected to a first temperature rise ranging from 20 ° C to 130. ° C, at the heating rate of 5 ° C / minute, then is cooled from 130 ° C to -80 ° C at a cooling rate of 5 ° C / minute and finally subjected to a second temperature rise ranging from - 80 ° C to 130 ° C at a heating rate of 5 ° C / minute.
• the melting point of the compound is the value of the temperature corresponding to the top of the peak of the curve representing the variation of the difference in power absorbed as a function of the temperature.
• the end of melting temperature corresponds to the temperature at which 95% of the sample has melted.
• the cohesiveness corresponds to the way in which the tested product resists the second deformation, relative to the way which he behaved during the first deformation.
• Cohesion corresponds to the surface of the second curve (Area. 2) on the surface of the first curve (Area 1) (ie Area. 2 / Area. 1).
• cohesion represents the forces within the tested sample.
• strong bonds within the gel will allow a completely reversible deformation during the first compression which will induce a force A2 identical to the force A1, and therefore 100% cohesion. Consequently, the stronger the cohesion, the more deformable the gel.
• the weaker the cohesion the more brittle the gel (weak bonds, no resistance to stress).
• the sample to be tested is placed in a mold 40 mm in diameter filled to 75% of its height.
• a lipophilic gelling agent is a thermosensitive gelling agent, ie which reacts with heat, and in particular is a solid gelling agent at room temperature and liquid at a temperature above 50 ° C, preferably above 60 ° C, and better above 70 ° C.
• a heat-sensitive lipophilic gelling agent according to the invention has a melting point of between 50 ° C and 130 ° C, and preferably between 60 ° C and 120 ° C.
• the lipophilic gelling agent according to the invention can be chosen from organic or inorganic, polymeric or molecular lipophilic gelling agents; fatty substances which are solid at ambient temperature and pressure; and their mixtures.
• Silicas thus treated are called “Silica dimethyl silylate” according to the CTFA (8th edition, 2000). They are for example marketed under the references Aerosil R972 ⁇ , and Aerosil R974 ⁇ by the company DEGUSSA, CAB-O-SIL TS-610 ⁇ and CAB-O-SIL TS-720 ⁇ by the company CABOT.
• Polymeric organic lipophilic gelling agents are, for example, partially or totally crosslinked elastomeric organopolysiloxanes, of three-dimensional structure, such as those sold under the names KSG6 ⁇ , KSG16 ⁇ and KSG18 ⁇ by the company Shin-ETSU, Trefil E-505CO and Trefil E- 506C ⁇ by the company DOW-CORNING, de Gransil SR-CYC ⁇ , SR DMF10 ⁇ , SR-DC556 ⁇ , SR 5CYC gel ⁇ , SR DMF 10 gel ⁇ and SR DC 556 gel ⁇ by the company GRANT INDUSTRIES, from SF 1204 ⁇ and from JK 113 ⁇ by the GENERAL ELECTRIC company; ethylcellulose such as that sold under the name Ethocel6 by the company DOW CFIEMICAL; galactommanans comprising from one to six, and in particular from two to four, hydroxyl groups per dose, substituted with a saturated or unsaturated alkyl chain, such as guar gum
• the gelling agents which can be used according to the invention can be chosen from the group consisting of polyacrylates; esters of sugar / polysaccharide and fatty acid (s), in particular esters of dextrin and fatty acid (s), esters of glycerol and fatty acid (s) or esters of inulin and 'Fatty acids ; polyamides, and mixtures thereof.
• lipophilic gelling agents which can be used in the present invention, mention may also be made of dextrin and fatty acid esters, such as dextrin palmitates.
• the ester of dextrin and of fatty acid (s) is a mono- or poly-ester of dextrin and of at least one fatty acid corresponding to the following formula (II): in which: n is an integer ranging from 2 to 200, preferably ranging from 20 to 150, and in particular ranging from 25 to 50, the radicals R4, R5 and R6, which are identical or different, are chosen from hydrogen or an acyl group -CORa in which the radical Ra represents a hydrocarbon radical, linear or branched, saturated or unsaturated, having from 5 to 50, preferably from 5 to 25 carbon atoms, with the proviso that at least one of said radicals R4, R5 or R6 is different from hydrogen.
