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
  • A61K8/066—Multiple emulsions, e.g. water-in-oil-in-water
• • 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
  • A61K8/36—Carboxylic acids; Salts or anhydrides 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
  • A61K8/30—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
  • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
  • A61K8/361—Carboxylic acids having more than seven carbon atoms in an unbroken chain; Salts or anhydrides 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
  • A61K8/30—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
  • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
  • A61K8/60—Sugars; Derivatives thereof
  • A61K8/602—Glycosides, e.g. rutin
• • 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
• • 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
  • A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
  • A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
  • A61K8/8152—Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
• • A—HUMAN NECESSITIES
  • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
  • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
  • A61K8/00—Cosmetics or similar toiletry preparations
  • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
  • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
  • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
  • A61K8/87—Polyurethanes
• • 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
  • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
• • 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
  • 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
  • A61K2800/10—General cosmetic use
• • 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

Definitions

• the present invention relates to stable double water-in-oil-in-water emulsions comprising an aqueous continuous phase and drops (G1), in particular macroscopic of a gelled fatty phase, in which the drops (G1) comprise in less one drop (G2), in particular macroscopic, of an internal aqueous phase. It also relates to their method of preparation as well as their use in compositions, in particular cosmetic.
• Encapsulating a compound for example hydrophilic, such as a cosmetic active principle, consists in isolating it from the external environment. This strategy is particularly necessary when this compound is incompatible with other elements of the aqueous phase and / or sensitive to the external environment. Double water-in-oil-in-water emulsions are particularly interesting because they allow the simultaneous encapsulation of hydrophilic and lipophilic compounds in different compartments.
• compositions in particular cosmetic compositions, devoid of silicone compounds because of their environmental impact, since they are not biodegradable, and / or their suspected danger to health.
• the inventors have observed that the presence of 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 emulsion and / or the homogeneity of delivery of the various constituent phases of the emulsion and / or the visual and aesthetic rendering of the emulsion, or even its sensoriality on application.
• the present invention aims to provide a double emulsion, in particular macroscopic, endowed with satisfactory encapsulation properties combined with satisfactory kinetic stability and ease of application and therefore particularly attractive to the consumer.
• the present invention relates to a water-in-oil-in-water emulsion, comprising an external continuous aqueous phase, preferably in the form of a gel, and, as a dispersed phase, a water-in-oil emulsion in the form of a gel.
• the fatty phase 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;
• the emulsion does not include amodimethicone.
• the fatty phase of the drops (G1) of an emulsion 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.
• An emulsion according to the invention therefore comprises at least:
• s continuous fatty phase in the form of drop (s) (G1), which may also be designated by the term “intermediate fatty phase”, “fatty phase”, “intermediate phase”, “oily phase” or “MF”, and
• a continuous aqueous phase which may also be designated by the terms “external aqueous phase”, “external continuous aqueous phase”, “external phase” or “OF”.
• an emulsion according to the invention exhibits satisfactory or even improved performance in terms of non-aggregation of the drops (G1) with one another, of non-adhesion of the drops (G1) to the packaging, and in terms of comfort and ease of application to the skin.
• an emulsion according to the invention also allows more freedom as to the compounds and / or their contents, in particular in active ingredients, which can be encapsulated, in particular in the fatty phase.
• An emulsion according to the invention is therefore particularly advantageous, on the one hand, in that it ensures a particularly satisfactory encapsulation of hydrophilic compounds thanks to the drops (G2), but also of lipophilic compounds thanks to the drops (G1), while being endowed with satisfactory properties in terms of kinetic stability and ease of application to the skin, despite the absence of amodimethicone and therefore of bark, which makes them unprecedented double emulsions.
• stable or “kinetic stability” is meant, within the meaning of the present invention, at room temperature and atmospheric pressure, the absence of creaming or sedimentation of the drops (G1) of fatty phase in the continuous aqueous phase, the absence of creaming or sedimentation of the drops (G2) of the internal aqueous phase in the associated fatty phase, the absence of opacification of the continuous aqueous phase and / or of the fatty phase and / or of the internal aqueous phase, the absence of aggregation of the drops (G1) between them and of the drops (G2) between them, and in particular the absence of coalescence or Oswald ripening of the drops (G1) between them and of the drops (G2) between them , the absence of adhesion of the drops (G1) to the packaging and the absence of material leakage (i) from the fatty phase to the continuous aqueous phase, or vice versa, (ii) from the fatty phase to the aqueous phase internal, or vice versa and (iii) from the
• 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.
• the drops (G1), or even the drops (G2) are macroscopic, that is to say visible to the naked eye.
• macroscopic or “macroscopic drop”, or “macroscopic emulsion” is meant, within the meaning of the present invention, drops (G1), or even drops (G2), visible to the naked eye, as opposed to to microscopic drops not visible to the naked eye.
• the drops (G1) have an average diameter greater than or equal to 400 ⁇ m, preferably greater than or equal to 600 ⁇ m , better still greater than or equal to 800 ⁇ m, in particular greater than or equal to 1000 ⁇ m, or even greater than or equal to 1500 ⁇ m; and or
• the drops (G2) having a diameter greater than or equal to 50 ⁇ m, preferably greater than or equal to 80 ⁇ m, in particular greater than or equal to 100 ⁇ m, or even greater than or equal to 150 ⁇ m, and better still greater than or equal to 200 ⁇ m represent a volume greater than or equal to 60%, or even greater than or equal to 70%, preferably greater than or equal to 80%, and better still greater than or equal to 90% of the total volume of the internal aqueous phase; and or
• the drops (G2) have an average diameter greater than or equal to 50 ⁇ m.
• the size of the drops (G1) is greater than 500 ⁇ m, or even greater than
• 2000 ⁇ m in particular between 800 ⁇ m and 1500 ⁇ m.
• size denotes the diameter, in particular the average diameter, of the drops.
• the aforementioned emulsions can also be designated by the term "dispersions".
• the continuous fatty phase is immiscible with the continuous aqueous phase and the internal aqueous phase at room temperature and atmospheric pressure.
• the solubility of the continuous fatty phase in the continuous aqueous phase and the internal aqueous phase is advantageously less than 5% by mass, and vice versa.
• An emulsion according to the invention can be described as a macroscopically inhomogeneous mixture of at least two immiscible phases, in particular when the drops (G1), or even the drops (G2), are macroscopic.
• each of the phases can be individualized, in particular with the naked eye.
• an emulsion according to the invention does not include a surfactant.
• an emulsion according to the invention does not comprise glyceryl trioctanoate, glycerol tricaprylate / caprate, and their mixture.
• an emulsion according to the invention does not include:
• the drops (G1), or even the drops (G2) advantageously have an apparent monodispersity (ie they are perceived to the eye as spheres identical in diameter).
• the drops (G1), or even the drops (G2), are advantageously substantially spherical.
• the drops (G1) and (G2) of an emulsion according to the invention are devoid of bark or membrane, in particular of polymeric membrane or formed by interfacial polymerization.
• the drops (G1) and (G2) are not stabilized using a coacervate membrane (anionic polymer (carbomer) / cationic polymer (amodimethicone) type).
• a coacervate membrane anionic polymer (carbomer) / cationic polymer (amodimethicone) type.
• an emulsion according to the invention does not include a bark, in particular a bark formed from a layer of coacervate interposed between the fatty phase and the external and internal aqueous phase.
• an emulsion according to the invention does not comprise (is devoid of) lipophilic cationic polymer corresponding to the following formula: in which :
• R1, R2 and R3, independently of each other, represent OH or CH3;
• - R4 represents a -CH2- group or a -X-NH- group in which X is a divalent C3 or C4 alkylene radical;
• - x is an integer between 10 and 5000, preferably between 30 and 1000, and better still between 80 and 300;
• - 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;
• - z is an integer between 0 and 10, preferably between 0 and 1, and better still equal to 1.