• formula (II) in which: n is an integer ranging from 2 to 200, preferably ranging from 20 to 150, and in particular ranging from 25 to 50, the radicals R4, R5 and R6, which are identical or different, are chosen from hydrogen or an acyl group -CORa in
• esters of dextrin and of fatty acid (s) there may be mentioned, for example, dextrin palmitates, dextrin myristates, dextrin palmitates / ethylhexanoates, and mixtures thereof. Mention may in particular be made of the esters of dextrin and of fatty acid (s) marketed under the names Rheopearl® KL2 or D2 (INCI name: dextrin palmitate), Rheopearl® TT2 (INCI name: dextrin palmitate ethylhexanoate), and Rheopearl® MKL2 ( INCI name: dextrin myristate) by the company Miyoshi Europe.
• the polyacrylates resulting from the polymerization of C10-C30 alkyl acrylate (s), preferably of C14- alkyl acrylate (s). C24, and even more preferably of C18-C22 alkyl acrylate (s).
• the polyacrylates are polymers of acrylic acid esterified with a fatty alcohol whose saturated carbon chain comprises from 10 to 30 carbon atoms, preferably from 14 to 24 carbon atoms, or a mixture of said fatty alcohols.
• the fatty alcohol comprises 18 carbon atoms or 22 carbon atoms.
• the polyacrylates mention may more particularly be made of stearyl polyacrylate and behenyl polyacrylate.
• the gelling agent is stearyl polyacrylate or behenyl polyacrylate.
• Interlimer® INCCI name: Poly C10-C30 alkyl acrylate
• said ester of glycerol and fatty acid (s) can be used alone or as a mixture.
• it may be an ester of glycerol and a fatty acid or an ester of glycerol and a mixture of fatty acids.
• the fatty acid is selected from the group consisting of behenic acid, isooctadecanoic acid, stearic acid, eicosanoic acid, and mixtures thereof.
• esters of glycerol and of fatty acid (s) marketed under the names Nomcort HK-G (INCI name: Glyceryl behenate / eicosadioate) and Nomcort SG (INCI name: Glyceryl tribehenate, isostearate, eicosadioate), by the Nisshin Oillio company.
• the fatty substance which is solid at ambient temperature and pressure is in particular chosen from the group consisting of waxes, pasty fatty substances, butters and their mixtures.
• the term “wax” is understood to mean a lipophilic compound, solid at room temperature (25 ° C), with a reversible solid / liquid change of state, having a melting point greater than or equal to 50 ° C. up to 120 ° C.
• waxes obtained by catalytic hydrogenation of animal or vegetable oils having fatty chains, linear or branched, C8-C32.
• animal or vegetable oils having fatty chains linear or branched, C8-C32.
• hydrogenated jojoba oil hydrogenated sunflower oil, hydrogenated castor oil, hydrogenated coconut oil and hydrogenated lanolin oil, di- (tetrastearate) trimethylol-1,1,1 propane) sold under the name "HEST 2T-4S" by the company HETERENE, tetrabhenate of di- (trimethylol-1, 1, 1 propane) sold under the name HEST 2T-4B by the company HETERENE.
• waxes obtained by transesterification and hydrogenation of vegetable oils such as castor or olive oil, such as the waxes sold under the names of Phytowax ricin 16L64® and 22L73® and Phytowax Olive 18L57 by the company SOPHIM.
• Such waxes are described in application FR2792190.
• silicone waxes which can advantageously be substituted polysiloxanes, preferably with a low melting point.
• the silicone waxes which can be used can also be alkyl or alkoxydimethicones such as the following commercial products: Abilwax 2428, 2434 and 2440 (GOLDSCHMIDT), or VP 1622 and VP 1621 (WACKER), as well as (C20-C60) alkyldimethicones, in in particular (C30-C45) alkyldimethicones such as the silicone wax sold under the name SF-1642 by the company GE-Bayer Silicones. It is also possible to use hydrocarbon waxes modified with silicone or fluorinated groups, such as, for example: siliconyl candelilla, siliconyl beeswax and Fluorobeeswax from Koster Keunen.
• the waxes can also be chosen from fluorinated waxes.
• the term “butter” (also called “pasty fatty substance”) means a lipophilic fatty compound with a reversible solid / liquid change of state and comprising, at a temperature of 25 ° C., a liquid fraction and a fraction. solid, and at atmospheric pressure (760 mm Hg).
• the starting melting point of the pasty compound can be less than 25 ° C.
• the liquid fraction of the pasty compound measured at 25 ° C. can represent from 9% to 97% by weight of the compound. This fraction which is liquid at 25 ° C. preferably represents between 15% and 85%, more preferably between 40 and 85% by weight.