• the drops (G1), or even the drops (G2) differ from solid capsules, that is to say capsules provided with a solid shell (or “membrane”), such as for example those described in WO 2010 / 063937, and capsules with an evanescent rind, such as for example those described in WO2018077986 and WO2018077977.
• a solid shell or “membrane”
• capsules with an evanescent rind such as for example those described in WO2018077986 and WO2018077977.
• microfluidic process used to manufacture an emulsion according to the invention makes it possible to form macroscopic drops (G1) and (G2) with at least drops (G1), or even drops (G2), which are monodisperse.
• the microfluidic process allows perfect control of the contents of each phase implemented, and therefore of the concentrations of the encapsulated active ingredients.
• the pH of an emulsion is typically between 4.0 and 8.0, in particular between 5.0 and 7.0.
• the invention also relates to the use of an emulsion according to the invention, for the preparation of a composition, in particular cosmetic.
• An emulsion according to the invention, or even a composition comprising it can also be dedicated, for example, to the field of medicine, pharmacy, agriculture, nutrition or (agro) -alimentary.
• the invention also relates to a composition, in particular cosmetic, comprising at least one emulsion according to the invention and, in particular, a physiologically acceptable medium.
• the viscosity of an emulsion according to the invention or of at least one of its phases can vary significantly, which makes it possible to obtain various textures.
• the viscosity is measured at ambient temperature and at ambient pressure according to the method described in WO20 17046305.
• an emulsion according to the invention has a viscosity of from 1 mPa.s to 500,000 mPa.s, preferably from 10 mPa.s to 300,000 mPa.s, better from 400 mPa.s to 100 000 mPa.s, and more particularly from 1000 mPa.s to 30,000 mPa.s, as measured at 25 ° C. according to the method described above.
• an emulsion according to the invention comprises an external continuous aqueous phase, preferably in the form of a gel, in particular of a gel having a viscosity suitable for suspending the drops (G1) and thus contributing to the kinetic stability. and the attractive visual of an emulsion according to the invention.
• a good suspension of the drops (G1) makes it possible to prevent / reduce unwanted phenomena such as the coalescence of the drops (G1) between them and / or the adhesion of the drops (G1) to the internal walls of the packaging and / or creaming or sedimentation of the drops (G1), such as to alter the appearance of the emulsion and the homogeneity of delivery of the various constituent phases of the emulsion.
• the continuous aqueous phase is not solid at room temperature and at room pressure, that is to say it is able to flow under its own weight.
• the continuous aqueous phase has a viscosity of between 400 mPa.s and 100,000 mPa.s, preferably between 800 mPa.s and 30,000 mPa.s, as measured at 25 ° C according to the method described above.
• the external continuous aqueous phase of the emulsions comprises at least water.
• a water suitable for the invention can also be a natural spring water or a floral water.
• the percentage by mass of water of the external aqueous continuous phase is at least 30%, preferably at least 40%, in particular at least 50%, and better still at least 60%, in particular between 70% and 98%, and preferably between 55% and 95%, in particular between 75% and 85%, relative to the total mass of said external aqueous phase.
• the external continuous aqueous phase of the emulsion according to the invention may further comprise at least one base. It can comprise a single base or a mixture of several different bases.
• the external continuous aqueous phase of an emulsion according to the invention comprises at least one pH-sensitive gelling agent, the presence of at least one base in said aqueous continuous phase contributes in particular to increasing the viscosity of the latter.
• the base present in the aqueous phase is a mineral base.
• the mineral base is chosen from the group consisting of alkali metal hydroxides and alkaline earth metal hydroxides.
• the inorganic base is an alkali metal hydroxide, and in particular
• the base present in the external aqueous phase is an organic base.
• organic bases mention may be made, for example, of ammonia, pyridine, triethanolamine, aminomethylpropanol, or also triethylamine.
• An emulsion according to the invention can comprise from 0.01% to 10% by weight, preferably from 0.01% to 5% by weight, and preferably from 0.02% to 1% by weight of base, preferably of mineral base, and in particular NaOH, relative to the total weight of said emulsion.
• the double emulsions according to the invention comprise, as the dispersed phase, a water-in-oil emulsion in the form of drops (G1).
• a drop (G1) according to the invention consists of a continuous fatty phase comprising at least one drop (G2) formed of a dispersed aqueous phase (also called internal aqueous phase).
• an emulsion according to the invention is obtained by a microfluidic process as defined below. Therefore, the drops (G1) present a uniform size distribution.
• the fatty phase of the emulsions of the invention consists of a population of monodisperse drops (G1), in particular such that they have an average diameter D of from 500 ⁇ m to 3000 ⁇ m and a coefficient of 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 dispersed phase 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, depending on the size of the container containing the drops of the emulsion.
• 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.
• the standard deviation s of an emulsion reflects the distribution of the diameters D, of the drops of the emulsion around the mean diameter D.
• the coefficient of variation can be calculated: s
• each drop (G1) comprises a fatty phase corresponding to the fatty phase of the emulsions according to the invention.
• the continuous fatty phase of an emulsion according to the invention has a melting point of between 50 ° C and 100 ° C, preferably between 60 ° C and 90 ° C.
• the melting point of a fatty phase can be measured using a differential scanning calorimeter (DSC), for example the calorimeter sold under the name “DSC Q2000” by the company TA Instruments.
• DSC differential scanning calorimeter
• the sample preparation and measurement protocols are as follows: a 5 mg sample of the sample to be tested, previously heated to 80 ° C and taken with magnetic stirring using a spatula also heated, is placed in an aluminum thermal capsule, or crucible. Two tests are carried out to ensure the reproducibility of the results. The measurements are carried out on the calorimeter mentioned above. The oven is subjected to a nitrogen sweep. Cooling is provided by the RCS 90 heat exchanger.
• 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 variation in the difference in power absorbed by the empty crucible and by the crucible containing the sample is measured as a function of the temperature.
• 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 continuous fatty phase of an emulsion according to the invention must satisfy at least the two following physicochemical criteria of hardness and tackiness:
• the hardness (x) is an indicator of the sensory rendering of an emulsion on application to a keratin material, in particular the skin.
• the hardness must not be too low to guarantee the drops (G1) of continuous fatty phase sufficient mechanical resistance, in particular to the shears and / or to the mechanical stresses linked, for example, to the manufacture and packaging of the liquid.
• the emulsion and / or its transport guarantee the emulsion satisfactory kinetic stability, in particular in the presence of non-airless packaging.
• the hardness should not be too great so as not to degrade the sensoriality, in particular the comfort and the ease of application of the emulsion when applying to the skin. The above is exacerbated the larger the diameter of the continuous fatty phase drops (G1).
• the sticky (y) is an indicator of the kinetic stability of the emulsion with regard to the phenomena of adhesion of the drops (G1) to the wall of the packaging.
• the continuous fatty phase of an emulsion 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.
• the fatty phase continuous advantageously has a cohesion (z) greater than or equal to 15, preferably greater than or equal to 20, and better still greater than or equal to 25.
• the continuous fatty phase has a cohesion (z) of between 15 and 40, preferably between 20 and 35, and better still between 20 and 30.
• Cohesiveness corresponds to the way in which the tested product resists the second deformation, relative to the way in which it behaved during the first deformation.
• Cohesion corresponds to the surface of the second curve (Area.
• the cohesion criterion (z) is an indicator of the kinetic stability of the emulsion with regard to the phenomena of aggregation, or even coalescence, of the drops (G1) with one another. Cohesion corresponds to the property of the drops (G1) to stick to themselves. Thus, a minimum of cohesion is needed to ensure the “gelled” nature of the drops (G1) but not too much to prevent the gelled drops (G1) from sticking together.
• the sample to be tested is placed in a mold 40 mm in diameter filled to 75% of its height.
• the mobile used is a cylindrical acrylic mobile 12.7 mm in diameter. Moving the mobile has 4 stages:
• This combination of physicochemical criteria constitutes a non-obvious compromise characterizing an anhydrous gel that is brittle but not very sticky and not very elastic.
• this combination of physicochemical criteria provides access to emulsions, in particular macroscopic, with satisfactory or even improved performance in terms of kinetic stability, and therefore of visual and aesthetic rendering, and of sensoriality. , in particular of comfort and ease of application on the skin, despite the absence of amodimethicone and therefore bark.
• the hardness values in N obtained by the above-mentioned measurement method, can easily be converted into Pa, for example with regard to the surface of the 12.7 mm acrylic cylindrical mobile mentioned above.
• 1 MPa is equivalent to 1 N / mm 2 .
• N the hardness values according to the invention measured into N.
• the continuous fatty phase drops (G1) are preferably based on a viscoelastic gel with an elastic modulus greater than the viscous modulus.
• the drops (G1) do not flow under their own weight, but can easily be deformed by pressure, for example with a finger. Thus, their consistency is close to that of butter, with a malleable and gripping character.
• the drops (G1) can be spread easily by hand, in particular on a keratin material, in particular the skin.
• the continuous fatty phase preferably has a viscosity suitable for suspending the drops (G2) and thus contributing to the kinetic stability and to the attractive appearance of an emulsion according to the invention. Indeed, a good suspension of the drops (G2) makes it possible to prevent / reduce unwanted phenomena such as the coalescence of the drops (G2) between them and / or the creaming or sedimentation of the drops (G2).
• the continuous fatty phase of an emulsion according to the invention comprises at least one lipophilic gelling agent. It is essentially the combination of at least one lipophilic gelling agent and at least one oily solvent which allows the dispersed fatty phase of an emulsion according to the invention to meet the physicochemical criteria x and y, or even z, mentioned above.
• the presence of at least one lipophilic gelling agent in the fatty phase of the drops (G1) contributes in particular to (i) suspend the drop (s) (G2) within each drop (G1) and (ii) to strengthen the mechanical resistance of the drops (G1) and therefore the kinetic stability of an emulsion according to the invention.
• 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.
• Lipophilic gelling agent organic or inorganic, polymeric or molecular Mention may be made, as mineral lipophilic gelling agent, of optionally modified clays, such as hectorites modified with a C 10 to C 22 ammonium chloride, such as hectorite modified with di-stearyl di-methyl ammonium chloride such as, for example, that marketed under the name Bentone 38V ® by the company ELEMENTIS.
• optionally modified clays such as hectorites modified with a C 10 to C 22 ammonium chloride, such as hectorite modified with di-stearyl di-methyl ammonium chloride such as, for example, that marketed under the name Bentone 38V ® by the company ELEMENTIS.
• quaternium-18 bentonite such as the products sold or manufactured under the names Bentone 34 by the company Rheox, Claytone XL, Claytone 34 and Claytone 40 sold or
• fumed silica optionally hydrophobic treated at the surface, the particle size of which is less than 1 ⁇ m. It is in fact possible to chemically modify the surface of the silica, by chemical reaction generating a reduction in the number of silanol groups present at the surface of the silica. It is in particular possible to substitute silanol groups with hydrophobic groups: a hydrophobic silica is then obtained.
• hydrophobic groups can be:
• Silicas thus treated are named "Silica Silylate” according to the CTFA (8th edition, 2000). They are for example marketed under the references Aerosil R812 ® by Degussa, Cab-O-Sil TS-530 ® by the company Cabot; Where
• silica thus treated are known as "silica dimethyl Silylate" according to the CTFA (8th edition, 2000). They are for example marketed under the references Aerosil R972 ® and Aerosil R974 ® by Degussa, Cab-O-Sil TS-610 ® and CAB-O-SIL TS-720 ® by the company Cabot.
• the hydrophobic fumed silica has in particular a particle size which can be nanometric to micrometric, for example ranging from about 5 to 200 nm.
• Polymeric organic lipophilic gelling agents are, for example, partially or totally crosslinked elastomeric organopolysiloxanes, of structure three-dimensional, such as those marketed under the names KSG6 ® , KSG16 ® and KSG18 ® by the company SHIN-ETSU, of Dow Corning® EL-7040, of Trefil E-505C ® and of Trefil E-506C ® by the company DOW -CORNING, of Gransil SR-CYC ® , SR DMF10 ® , SR- DC556 ® , SR 5CYC gel ® , SR DMF 10 gel ® and of SR DC 556 gel ® by the company GRANT INDUSTRIES, of SF 1204 ® and of JK 113 ® by the company GENERAL ELECTRIC; ethyl cellulose such as that sold under the name Ethocel ® by Dow CFIEMICAL; galactommanans comprising from one to six, and in
• 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 inulin and fatty acid (s) or esters of glycerol and 'Fatty acids ; polyamides; and their mixtures.
• lipophilic gelling agent mention may also be made of polymers with a weight-average molecular mass of less than 100,000, comprising a) a polymeric backbone having hydrocarbon repeating units provided with at least one heteroatom, and optionally b) at least one fatty chain pendant and / or at least one optionally functionalized terminal fatty chain, having from 6 to 120 carbon atoms and being linked to these hydrocarbon-based units, as described in applications WO 02/056847, WO 02/47619, in particular the resins of polyamides (in particular comprising alkyl groups having from 12 to 22 carbon atoms) such as those described in US Pat. No. 5,783,657.
• polymers with a weight-average molecular mass of less than 100,000 comprising a) a polymeric backbone having hydrocarbon repeating units provided with at least one heteroatom, and optionally b) at least one fatty chain pendant and / or at least one optionally functionalized terminal fatty chain, having from 6 to 120 carbon atoms and being linked to these hydrocarbon
• Silicone polyamides of the polyorganosiloxane type such as those described in US Pat. No. 5,874,069, US 5,919,441, US 6,051,216 and US 5,981,680 can also be used. These silicone polymers can belong to the following two families:
• Polyorganosiloxanes comprising at least two groups capable of establishing hydrogen interactions, these two groups being located on grafts or branches.
• esters of dextrin and of fatty acid 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 FU , Rset FÎ 6, which are identical or different, are chosen from hydrogen or an acyl group -COR a in which the radical R a 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 R 4 , R 5 OR R 6 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 FU , Rset FÎ 6, which are identical or different, are chosen from hydrogen or an
• 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.
• esters of inulin and of fatty acid there may also be mentioned esters of inulin and of fatty acid. Mention may in particular be made of the esters of inulin and of fatty acid (s) sold under the names Rheopearl® ISK2 or Rheopearl® ISL2 (INCI name: Stearoyl Inulin) by the company Miyoshi Europe.
• 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.
• esters of glycerol and of fatty acid (s) in particular a mono-, di- or triester of glycerol and of fatty acid (s).
• said ester of glycerol and of 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 chosen from the group consisting of behenic acid, isooctadecanoic acid, stearic acid, eicosanoic acid, and mixtures thereof.
• the ester of glycerol and of fatty acid (s) has the following formula (III): in which: R 1, R 2 and R 3 are, independently of one another, chosen from H and a saturated alkyl chain comprising from 4 to 30 carbon atoms, at least one of R 1, R 2 and R 3 being different from H. According to one embodiment, Ri, R 2 and R3 are different.
• 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 30 ° C. up to 120 ° C.
• the waxes capable of being used in an emulsion according to the invention can be chosen from waxes, solid, deformable or not at room temperature, of animal, plant, mineral or synthetic origin, and mixtures thereof. It is in particular possible to use hydrocarbon waxes such as beeswax, lanolin wax, and Chinese insect waxes; rice wax, Carnauba wax, Candellila wax, Ouricurry wax, Alfa wax, cork fiber wax, sugar cane wax, Japanese wax and sumac wax ; montan wax, microcrystalline waxes, paraffins and ozokerite; polyethylene waxes, waxes obtained by Fisher-Tropsch synthesis and waxy copolymers as well as their esters.