• the butter (s) have an end-of-melting temperature of less than 60 ° C.
• the butter (s) have a hardness less than or equal to 6 MPa.
• the butters or pasty fatty substances exhibit in the solid state an anisotropic crystalline organization, visible by X-ray observations.
• the melting temperature corresponds to the temperature of the most endothermic peak observed in thermal analysis (DSC) as described in standard ISO 11357-3; 1999.
• the melting point of a paste or a wax can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name “DSC Q2000” by the company TA Instruments .
• the enthalpy of fusion of the butter is equal to the integral of the whole of the melting curve obtained using the calorimeter involved, with a temperature rise of 5 ° C or 10 ° C per minute, according to the standard ISO 11357-3: 1999.
• the enthalpy of fusion of butter is the amount 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 25 ° C is the quantity of energy absorbed by the sample to change from the solid state to the state that it presents at 25 ° C consisting of a liquid fraction and a solid fraction.
• the liquid fraction of the butter measured at 32 ° C. preferably represents from 30% to 100% by weight of the compound, preferably from 50% to 100%, more preferably from 60% to 100% by weight of the compound.
• the temperature of the end of the melting range of the pasty compound is less than or equal to 32 ° C.
• the liquid fraction of butter measured at 32 ° C is equal to the ratio of the enthalpy of fusion consumed at 32 ° C to the enthalpy of fusion of the butter.
• the enthalpy of fusion consumed at 32 ° C is calculated in the same way as the enthalpy of fusion consumed at 23 ° C.
• sample preparation and measurement protocols are as described in WO2017046305.
• the pasty fatty substance or butter can be chosen from synthetic compounds and compounds of plant origin.
• a pasty fatty substance can be obtained by synthesis from starting products of plant origin.
• the particular butter (s) are of plant origin such as those described in Ullmann's Encyclopedia of Industrial Chemistry (“Fats and Fatty Oils”, A. Thomas, published on 06/15/2000, D01 : 10.1002 / 14356007.a10_173, point 13.2.2.2. Shea Butter, Borneo Tallow, and Related Fats (Vegetable Butters)).
• the lipophilic gelling agent is chosen from Castor Oil / IPDI Copolymer (and) Caprylic / Capric Triglyceride, in particular sold under the name Estogel M by PolymerExpert, Caprylic / Capric Triglycéride (and) Polyurethane- 79, in particular marketed under the name OILKEMIA TM 5S polymer by the company Lubrizol, Trihydroxystearin, in particular marketed under the name THIXCIN® R by the company Elementis Specialties, and their mixtures, and better still Castor Oil / IPDI Copolymer (and) Caprylic / Capric Triglyceride.
• a dispersion according to the invention in particular the fatty phase, does not comprise an elastomer gel comprising at least a dimethicone, in particular as marketed by NuSil Technology under the name CareSil TM CXG-1104 (INCI: Dimethicone (and) Dimethicone / Vinyl Dimethicone Crosspolymer).
• the dispersed fatty phase can comprise at least one oil.
• oils according to the invention there may be mentioned, for example: - hydrocarbon-based oils of plant origin, as described below;
• hydrocarbon oils of animal origin such as perhydrosqualene and squalane
• esters and ethers in particular of fatty acids, such as oils of formulas R1COOR2 and R1OR2 in which R1 represents the residue of a Cs to C29 fatty acid, and R2 represents a hydrocarbon chain, branched or not, C3 to C30, such as, for example, Purcellin oil, isononyl isononanoate, isodecyl neopentanoate, isostearyl neopentanoate, isopropyl myristate, octyldodecyl myristate, 2-ethylhexyl palmitate, 2-octyl-dodecyl stearate, 2-octyl-dodecyl erucate, isostearyl isostearate; hydroxylated esters such as isostearyl lactate, octylhydroxystearate, octyldodecyl hydroxystearate
• silicone oils such as for example polymethylsiloxanes (PDMS) volatile or not with a linear or cyclic silicone chain, liquid or pasty at room temperature, in particular cyclopolydimethylsiloxanes (cyclomethicones) such as cyclohexasiloxane and cyclopentasiloxane; polydimethylsiloxanes (or dimethicones) comprising alkyl, alkoxy or phenyl groups, pendant or at the end of the silicone chain, groups having from 2 to 24 carbon atoms; phenylated silicones such as phenyltrimethicones, phenyldimethicones, phenyltrimethylsiloxydiphenylsiloxanes, diphenyl-dimethicones, diphenylmethyldiphenyl trisiloxanes, 2-phenylethyltrimethyl-siloxysilicates, and polymethylsiloxysilicates;
• PDMS polymethylsilox
• - fatty alcohols having 8 to 26 carbon atoms such as cetyl alcohol, stearyl alcohol and their mixture (cetylstearyl alcohol), or octyldodecanol;
• the fatty phase of a dispersion according to the invention comprises at least one vegetable oil.