• hydrocarbon waxes such as beeswax, lanolin wax, and Chinese insect waxes
• rice wax Carnauba wax, Candellila wax, Ouricurry wax, Alfa wax, cork fiber wax, sugar cane wax, Japanese wax and sumac wax
• montan wax microcrystalline wax
• Mention may in particular be made of the waxes sold under the names Kahlwax®2039 (INCI name: Candelilla cera) and Kahlwax®6607 (INCI name: Helianthus Annuus Seed Wax) by the company Kahl Wachsraffinerie, Casid HSA (INCI name: Hydroxystearic Acid) by the SACI CFPA company, Performa®260 (INCI name: Synthetic wax) and Performa®103 (INCI name: Synthetic wax) by New Phase company, and AJK-CE2046 (INCI name: Cetearyl alcohol, dibutyl lauroyl glutamide, dibutyl ethylhaxanoyl glutamide) by the company Kokyu Alcohol Kogyo. Mention may also be made of waxes obtained by catalytic hydrogenation of 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 FR 2 792 190.
• 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 (C oC 6 o) alkyldimethicones, 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. Butter (s) or pasty fatty substance
• 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 liquid fraction 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 present 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 analysis. thermal (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 .
• DSC differential scanning calorimeter
• the sample preparation and measurement protocols are as described in WO2017046305.
• the liquid fraction by weight of the butter (or pasty fatty substance) at 25 ° C. is equal to the ratio of the enthalpy of fusion consumed at 25 ° C. to the enthalpy of fusion of the butter.
• the enthalpy of fusion of butter or pasty compound is the enthalpy consumed by the compound to change from the solid state to the liquid state.
• Butter is said to be in the solid state when all of its mass is in crystalline solid form.
• Butter is said to be in the liquid state when all of its mass is in liquid form.
• 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.
• 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 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.
• lanolin and its derivatives such as lanolin alcohol, oxyethylenated lanolins, acetylated lanolin, lanolin esters such as isopropyl lanolate, oxypropylenated lanolins, polymeric or non-polymeric silicone compounds such as polydimethysiloxanes of high molecular masses, polydimethysiloxanes with side chains of the alkyl or alkoxy type having from 8 to 24 carbon atoms, in particular stearyl dimethicones,
• 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 13.2.2.2F. Shea Butter, Borneo Tallow, and Related Fats (Vegetable Butters)).
• C10-C18 triglycerides comprising at a temperature of 25 ° C and at atmospheric pressure (760 mm Fig) a liquid fraction and a solid fraction, shea butter, Nilotica shea butter (Butyrospermum parkii), Galam butter, (Butyrospermum parkii), Borneo butter or fat or tengkawang tallow) (Shorea stenoptera), Shorea butter, Illipe butter, Madhuca butter or Bassia Madhuca longifolia, mowrah butter (Madhuca Latifolia), Katiau butter (Madhuca mottleyana), Phulwara butter (M.
• C10-C18 Triglycerides comprising at a temperature of 25 ° C and at atmospheric pressure (760 mm Fig) a liquid fraction and a solid fraction, shea butter, Nilotica shea butter (Butyrospermum parkii), Galam butter, (Butyrospermum parkii), Borneo butter or
• Butyracea mango butter (Mangifera indica), Murumuru butter (Astrocatyum murumuru), Kokum butter ( ' Garcinia Indica) , Ucuuba butter (Virola sebifera), Tucuma butter, Painya butter (Kpangnan) (Pentadesma butyracea), coffee butter (Coffea arabica), apricot butter (Prunus Armeniaca), Macadamia (Macadamia Temifolia), grape seed butter (Vitis vinifera), avocado butter (Persea gratissima), olive butter (Olea europaea), sweet almond butter (Prunus amygdalus dulcis), cocoa butter (Theobroma cacao) and sunflower butter, butter under the INCI name Astrocaryu m Murumuru Seed Butter, butter under the INCI name Theobroma Grandiflorum Seed Butter, and butter under the INCI name Irvingia Gabonensis Kernel Butter, jojoba esters (mixture
• 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 Triglyceride (and) Polyurethane-79, in particular sold under the name OILKEMIA TM 5S polymer by the company Lubrizol, Trihydroxystearin, in particular sold under the name THIXCIN® R by the company Elementis Specialties, and their mixtures, and better still Castor Oil / IPDI Copolymer (and) Caprylic / Capric Triglycéride.
• an emulsion according to the invention in particular the fatty phase of the drops (G1), does not comprise an elastomer gel comprising at least one dimethicone, in particular as marketed by NuSil Technology under the name CareSil. TM CXG-1104 (INCI: Dimethicone (and) Dimethicone / Vinyl Dimethicone Crosspolymer).
• the viscosity of the fatty phase of the drops (G1) of an emulsion according to the invention is between 20,000 and 100,000,000 mPa.s, preferably between 50,000 and 1,000,000 mPa.s, and better still between 100,000 to 500,000 mPa.s, at 25 ° C.
• lipophilic gelling agent (s) and / or their quantity so as to satisfy the melting points and physicochemical properties x and y, or even z, of the phase. oily the aforementioned.
• the nature and / or the amount of lipophilic gelling agent (s) must take into account the process used (in particular of the “non-microfluidic” or “microfluidic” type) for the manufacture of the liquid. emulsion according to the invention. These adjustments fall within the competence of those skilled in the art with regard to the teaching of the present description.
• an emulsion according to the invention can comprise from 0.5% to 25%, preferably from 1% to 20%, in particular from 1.5% to 15%, and better still from 2% to 10%, in weight of lipophilic gelling agent (s) relative to the total weight of the continuous fatty phase of the drops (G1). These percentages therefore mean lipophilic gelling agent (s) only present in the dispersed fatty phase.
• the content of lipophilic gelling agent (s) is greater than or equal to 2%, preferably greater than or equal to 5%, and better still greater than or equal to 8% by weight, relative to the weight total of the continuous fatty phase of the drops (G1).
• the continuous fatty phase of the drops (G1) can comprise at least one oil.
• oil means a fatty substance that is liquid at room temperature (25 ° C.).
• oils which can be used in the emulsion of the invention there may be mentioned, for example:
• 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, isopropyl myristate, 2-ethylhexyl palmitate, 2-octyl stearate -dodecyl, octyl-2-dodecyl erucate, isostearyl isostearate; hydroxylated esters such as isostearyl lactate, octylhydroxystearate, octyldodecyl hydroxy stearate, diisostearyl malate, triisoketyl citrate, fatty alcohol heptanoates
• hydrocarbons of mineral or synthetic origin, such as paraffin oils, volatile or not, and their derivatives, petroleum jelly, polydecenes, hydrogenated polyisobutene such as sesam oil;
• 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 2 to 24 carbon atoms; phenylated silicones such as phenyltrimethicones, phenyldimethicones, phenyltrimethylsiloxydiphenyl-siloxanes, diphenyl-dimethicones, diphenylmethyldiphenyl trisiloxanes, 2-phenylethyltrimethylsiloxysilicates, and polymethylsiloxysphilicates;
• PDMS polymethylsiloxa
• - fatty alcohols having 8 to 26 carbon atoms such as cetyl alcohol, stearyl alcohol and their mixture (cetylstearyl alcohol), or octyldodecanol;
• the continuous fatty phase 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, meadowfoam seed oil Limnanthes Alba (INCI name: Limnanthes Alba (Meadowfoam) Seed Oil), macadamia nut oil (name INCI: Macadamia Ternifolia Seed Oil), rosehip oil Rosa Canina (INCI name: Rosa Canina Fruit Oil), soybean oil (INCI name: Glycine Soja (Soybean) Oil), sunflower seed oil (INCI name: Helianthus Annuus (Sunflower) Seed Oil), tribhenin (INCI name: tribehenin), triisostearin (INCI name: triis
• 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 an emulsion according to the invention comprises at least one, or even at least two, hydrocarbon oil (s) of vegetable origin, preferably chosen from seed oil of meadowfoam.
• Hydrocarbon oil (s) of vegetable origin preferably chosen from seed oil of meadowfoam.
• Limnanthes Alba INCI name: Limnanthes Alba (Meadowfoam) Seed Oil, triglycerides of caprylic and capric acids, and their mixture.
• the oil which may be present in the fatty phase of an emulsion according to the invention is not a silicone oil or a fluorinated oil.
• an emulsion according to the invention in particular the dispersed fatty phase, does not comprise polydimethylsiloxane (PDMS or dimethicone) or one of its derivatives, and preferably does not comprise silicone oil, and in particular of 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
• An emulsion according to the invention can comprise between 0% and 99.5%, preferably between 5% and 95%, in particular between 20% and 90%, better still between 30% and 80%, or even between 50% and 70%, by weight of oil (s) relative to the total weight of the continuous fatty phase of the drops (G1).
• An emulsion according to the invention can comprise from 1% to 50%, preferably from 5% to 40%, and better still from 10% to 25%, by weight of oil (s) relative to the total weight of said emulsion.
• an emulsion according to the invention is also advantageous in that its kinetic stability allows high percentages of continuous fatty phase and therefore in drops (G1).
• an emulsion according to the invention can comprise from 0.1% to 70%, preferably from 0.5% to 65%, in particular from 1% to 60%, or even from 3% to 50%, preferably from 5% to 40%, better still 10% to 30%, and in particular from 15% to 20%, by weight of continuous fatty phase, and therefore of drops (G1), relative to the total weight of the emulsion.
• each drop (G1) comprises at least one drop (G2) comprising the internal aqueous phase.
• each drop (G1) comprises at least two, preferably at least five, and in particular at least 10, drop (G2) comprising the internal aqueous phase.
• each drop (G1) comprises the same number of drop (s) (G2).
• the drops (G2) do not flow under their own weight, but can be easily deformed by pressure, for example with a finger, including in the presence of a hydrophilic gelling agent as described below.
• the size (or diameter) of the drops (G1) is necessarily greater than the size (or diameter) of the associated drop (s) (G2) ).
• the size of the drops (G2) is greater than 50 ⁇ m, or even greater than 80 ⁇ m, and better still between 50 ⁇ m and 2000 ⁇ m, in particular between 80 ⁇ m and 1500 ⁇ m, better still between 100 ⁇ m and 1.
• an emulsion according to the invention comprises from 0.1% to 50%, preferably from 1% to 40%, in particular from 2.5% to 30%, and better still from 5% to 20%, by weight of internal aqueous phase, and therefore of drops (G2), relative to the total weight of the continuous fatty phase, and therefore of drops (G1).
• the volume fraction p (IF / (IF + MF) is between 0.1 and 0.7, preferably between 0.3 and 0.6, and better still between 0.4 and 0.5, where:
• IF represents the total volume of drops (G2)
• MF represents the total volume of the drops (G1) (and therefore without the total volume of the drops (G2)).
• an emulsion according to the invention is obtained by a microfluidic process as defined below. Therefore, the drops (G2) advantageously have a uniform size distribution.
• the internal aqueous phase of the emulsions of the invention consists of a population of monodisperse drops (G2), in particular such that they have an average diameter D of from 50 ⁇ m to 2000 ⁇ m and a coefficient of variation Cv less than 10%, or even less than 3%, measured according to the methods described above.
• the drops (G1) and (G2) are respectively monodisperse drops as defined above.
• the internal aqueous phase of the drops (G2) of an emulsion according to the invention can be a gas phase.
• the internal phase of such drops (G2) comprises at least one gas, for example chosen from air, oxygen, nitrogen, nitrous oxides, rare gases, carbon dioxide, and their mixtures.
• an emulsion according to the invention can comprise at least two populations of drops (G1) which differ from one another by, in particular, the diameter of the drops (G1) and / or the nature of the materials.
• raw materials is intended to denote any type of compound capable of being used in the fatty phase of the drops (G1) and the internal aqueous phase of the drops (G2), for example oils, gelling agents, oils. texturing agents, the active agents and the additional compounds described in the present description.
• the drops (G2) according to the invention comprise an internal aqueous phase, identical to or different, preferably different, from the continuous aqueous phase described above.
• the internal aqueous phase is not solid at room temperature and at room pressure, that is to say it is able to flow under its own weight.
• the internal aqueous phase has a viscosity of between 0 mPa.s and 10,000 mPa.s, 10,000 mPa.s, preferably between 0 mPa.s and 2,000 mPa.s, as measured at 25 ° C. This viscosity is measured according to the method described above.
• the internal aqueous phase of the emulsions comprises at least water.
• a water suitable for the invention can also be a natural spring water or a floral water.
• the mass percentage of water in the internal aqueous phase is at least 30%, preferably at least 40%, in particular at least 50%, and better still at least 60 %, in particular between 70% and 98%, and preferably between 75% and 95%, relative to the total mass of said internal aqueous phase.
• the external continuous aqueous phase and / or the internal aqueous phase can be provided in the form of an oil-in-water emulsion, identical or different, said emulsion comprising a continuous aqueous phase. and a fatty phase dispersed in the form of drops (G3), the size of the drops (G3) being less than 500 ⁇ m, preferably less than 400 ⁇ m, in particular less than 300 ⁇ m, better still less than 200 ⁇ m, in particular less than 100 ⁇ m, or even less than 20 ⁇ m, and better still less than 10 ⁇ m.
• the size of the drops (G3) is between 0.1 and 200 ⁇ m, preferably between 0.25 and 100 ⁇ m, in particular between 0.5 ⁇ m and 50 ⁇ m, preferably between 1 ⁇ m and 20 ⁇ m, and better between 1 ⁇ m and 10 ⁇ m, or even between 3 ⁇ m and 5 ⁇ m.
• the fatty phase of the drops (G1) can be in the form of a water-in-oil emulsion, said emulsion comprising the continuous fatty phase and an aqueous phase dispersed in the form of drops (G4 ), the size of the drops (G4) being necessarily smaller than the drops (G1) and preferably smaller than the drops (G2).
• the size of the drops (G4) is less than 500 ⁇ m, preferably less than 400 ⁇ m, in particular less than 300 ⁇ m, better still less than 200 ⁇ m, in particular less than 100 ⁇ m, or even less than 20 ⁇ m, and better less than 10 ⁇ m.
• the size of the drops (G4) is between 0.1 and 200 ⁇ m, preferably between 0.25 and 100 ⁇ m, in particular between 0.5 ⁇ m and 50 ⁇ m, preferably between 1 ⁇ m and 20 ⁇ m, and better between 1 ⁇ m and 10 ⁇ m, or even between 3 ⁇ m and 5 ⁇ m.
• the drops (G3) and / or (G4) are not macroscopic, and are therefore microscopic, that is to say not visible to the naked eye.
• the drops (G3) and / or (G4) are different and independent of the drops (G1) and (G2). Furthermore, when the drops (G3) are present in the internal aqueous phase, the size of the drops (G3) is smaller than the size of the drops (G2).
• an emulsion according to the invention comprising drops (G3) and / or (G4) spread easily on the skin.
• the first moments of application are very watery with a marked brittle effect.
• the feeling evolves into an oily veil that fades to leave skin light and hydrated.
• This texture is particularly advantageous and surprising for those skilled in the art in view of the absence of surfactants and of bark in these emulsions.
• An emulsion according to the invention and in particular the internal aqueous phase and / or the external aqueous phase and / or the fatty phase, can / can also comprise at least one additional compound different from the lipophilic gelling agent and from the aforementioned oils. .