• hydrocarbon oil (s) of vegetable origin mention may be made of triglycerides of caprylic and capric acids, triglycerides of caprylic and capric acids (also known under the name of "MCT oil"), myristic and stearic (INCI name: Caprylic / capric / myristic / stearic Triglyceride), triethylhexanoine, Limnanthes Alba seed oil (INCI name: Limnanthes Alba (Meadowfoam) Seed Oil), macadamia nut oil ( INCI name: Macadamia Ternifolia Seed Oil), rosehip oil Rosa Canina (INCI name: Rosa Canina Fruit Oil), soybean oil (INCI name: Glycine Soja (Soybean) Oil), seed oil sunflower (INCI name: Helianthus Annuus (Sunflower) Seed Oil), tribhenin (INCI name: tribehenin), triisostearin (INCI name: triisostearin),
• Sinensis Seed Oil sea buckthorn oil (INCI name: Hippophae Rhamnoides Oil), Camellia Kissi seed oil (INCI name: Camellia Kissi Seed Oil), Moringa seed oil (INCI name: Moringa Pterygosperma Seed Oil), canola oil (INCI name: Canola Oil), tea seed oil (INCI name: Camellia Oleifera Seed Oil), carrot seed oil (INCI name: Daucus Carota Sativa Seed Oil), triheptanoine (INCI name: Triheptanoin), vanilla oil (INCI name: Vanilla Planifolia Fruit Oil), canola oil glycerides and phytosterols (INCI name: Phytosteryl Canola Glycerides), blackcurrant seed (INCI name: Ribes Nigrum (Black Currant) Seed Oil), karanja seed oil (INCI name: Pongamia Glabra Seed Oil), annatto oil (INCI name: Roucou (Bixa orellana) Oil)
• the oil is chosen from vegetable oils rich in polyunsaturated fatty acids.
• unsaturated fatty acid means a fatty acid comprising at least one double bond.
• unsaturated fatty acids comprising from 18 to 22 carbon atoms, in particular polyunsaturated fatty acids, in particular w-3 and w-6 fatty acids, are used as the oil.
• the fatty phase comprises at least one oil having a refractive index close to that of the aqueous continuous phase, namely an oil having a refractive index, at room temperature and atmospheric pressure, preferably between 1, 2 and 1. , 6, preferably between 1, 25 and 1, 5, in particular between 1, 3 and 1, 4.
• an oil having a refractive index close to that of the aqueous continuous phase, namely an oil having a refractive index, at room temperature and atmospheric pressure, preferably between 1, 2 and 1. , 6, preferably between 1, 25 and 1, 5, in particular between 1, 3 and 1, 4.
• the oil having a refractive index of between 1, 2 and 1, 6 is a silicone oil, in particular a phenylated silicone oil.
• the fatty phase of a dispersion according to the invention comprises at least one, or even at least two, oil (s), preferably chosen from one or more hydrocarbon oil (s) of vegetable origin. , and preferably chosen from limnanthes seed oil Limnanthes Alba (INCI name: Limnanthes Alba (Meadowfoam) Seed Oil, triglycerides of caprylic and capric acids, and their mixture.
• the oil may be present in the fatty phase of a dispersion according to the invention is not a silicone oil or a fluorinated oil.
• a dispersion according to the invention does not comprise polydimethylsiloxane (PDMS or dimethicone) or a derivative thereof, and preferably does not include silicone oil, and in particular octamethylcyclotetrasiloxane (or Cyclotetrasiloxane or D4), decamethylcyclopentasiloxane (or Cyclopentasiloxane or D5) and Cyclohexasiloxane (or D6).
• PDMS or dimethicone polydimethylsiloxane
• D4 octamethylcyclotetrasiloxane
• decamethylcyclopentasiloxane or Cyclopentasiloxane or D5
• Cyclohexasiloxane or D6
• a dispersion according to the invention may comprise between 10% and 99.5%, preferably between 20% and 90%, better still between 30% and 85%, and in particular between 50% and 80%, by weight of oil ( s) relative to the total weight of the fatty phase.