• An emulsion according to the invention can thus further comprise, as additional compound, 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; modifying agents chosen from gelling agents / texture, viscosity, in particular hydrophilic such as those described below, different from the base and lipophilic gelling agents mentioned above, pH, osmotic strength and / or modifiers of refractive index etc ... or any usual cosmetic additive; and their mixtures.
• 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
• 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.
• pill agents insoluble in the fatty phase is meant within the meaning of the invention the group consisting of pigments, ceramics, polymers, in particular acrylic polymers, and mixtures thereof.
• the emulsions according to the invention and in particular the internal aqueous phase and / or the external aqueous phase and / or the continuous fatty phase of the emulsions can also further comprise at least one active agent, in particular biological or cosmetic, preferably chosen from among moisturizing 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, anti-aging agents, perfuming agents and mixtures thereof.
• active agents are in particular described in FR 1 558 849. Hydrophilic gelling agent (s)
• an emulsion according to the invention in particular the external aqueous phase and / or the internal aqueous phase, may further comprise at least one hydrophilic gelling agent different from the oils and lipophilic gelling agents described above.
• hydrophilic gelling agent can be designated interchangeably by the term “hydrophilic texturizing agent”.
• the hydrophilic gelling agent makes it possible to modulate the fluidity of the emulsion, and therefore the sensorality and / or galenic nature, which it is desired to obtain and / or contribute to further improve the kinetic stability of the emulsion, in particular by preventing / preventing the phenomena of transfer of compounds from the internal aqueous phase to the continuous aqueous phase, or vice versa.
• hydrophilic gelling agents that is to say soluble or dispersible in water, and therefore which may be present in the external aqueous phase and / or the internal aqueous phase of an emulsion according to the invention, there may be mentioned those cited in FR3041251, and in particular:
• alkasealan Alcaligenes Polysaccharides
• other natural agents in particular l 'hyaluronic acid
• - semi-synthetic gelling agents in particular chosen from cellulose derivatives and modified starches,
• gelling agents in particular chosen from glycols, polyethylene glycols (marketed under the name Carbowax), clays, silicas such as those marketed under the names Aerosil® 90/130/150/200/300/380), in particularly glycerin, propylene glycol, butylene glycol, pentethylene glycol, propanediol, methylpropanediol, hexanediol, 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 FR 2 999 921. Preferably, they are amphiphilic and anionic associative polymers and amphiphilic and nonionic associative polymers as described below.
• the continuous aqueous phase and / or the internal aqueous phase comprises at least one hydrophilic gelling agent chosen from Carbomer, alkasealan (INCI: Alcaligenes Polysaccharides), agar-agar and their mixtures.
• hydrophilic gelling agent chosen from Carbomer, alkasealan (INCI: Alcaligenes Polysaccharides), agar-agar and their mixtures.
• the continuous aqueous phase and / or the internal aqueous phase comprises at least one hydrophilic gelling agent chosen from natural texturing agents, in particular algae extracts such as agar-agar, carrageenans, alginates, and mixtures thereof, and preferably agar-agar.
• hydrophilic gelling agent chosen from natural texturing agents, in particular algae extracts such as agar-agar, carrageenans, alginates, and mixtures thereof, and preferably agar-agar.
• a hydrophilic gelling agent in particular when present in the internal aqueous phase, is a thermosensitive gelling agent, namely which reacts with heat, and in particular is a solid gelling agent at room temperature and liquid at a temperature above 50 ° C. , preferably greater than 60 ° C, and more preferably greater than 70 ° C.
• a thermosensitive hydrophilic 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, and advantageously chosen from agar-agar.
• thermosensitive hydrophilic gelling agent in the internal aqueous phase advantageously makes it possible to prevent the phenomena of coalescence of the drops (G2) between them and / or of migration of compounds present in the internal aqueous phase towards the external aqueous phase, or Conversely.
• the internal aqueous phase and the external aqueous phase of an emulsion according to the invention differ in nature and / or in the content of hydrophilic gelling agent (s).
• an emulsion 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%, in weight of hydrophilic gelling agent (s) relative to the total weight of the aqueous phase comprising it.
• the internal aqueous phase and / or the external aqueous phase comprises at least one additional and / or active compound, in particular a hydrophilic cosmetic active agent, which has a LogP of less than 1, in particular less than 0.5 , better less than 0, or even between 0.5 and -2.5, and better still between 0 and -2.5.
• a hydrophilic cosmetic active agent which has a LogP of less than 1, in particular less than 0.5 , better less than 0, or even between 0.5 and -2.5, and better still between 0 and -2.5.
• the additional and / or active compound (s), in particular a lipophilic cosmetic active ingredient, added in the continuous fatty phase to the drops (G1) of an emulsion according to the invention preferably has a LogP greater than 1, in particular greater than 2, better still greater than 3, or even between 1 and 7, in particular between 1, 5 and 5, and better still between 2 and 3 , 5.
• log P (known as the octanol / water partition coefficient of a molecule) gives an estimate of the hydrophobicity of the molecule considered and has the advantage of being referenced / tabulated and therefore of being easily accessible for most molecules. classic.
• log P log (K)
• log (K)) can be easily evaluated using molecular modeling software easily accessible on the internet such as for example on www. mo I isp i rat ion.com, www. vcclab. org / lab / alogps / start. html.
• An experimental determination is possible by the following method: weigh a precise amount of the active ingredient and dissolve it in one of the two phases of water or octanol. Two equivalent volumes of the 2 phases are then brought into contact with stirring. The concentrations of the active product in each of the two phases are then carried out after thermodynamic equilibrium of the system. This concentration measurement can, for example, be carried out by direct measurement of the absorbance, if the molecule absorbs light, or by liquid chromatography. This measurement is carried out for example at 22 ° C.
• the K coefficient is then determined experimentally by the ratio of the concentration of the active ingredient in octanol to that in water.
• an emulsion according to the invention is such that the continuous fatty phase of the drops (G1) comprises at least one lipophilic (or liposoluble) active agent and the internal aqueous phase comprises at least one hydrophilic (or water-soluble) active agent. , preferably endowed with the aforementioned Log P values.
• the internal aqueous phase and / or the external aqueous phase of an emulsion according to the invention further comprises glycerin.
• the emulsions of the invention comprise at least 5% by weight of glycerin relative to the total weight of said emulsions.
• the emulsions according to the invention provide another advantage over "conventional" emulsions because they allow the use of glycerin, which is more in high contents.
• glycerin in particular comprise glycerin in a content greater than or equal to 10%, greater than or equal to 20%, greater than or equal to 30%, greater than or equal to 40%, or even up to 50%, by weight, by weight. relative to the total weight of the emulsions.
• an emulsion according to the invention is such that the continuous fatty phase of the drops (G1) further comprises at least one coloring agent (C1) and the internal aqueous phase of the drops (G2) further comprises at least one coloring agent (C1). less one coloring agent (C2), (C2) being different from (C1), in particular in terms of the color effect.
• the coloring agents (C1) and (C2) are chosen from pigments, nacres, and mixtures thereof.
• the predominantly visible color effect, or even the only visible color effect is that manifested by the drops (G1).
• the application of an emulsion according to the invention to a keratin material leads (i) to reveal the color effect of the drops (G2) and therefore (ii) to a new and unexpected color effect resulting from the mixture of coloring agents (C1) and (C2).
• an emulsion according to the invention is such that the continuous fatty phase of the drops (G1) further comprises at least one UV filter and the internal aqueous phase of the drops (G2) further comprises at least one active, in particular biological or cosmetic, different from the UV filter, and in particular an active sensitive (or unstable) to solar radiation and more particularly to UV.
• This embodiment is advantageous in that the presence of UV filters in the fatty phase of the drops (G1) makes it possible to protect the active agent present in the internal aqueous phase of the drops (G2) from the effects of solar radiation and in particular UV rays. Thus, the integrity of said asset can be preserved over even longer periods of time.
• active ingredients sensitive to solar radiation such as for example B vitamins, vitamin C, dihydroxyacetone or DHA, EUK 134 (INCI name: Ethylbisiminomethylguaiacol manganese chloride), etc ...
• an emulsion according to the invention in particular the continuous fatty phase of the drops (G1), further comprises at least one perfuming agent, the external aqueous phase and / or the internal aqueous phase, little (ven) t in further comprising at least one buffer having a pKa of 4.0 to 9.0, in particular selected from the group consisting of phosphate buffers, 2- (N-morpholino) ethane sulfonic acid, 2-amino-2 -hydroxymethyl-1,3-propanediol, 2- (bis (2-hydroxyethyl) amino) acetic acid, 4- (2-hydroxyethyl) -1 -piperazine ethanesulfonic acid, sodium citrate and mixtures thereof, preferably 4- (2-hydroxyethyl) -1 -piperazine ethanesulfonic acid.
• an emulsion according to the invention comprises from 0.1% to 10% by weight of buffer (s), preferably from 0.5% to 5% by
• the optional additional and / or active compound (s), in particular the hydrophilic gelling agents, mentioned above and / or their respective amounts in such a way that the advantageous properties of the emulsion according to the invention are not or substantially not altered by the addition envisaged.
• the nature and / or the amount of the additional and / or active compound (s) depend (s) on the aqueous or fatty nature of the phase considered of the emulsion according to the invention .
• An emulsion according to the invention can be prepared by various methods.
• an emulsion according to the invention has the advantage of being able to be prepared according to a simple "non-microfluidic" process in two stages, namely by simple emulsification, in particular using a stirring device of the Rayneri type. or a paddle shaker.
• the first step consists in preparing, at a temperature above the melting point of the gelling agents used, an inverse emulsion (E1).
• An aqueous solution and a fatty solution are prepared separately. It is the addition of the aqueous phase to the fatty phase with stirring that creates the reverse emulsion (E1).
• the second step consists in preparing, at a temperature above the melting point of the gelling agents used, in particular in the emulsion (E1), a double emulsion (E2) comprising the emulsion (E1) as the dispersed phase. It is the addition of the emulsion (E1) to the aqueous phase with stirring that creates the water-in-oil-in-water (E2) double emulsion.
• the viscosity of the external aqueous phase can be controlled, in particular, by adjusting the amount of hydrophilic gelling agent and / or the pH of the solution.
• the pH of the aqueous phase is less than 4.5, which may involve the addition of a third sodium hydroxide solution (BF) as a last step to reach a pH between 5.5 and 6, 5.
• BF sodium hydroxide solution
• the viscosity of the phases and the shear force applied to the mixtures are the two main parameters which influence the size and the monodispersity of the drops (G1) and (G2) of the emulsions (E1) and (E2).
• a person skilled in the art will know how to adjust the parameters of the non-microfluidic process in order to achieve an emulsion according to the invention and in particular to satisfy the criteria for the diameters of the drops (G1) and (G2) sought.
• An emulsion 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 (G1), or even the drops (G2), obtained by this microfluidic process advantageously have a uniform size distribution, as described above.
• the presence, in the continuous fatty phase of the drops (G1), of lipophilic gelling agent (s), or even optionally in the internal and / or external aqueous phase, of gelling agent (s) ) hydrophilic (s), may require adjustments at the level of the process for preparing an emulsion according to the invention.
• the process for preparing an emulsion 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 internal and external aqueous phases and, where appropriate, maintaining this heating (i) during stirring in the case of a “non-microfluidic” process or (ii) at the level of the microfluidic device in the case of a “microfluidic” process, until the desired emulsion is obtained.
• the process for preparing an emulsion according to the invention comprises at least the following steps: a) having at least:
• an aqueous fluid FE1 optionally at a temperature of from 50 ° C to 150 ° C;
• an aqueous fluid FE2 optionally at a temperature of from 50 ° C to 150 ° C; b) bringing the aqueous fluid FE1 into contact with the oily fluid Fl to form a water-in-oil emulsion consisting of drops (G2), said drops (G2) being formed of the aqueous fluid FE1 dispersed in a continuous fatty phase consisting of the oily fluid F1, and c) bringing the water-in-oil emulsion obtained in step b) into contact with the aqueous fluid FE2 to form the drops (G1), each drop (G1) comprising at least one, preferably at least two, in particular at least five, or even at least ten, drop (s) (G2); in which :
• the aqueous fluid FE1 comprises at least water and optionally at least one hydrophilic gelling agent, at least one active agent, and their mixture,
• the oily fluid F1 comprises at least one lipophilic gelling agent, and optionally at least one oil and / or at least one active agent, the oily fluid F1 having a melting point of between 50 ° C and 100 ° C, preferably between 60 ° C and 90 ° C, and, at ambient 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;
• the aqueous fluid FE2 comprises at least water and optionally at least one hydrophilic gelling agent, at least one active agent, and a mixture thereof.
• Steps (b) and (c) are carried out at a temperature greater than or equal to the melting point of the gelling agent (s) used.
• steps (b) and (c) are produced with an oily fluid F1 in a form capable of emulsifying with the aqueous fluid FE1 and the aqueous fluid FE2, or in other words to ensure the formation of drops (G1) and (G2), and in particular with fluids , and in particular an oily fluid F1, in liquid form.
• the aforementioned steps b) and c) are simultaneous.
• the fluid FE1 is initially prepared by mixing an aqueous phase intended to form the core of the drops (G2), comprising at least water and in addition, optionally, at least one hydrophilic gelling agent and / or at least one additional compound as mentioned above.
• the fluid F1 is initially prepared by mixing a fatty phase intended to form the heart of the drops (G1), comprising at least one lipophilic gelling agent and in addition, optionally, at least one oil and / or at least one additional compound as mentioned above.
• the FE2 fluid is initially prepared by mixing an aqueous phase intended to form the continuous phase of the emulsion with, optionally, at least one base, at least one additional compound, preservatives and / or the like.
• water-soluble products such as glycerin, and very particularly at least one hydrophilic gelling agent.
• the aqueous continuous phase of the emulsion formed comprises, or even is represented by, the aqueous fluid FE2.
• the method according to the invention may further comprise a step d) of adding a solution for increasing the viscosity of the external aqueous phase, namely fluid FE2, for example as described. in WO2015 / 055748.
• the viscosity enhancing solution is aqueous.
• This viscosity increasing solution is typically added to the aqueous fluid FE2 after formation of the drops (G1) and (G2), step d) therefore being subsequent to step c).
• the viscosity increasing solution comprises a base, in particular an alkali hydroxide, such as sodium hydroxide.
• the process for preparing an emulsion is such that:
• step b) of formation of drops (G2) can comprise the formation of drops of oily fluid FE1 at the outlet of a first duct opening into the oily fluid F1.
• the oily fluid F1 is circulated in a second duct, the outlet of the first duct opening into the second duct, advantageously coaxially with the local axis of the second duct, and
• step c) of formation of drops (G1) can comprise the formation of drops of oily fluid F1 at the outlet of the second duct opening into the aqueous fluid FE2.
• the aqueous fluid FE2 is circulated in a third duct, the outlet of the second duct opening into the third duct, advantageously coaxially with the local axis of the third duct.
• the process for preparing an emulsion is such that:
• step (b) of formation of the drops (G2) comprises the formation of drops of aqueous fluid FE1 inside a conduit opening into the aqueous fluid FE2;
• Step (c) of formation of the drops (G1) comprises the formation of drops of oily fluid F1 at the outlet of said conduit opening into the aqueous fluid FE2.
• a method of the invention can comprise, after step c) but before step d), a cooling step e) to accelerate the cooling kinetics of the emulsion formed, and thus prevent the risks of coalescence. and fragmentation of the post-formation drops (between 10 and 30 ° C).