• a dispersion according to the invention is also advantageous in that its kinetic stability allows high percentages of dispersed fatty phase.
• a dispersion according to the invention may comprise from 1% to 60%, in particular from 5% to 50%, preferably from 10% to 40%, and better still from 15% to 30%, by weight of dispersed fatty phase. relative to the total weight of the dispersion. Additional compound (s)
• a dispersion according to the invention in particular the continuous aqueous phase and / or the dispersed fatty phase, may / may further comprise at least one additional compound other than the lipophilic gelling agent and the aforementioned oils.
• a dispersion according to the invention in particular the continuous aqueous phase and / or the dispersed fatty phase, can / can thus further comprise powders; charges ; Glitter ; coloring agents, in particular chosen from coloring agents which are water-soluble or not, liposoluble or not, organic or inorganic, materials with an optical effect, liquid crystals, and mixtures thereof; particulate agents insoluble in the fatty phase; preservatives; humectants; perfuming agents, in particular as defined in WO2019002308; stabilizers; chelators; emollients; modifiers chosen from gelling / texture agents, viscosity different from the base and lipophilic gelling agents mentioned above, pH, osmotic strength and / or refr
• the term "filler” means colorless or white particles, solid of all shapes, which are in an insoluble form and dispersed in the medium of the composition. Mineral or organic in nature, they make it possible to impart body or rigidity and / or softness, and uniformity to the deposit, in particular in a makeup context, and improved stability with regard to exudation and properties. non-migration after application and / or mattness and / or coverage.
• a dispersion according to the invention in particular the continuous aqueous phase and / or the dispersed fatty phase, may / may further comprise at least one biological / cosmetic active agent, in particular chosen from moisturizing agents, agents. healing agents, depigmenting agents, UV filters, desquamating agents, antioxidants, active agents stimulating the synthesis of dermal and / or epidermal macromoleculars, dermodecontracting agents, antiperspirants, soothing agents and / or anti-aging agents. -age, and their mixtures.
• active agents are in particular described in FR1558849.
• hydrophilic gelling agents there may be mentioned:
• - natural gelling agents in particular chosen from algae extracts, plant exudates, seed extracts, microorganism exudates, such as alkasealan marketed by the company Hakuto (INCI: Alcaligenes Polysaccharides), and other agents natural, in particular hyaluronic acid,
• - semi-synthetic gelling agents in particular chosen from cellulose derivatives and modified starches,
• gelling agents in particular chosen from polyethylene glycols (marketed under the name Carbowax), clays, silicas such as those marketed under the names Aerosil® 90/130/150/200/300/380), glycerin, and
• the term “associative polymer” means any amphiphilic polymer comprising in its structure at least one fatty chain and at least one hydrophilic portion; the associative polymers in accordance with the present invention can be anionic, cationic, nonionic or amphoteric; these are in particular those described in FR2999921. Preferably, they are amphiphilic and anionic associative polymers and amphiphilic and nonionic associative polymers as described below.
• hydrophilic gelling agents are described in more detail in FR3041251.
• the dispersion according to the invention comprises from 0.0001% to 20%, preferably from 0.001% to 15%, in particular from 0.01% to 10%, and better still from 0.1% to 5% by weight of hydrophilic gelling agent (s) relative to the total weight of the aqueous continuous phase.
• hydrophilic gelling agent (s) refer to hydrophilic gelling agent (s) only present in the continuous aqueous phase.
• the dispersion according to the invention comprises from 0.0001% to 20%, preferably from 0.001% to 15%, and preferably from 0.01% to 10%, by weight of additional compound (s) (s) relative to the total weight of said dispersion.
• additional compound (s) s
• a person skilled in the art will take care to choose the optional additional compound (s) and / or their quantity in such a way that the advantageous properties of the dispersion according to the invention, in particular its kinetic stability and, having regard to in the dispersed fatty phase, its melting point and its physicochemical properties x and y, or even z, mentioned above, are not or not substantially altered by the addition envisaged.
• a dispersion according to the invention can be prepared by various methods.
• an aqueous solution and a fatty solution are prepared separately. It is the stirring of the fatty phase in the aqueous phase that creates the direct emulsion.
• the viscosity of the aqueous phase and the shear force applied to the mixture are the two main parameters which influence the size and the monodispersity of the drops of the emulsion.
• a person skilled in the art will know how to adjust the parameters of the non-microfluidic process in order to achieve the dispersion according to the invention, and in particular to satisfy the desired drop diameter criterion.
• the dispersions according to the invention can also be prepared according to a microfluidic process, in particular as described in applications WO2012 / 120043 or WO2019 / 145424.
• the microfluidic nozzle (s) used can have a configuration according to the T geometry, in co-flow (or co-currents), or flow-focusing.
• the drops obtained by this microfluidic process advantageously have a uniform size distribution.
• the dispersions of the invention consist of a population of monodisperse drops, in particular such that they have an average diameter D of from 100 ⁇ m to 3,000 ⁇ m, in particular from 500 ⁇ m to 3,000 ⁇ m and a coefficient variation Cv less than 10%, or even less than 3%.
• the term "monodisperse drops” is understood to mean the fact that the population of drops of the dispersion according to the invention has a uniform size distribution. Monodispersed drops exhibit good monodispersity. Conversely, drops with poor monodispersity are said to be “polydisperse”.
• the mean diameter D of the drops is for example measured by analyzing a photograph of a batch consisting of N drops, by image processing software (Image J).
• Image J image processing software
• the diameter is measured in pixels, then reported in ⁇ m, as a function of the size of the container containing the drops of the dispersion.
• the value of N is chosen to be greater than or equal to 30, so that this analysis reflects in a statistically significant manner the distribution of diameters of the drops of said emulsion.
• N is advantageously greater than or equal to 100, in particular in the case where the dispersion is polydispersed.
• the standard deviation s of a dispersion reflects the distribution of the diameters Di of the drops of i dispersion around the mean diameter D.
• the coefficient of variation can be calculated:
• This parameter reflects the distribution of the diameters of the drops as a function of their average diameter.
• the coefficient of variation Cv of the diameters of the drops according to this embodiment of the invention is less than 10%, preferably less than 5%, or even less than 3%.
• monodispersity can be demonstrated by placing a dispersion sample in a flask with constant circular section. A gentle agitation by rotation of a quarter of a turn for half a second around the axis of symmetry crossing the bottle, followed by a rest of half a second is carried out, before repeating the operation in the opposite direction, and this four times in a row.
• the drops of the dispersed phase organize in a crystalline form when they are monodispersed. Thus, they present a stack according to a pattern repeating itself following in the three dimensions. It is then possible to observe a regular stacking which indicates good monodispersity, an irregular stacking reflecting the polydispersity of the dispersion.
• the presence, in the dispersed fatty phase, of lipophilic gelling agent (s), or even in the aqueous continuous phase, of hydrophilic gelling agent (s), may require adjustments. at the level of the process for preparing a dispersion according to the invention.
• the process for preparing such a dispersion according to the invention comprises a heating step (between 50 ° C and 150 ° C, in particular between 60 ° C and 90 ° C) at least of the fatty phase before mixing / bringing said fatty phase into contact with the aqueous phase and, where appropriate, maintaining this heating (i) during stirring in the case of a “non-microfluidic” process or (ii) at the device level microfluidics in the case of a “microfluidic” process, until the desired dispersion is obtained.
• the process for preparing a dispersion of the invention comprises at least the following steps: a) heating an oily fluid F1 to a temperature between 50 ° C and 150 ° C, preferably from 60 ° C to 120 ° C, and better still from 70 ° C to 100 ° C; b) optionally heating an aqueous fluid FE to a temperature of from 50 ° C to 150 ° C, preferably from 60 ° C to 120 ° C, and better still from 70 ° C to 100 ° C; c) contacting the aqueous fluid FE and the oily fluid F1; and d) the formation of drops of fatty phase, consisting of oily fluid F1, dispersed in a continuous aqueous phase, consisting of aqueous fluid FE, in which:
• the oily fluid F1 comprises at least one lipophilic gelling agent and optionally at least one oil and has a melting point of between 50 ° C and 100 ° C, preferably between 60 ° C and 90 ° C, and at room temperature and atmospheric pressure, meets the following physicochemical criteria:
• x a hardness (x) of between 2 and 14 N, preferably between 2.5 and 12 N, better still between 3 and 9 N, and very particularly between 4 and 6 N;
• oily fluid F1 further being devoid of amodimethicone and, optionally, further comprises at least one additional compound as mentioned above;
• Steps (c) and (d) are carried out at a temperature greater than or equal to the melting point of the gelling agent (s) used.
• steps (c) and (d) are carried out with an oily fluid F1 in a form capable of emulsifying with the aqueous fluid FE, and therefore capable of ensuring the formation of drops, and in particular with a oily fluid F1 in liquid form.