• the microfluidic device implemented according to the invention comprises one or more of the following characteristics, taken in all technically possible combinations:
• each drop (G1) and each internal drop (s) (G2) associated (s) are formed simultaneously (in other words, the ends of the NF and MF channels are placed at the same height to generate a single drop formation step).
• This embodiment is advantageous in that it allows better control of the number of drop (s) (G2) in each drop (G1);
• the various fluids used form a multi-component drop, according to a hydrodynamic mode called “dripping”.
• the present invention also relates to an emulsion that can be obtained by a process such as those described above.
• an emulsion according to the invention can be used directly, at the end of the aforementioned preparation processes, as a composition, in particular a cosmetic.
• a composition 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, in particular after separation of the drops (G1) and redispersion of the latter in a second phase appropriate.
• the invention also relates to the use of an emulsion according to the invention for the preparation of a composition, in particular cosmetic, pharmaceutical, in nutrition or in the food industry, preferably of a cosmetic composition and in particular of a composition of care and / or make-up of a keratin material, in particular of the skin.
• the present invention thus also relates to a composition, in particular cosmetic, and in particular for caring for and / or making up a keratin material, in particular the skin, comprising at least one emulsion according to the invention, optionally in combination with at least a physiologically acceptable medium.
• compositions according to the invention can in particular be used in the cosmetics field.
• They can comprise, in addition to the aforementioned ingredients, at least one physiologically acceptable medium.
• physiologically acceptable medium is intended to denote a medium which is particularly suitable for the application of a composition of the invention to keratin materials, in particular the skin, lips, nails, eyelashes or eyebrows, and preferably the skin.
• 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 external aqueous phase as described above.
• the present invention also relates to the non-therapeutic cosmetic use of an above-mentioned cosmetic composition, as a make-up, hygiene, cleansing and / or care product for keratin materials, in particular for 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.
• an emulsion or composition according to the invention is oral or topical, preferably topical, and better still topical on a keratinous material, in particular the skin, and better still the skin of the face.
• the present invention also relates to a non-therapeutic process for the cosmetic treatment of a keratin material, in particular the skin and / or the hair, and more particularly the skin, comprising at least one step of applying to said keratin material at least one emulsion or a composition according to the invention.
• the present invention relates to a non-therapeutic process for cosmetic treatment of the skin, comprising a step of applying to the skin at least one emulsion or a composition according to the invention.
• the present invention also relates to the use of an emulsion or of a composition according to the invention, for encapsulating at least one hydrophilic compound, in particular a hydrophilic cosmetic active agent and, optionally, at least one lipophilic compound, in particular a lipophilic cosmetic active agent. .
• the present invention also relates to the use of an emulsion or of a composition according to the invention, for improving the surface appearance of the skin, in particular for moisturizing the skin and / or reducing fine lines and wrinkles.
• 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 continuous fatty phase of the G1 drops of an emulsion 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 essentially differ in the nature of the oily solvent and / or by 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 the 1 D test differs from the 1 C test by the nature of the solvent. Table 1 below shows the composition of these various anhydrous gels. Table 1
• 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 protocol for preparing these anhydrous gels is as follows.
• the solvent (Labrafac CC or DUB Inin) is stirred and heated to 80 ° C / 90 ° C depending on the gelling agent to be dispersed; the lipophilic gelling agent (ie Estogel M, Rheopearl D2 or OILKEMIA TM 5S polymer) is added thereto with magnetic stirring at 80 ° C / 90 ° C until a homogeneous solution is obtained guaranteeing good dispersion of the polymer.
• the lipophilic gelling agent ie Estogel M, Rheopearl D2 or OILKEMIA TM 5S polymer
• 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 using the EZ-X texturometer from shimadzu, whose maximum force in terms of hardness is 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 tack (y) criterion of anhydrous gels from 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 representing the cohesion criterion (z) of anhydrous gels 1B, 1D, 2B, 3B, 5 and 6 of Table 1.
• Figures 5 to 7 are graphs representing the texturometry curves of the anhydrous gels in Table 1. These Figures 5 to 7 provide the force (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) at a second relaxation stage where the mobile rises (5 to 10 s). After a rest period (10s), 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. Results:
• 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 1 C and 1 D, it is observed that the hardness is impacted by the nature of the solvent.
• thirteen emulsions are prepared comprising an external continuous aqueous phase and a water-in-oil emulsion in the form of drops (G1), each drop (G1) comprising a continuous fatty phase represented by one of the anhydrous gels of the example
• emulsions are obtained by means of a microfluidic manufacturing process as described in WO2015 / 055748.
• the microfluidic device used can be broken down into two parts, a first part where the contact between the internal aqueous phase (also called IF or FE1) and the fatty phase is carried out, hot (between 70 and 90 ° C).
• compositions of the phases (fluids) allowing the preparation of the emulsions are described in Table 3 below.
• Table 3 The compositions of the phases (fluids) allowing the preparation of the emulsions are described in Table 3 below.
• composition of the sodium hydroxide solution (BF) Table 4
• the preparation of each of the above phases fall within the general skills of those skilled in the art.
• the equipment necessary for the manufacture of the emulsions is composed of: 4 syringe pumps (one for OF, MF, IF and BF), a syringe heater (for MF), a thermostatic bath, a microfluidic device (or nozzle) fitted with concentric tracks.
• the nozzle and the pipe conveying the oily phase (MF) are placed in a thermostatic bath heated between 70 ° C and 90 ° C.
• the microfluidic device is also suitable for adding the sodium hydroxide solution (BF) after formation of the drops (G1) and (G2) in order to increase the viscosity of the OF.
• the emulsions obtained may comprise G1 drops endowed with satisfactory monodispersity and having an average diameter of between 400 ⁇ m and 1500 ⁇ m, in particular between 700 and 1300 ⁇ m.
• the emulsions obtained can comprise drops G1 comprising between 1 and 20 drops G2, or even between 5 and 10 drops G2, said drops G2 having an average diameter of between 50 ⁇ m and 200 ⁇ m, in particular between 50 and 100 ⁇ m.
• each of the thirteen emulsions is then packaged in three half-filled 30 ml polypropylene (PP) containers.
• PP polypropylene
• 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; vibrating table (i.e. vertical circular movement): Heidolph Unimax 1010 reference, for 1 hour; and 3D mixer (i.e. random movements): for 6 minutes.
• roller test i.e. horizontal circular movement
• Wheaton reference for 1 hour
• vibrating table i.e. vertical circular movement
• Heidolph Unimax 1010 reference for 1 hour
• 3D mixer i.e. random movements
• D1A water-in-oil-in-water emulsion according to Example 2 using as intermediate fatty phase the anhydrous gel 1 A of Example 1.
• the D1 A and D2A emulsions exhibit unsatisfactory stability results.
• the corresponding fatty phases are therefore excluded from the rest of the study.
• the D3A emulsion exhibits average stability results but considered satisfactory enough to be stored for further study.
• the other emulsions 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.
• x a hardness (x) of between 2 and 14 N, in particular between 2.5 and 12 N, preferably between 3 and 9 N, and better still between 4 and 6 N;
• tack (y) greater than or equal to -2 N, better still greater than or equal to -1 N, and in particular greater than or equal to -0.6 N;
• Example 3 Preparation of a macroscopic double emulsion with a gelled internal aqueous phase
• Example 3 consists in preparing a double emulsion according to the invention which differs from the D2B emulsion of example 2 above by the additional presence in IF of a thermosensitive hydrophilic gelling agent, the agar-agar present at at 0.10% by weight relative to the total weight of N F.
• this heat-sensitive gelling agent is advantageous in that it makes it possible to further strengthen the kinetic stability of the emulsion according to the invention, and in particular to further reduce the risks of transfer of compounds present in the colored internal aqueous phase to the other phases (in particular the external continuous aqueous phase), without negatively impacting the ease (or comfort) of application to the skin.

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