• the FE fluid is initially prepared by mixing an aqueous phase intended to form the continuous phase of the dispersion with, optionally, at least one base, at least one additional compound, preservatives and / or other products.
• soluble in water such as glycerin, and very particularly at least one hydrophilic gelling agent.
• the viscosity increasing solution comprises a base, in particular an alkali hydroxide, such as sodium hydroxide.
• step c) is represented by stirring during which heating can be maintained during this stirring, allowing the desired dispersion to be obtained.
• step d) of formation of drops may comprise the formation of drops of oily fluid F1 at the outlet of a first duct opening into the aqueous fluid FE.
• the aqueous fluid FE is circulated in a second conduit, the outlet of the first conduit opening into the second conduit, advantageously coaxially with the local axis of the second conduit.
• the present invention also relates to a dispersion that can be obtained by a process such as those described above.
• a dispersion according to the invention can be used directly, at the end of the aforementioned preparation processes, as a composition, in particular a cosmetic.
• the dispersion according to the invention when prepared by means of a microfluidic process as described above, can also be used as a composition, in particular cosmetic, after separation of the drops and redispersion of the latter in an appropriate second phase.
• the invention also relates to the use of a dispersion according to the invention for the preparation of a composition, in particular cosmetic, pharmaceutical, in nutrition or in food industry, preferably a cosmetic composition and in particular a care and / or makeup composition for a keratin material, in particular the skin.
• a composition in particular cosmetic, pharmaceutical, in nutrition or in food industry, preferably a cosmetic composition and in particular a care and / or makeup composition for a keratin material, in particular the skin.
• the present invention thus also relates to a composition, in particular cosmetic, in particular for caring for and / or making up a keratin material, in particular the skin and / or the hair, and more particularly the skin, comprising at least one dispersion according to FIG. invention, optionally in combination with at least one physiologically acceptable medium.
• the dispersions or compositions according to the invention can therefore in particular be used in the cosmetics field.
• They can comprise, in addition to the aforementioned ingredients or compounds, at least one physiologically acceptable medium.
• the physiologically acceptable medium is generally suited to the nature of the support to which the composition is to be applied, as well as to the appearance in which the composition is to be packaged.
• the physiologically acceptable medium is represented directly by the aqueous continuous phase as described above.
• physiologically acceptable medium means a medium suitable for cosmetic applications, and suitable in particular for the application of a composition of the invention to a keratin material, in particular the skin and / or the hair, and more particularly the skin.
• the cosmetic compositions of the invention can be, for example, a cream, a lotion, a serum and a gel for the skin (hands, face, feet, etc.), a foundation (liquid, paste), a preparation for baths and showers (salts, foams, oils, gels, etc.), a hair care product (hair dyes and bleaches), a cleaning product (lotions, powders, shampoos), a hair care product (lotions, creams , oils), a styling product (lotions, lacquers, brilliants), a shaving product (soaps, foams, lotions, etc.), a product intended to be applied to the lips, a sun product, a tanning product sunless, a product to whiten the skin, an anti-wrinkle product.
• the cosmetic compositions of the invention can be an anti-aging serum, a youth serum, a moisturizing serum or a scented water.
• Example 1 Physicochemical study of fatty phases comprising at least one lipophilic gelling agent
• This example consisted in preparing thirteen anhydrous gels capable of representing the dispersed fatty phase of a dispersion according to the invention, and in evaluating their physicochemical properties in terms of hardness. (or firmness) (x), stickiness (or adhesion) (y) and cohesion (z).
• These anhydrous gels differ essentially in the nature of the oily solvent and / or the lipophilic gelling agent (ie Rheopearl D2 (equivalent to Rheopearl KL2), Estogel M or OILKEMIA TM 5S polymer) and their concentrations (ie 5%, 10 % and 15%).
• Rheopearl D2 equivalent to Rheopearl KL2
• Estogel M or OILKEMIA TM 5S polymer ie 5%, 10 % and 15%.
• test 1D differs from test
• EMC30 is a premix of Estogel M (INCI: Castor Oil / IPDI Copolymer (and) Caprylic / Capric Triglyceride) in Caprylic / Capric Triglyceride oil in a 30/70 ratio; the corresponding concentrations of lipophilic gelling agent (ie Estogel M) are therefore respectively 5% / 10% / 15% relative to the total weight of the anhydrous gel.
• the melting points of the anhydrous gels are measured according to the method described above and are presented in Table 2 below.
• the physicochemical criteria x, y and z of the anhydrous gels are then measured using the texturometer protocol described above. Note the impossibility of measuring the hardness of the fatty phases of example 18 of application US 2004/137020 and of example 31 of application EP 2 189 081. In fact, these fatty phases are too hard for the texturometer. EZ-X from shimadzu whose maximum force in terms of hardness is however 50 N.
• Figure 1 is a graph showing the hardness criterion (x) of the anhydrous gels in Table 1.
• Figure 2 is a graph showing the tackiness criterion (y) of the anhydrous gels in Table 1.
• Figure 3 is an enlargement of Figure 2 of the tack (y) values of anhydrous gels 2A, 2B, 2C, 3A, 3B, 3C, 5 and 6.
• Figure 4 is a graph showing the cohesion criterion (z) anhydrous gels
• Figures 5 to 7 are graphs representing the texturometry curves of the anhydrous gels in Table 1. These Figures 5 to 7 provide the strength (in N) of the gels in Table 1 as a function of the time (in seconds) during which the gels are subjected (1) to a first compression step (0 to 5 s) then (2) to a second step relaxation where the mobile rises (5 to 10 s). The previous steps (1) and (2) are repeated. These Figures 5 to 7 therefore provide information on the physicochemical properties of the gels in Table 1, in particular in terms of hardness, tackiness and cohesion.
• Hardness (x) as shown in Figure 1, with the percentage of lipophilic gelling agent and oily solvent identical (for example 1 B vs 2B vs 3B), the differences in terms of hardness profiles of the different anhydrous gels tested are not very significant . Furthermore, from tests 1C and 1D, it is observed that the hardness is impacted by the nature of the solvent.
• Cohesion (z) as can be seen from FIG. 4, gels 2B, 3B, 5 and 6 exhibit similar physicochemical properties in terms of cohesion, clearly lower than those of gels 1 B and 1 D.
• ten dispersions are prepared comprising a continuous aqueous phase and a phase dispersed in the form of drops, each time represented by one of the anhydrous gels of example 1. These dispersions are obtained by means of a microfluidic manufacturing process. as described in WO2015 / 055748.
• the microfluidic device used is broken down into two parts, a first part where is carried out, hot (between 70 and 90 ° C), the contact between the fatty phase (also designated IF or Fl) and the aqueous phase (also designated OF or FE) so as to form the dispersion, and a second part ensuring rapid cooling of the dispersion formed to accelerate the gelation kinetics of the drops and thus prevent the risks of coalescence and fragmentation of the drops post-formation (between 10 and 30 ° C).
• compositions of the phases (fluids) allowing the preparation of the dispersions are described in Table 3 below. Table 3
• the OF solution is then introduced into an SOF syringe connected to a heater to keep the OF hot (80 ° C).
• the IF and OF are injected into the microfluidic device and the BF is injected into the dispersion at the outlet of the microfluidic device, according to the flow rates described in the Table 4 below.
• the dispersions obtained can comprise drops endowed with a satisfactory monodispersity and having an average diameter of between 100 ⁇ m and 1500 ⁇ m, in particular between 700 and 1300 ⁇ m.
• each of the ten dispersions is then packaged in three half-filled 30 ml polypropylene (PP) containers. After 1 day at room temperature, each test undergoes one of the three transport tests below (one receptacle per test), namely: - roller test (i.e. horizontal circular movement): Wheaton reference, for 1 hour;
• D1 A dispersion according to Example 2 using as the dispersed fatty phase the anhydrous gel 1A of Example 1.
• the dispersions D1A and D2A exhibit unsatisfactory stability results.
• the corresponding fatty phases are therefore excluded from the rest of the study.
• the D3A dispersion exhibits average stability results but deemed sufficiently satisfactory to be kept for the rest of the study.
• the other dispersions tested exhibit satisfactory stability results.
• the fatty phase must have a cohesion (z) less than or equal to 40, preferably less than or equal to 35, and better still less than or equal to 30.
• a dispersion comprising a dispersed phase comprising drops and a continuous aqueous phase
• the stability of this dispersion is not ensured by the presence of a shell at the interface " continuous aqueous phase / dispersed fatty phase ”or of surfactant, may despite everything and unexpectedly exhibit satisfactory properties in terms of kinetic stability and sensoriality, in particular in terms of comfort and ease of application, provided that the gelled fatty phase either endowed with:
• a tack (y) greater than or equal to -2 N, and better still greater than or equal to -1 N, and in particular greater than or equal to -0.6 N;

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