Microspheres of cosmetic ingredients

Abstract

The inventors have advantageously developed microspheres of cosmetic ingredient(s) having a volume diameter d(50) of between 0.5 and 20 µm, and allowing the formulation of cosmetic ingredient(s) in cosmetic compositions without temperature constraints, while preserving the efficacy and sensory properties thereof.

Description

Description Title: Microspheres of cosmetic ingredientsTechnical field

[0001] La présente divulgation relève du domaine de la formulation de compositions cosmétiques. Prior art

[0002] Les ingrédients jouent un rôle essentiel dans la formulation des produits cosmétiques que ce whether hair, hygiene, or makeup products. Each ingredient provides specific properties, contributing to the effectiveness and sensory experience of users.

[0003] Cependant, ces ingrédients cosmétiques posent des défis lors de leur formulation. Certains Some of them are sensitive to factors such as heat, pH, light, or oxygen. Others require specific reaction conditions, such as heating. Finding the right balance between formulation efficiency, raw material compatibility, and process simplification is a major challenge for cosmetic formulators.

[0004] Typiquement, les ingrédients cosmétiques qui nécessitent un chauffage du mélange reaction impose significant constraints. Indeed, this temperature increase may be incompatible with the introduction of other components into the formulation and thus risks altering the properties of heat-sensitive ingredients.

[0005] Par ailleurs, la formulation de ces ingrédients devant être chauffés peut également nécessiterthe addition of additional ingredients, either to form an emulsion or to be co-solubilized, thus complicating the formulation.

[0006] Enfin, si le chauffage n’est pas réalisé à une température adéquate pour l’ingrédient actif, des Phase separation problems between constituents may occur, altering the texture and performance of the product or resulting in non-uniform distribution of the ingredient throughout the product.

[0007] Il est donc nécessaire de mettre au point des ingrédients cosmétiques actifs qui puissent can easily be incorporated into any type of galenic, without the need for heating or only moderate heating, while preserving their properties in terms of efficacy and stability. Summary

[0008] Les inventeurs ont avantageusement mis au point des microsphères d’ingrédient(s) cosmetic(s) with a volume diameter d(50) between 0.5 and 20 µm, and allowing the formulation of cosmetic ingredient(s) in cosmetic compositions without temperature constraints, while preserving its effectiveness and its sensory properties.

[0009] Ainsi, les microsphères selon l’invention, pourront être mises en œuvre dans tout type degalenic whether solid or liquid, in varying proportions, in a fatty or aqueous phase or within a powder, without the addition of co-formulants, necessary for integration into the formula, nor a heating step. Their "ready to use" character simplifies the process of formulation. In addition, the absence of heating or the implementation of moderate heating for their formulation allows significant energy savings during the formulation processes.

[0010] De plus, les ingrédients sous forme de microsphères selon l’invention peuvent être formulés with a priori incompatible active ingredients, such as heat-sensitive active ingredients, which would otherwise be unusable in a formulation requiring a heating step.

[0011] De manière avantageuse encore, l’intégration de cette technologie au sein d’une formulationdoes not affect the integrity of the microspheres. Indeed, the inventors were able to demonstrate, for example, that an extrusion process used to formulate a solid shampoo from syndet, comprising these microspheres, does not alter their structure. After solubilization of the shampoo in water, and therefore during use of the shampoo, the microspheres remain intact.

[0012] Par ailleurs, et de manière inattendue, les inventeurs ont démontré que la formulation of cosmetic ingredient in the form of a microsphere according to the invention makes it possible to improve the properties of the cosmetic ingredient, both during its application and its cosmetic properties.

[0013] Ainsi, la présente invention concerne des microsphères d’ingrédient cosmétique, de diamètrein volume d(50) between 0.5 and 20 µm, preferably between 1 and 10 µm, and more preferably between 2 and 8 µm, the cosmetic ingredient having a melting point above 30°C and in which:- when the cosmetic ingredient is other than a wax, it represents at least 80% by mass of said microspheres, and- when the cosmetic ingredient is a wax, it represents at least 95% by mass of said microspheres.

[0014] La présente invention concerne également des microsphères de diamètre en volume d(50) between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, said microspheres comprising at least one ingredient and at least one wax, said cosmetic ingredient having a melting point above 30°C and not being a wax.

[0015] La présente invention a également pour objet un procédé de fabrication des microsphères according to the invention, said microspheres being obtained in the form of a suspension in an aqueous medium.

[0016] La présente invention a également pour objet une suspension aqueuse de microsphères.

[0017] La présente invention a donc pour objet également des microsphères, préférentiellement une suspension of microspheres capable of being obtained by a process according to the invention.

[0018] Avantageusement toujours, la forme sphérique, de granulométrie en volume d(50) comprisbetween 0.5 and 20 µm allows easy mechanical adhesion to hair from 30 µm (fine hair) to 70 µm (thick hair). The particle size / hair size ratio promotes the adhesion of the particle to the hair. This adhesion allows for better resistance to the leaching of the particles when rinsing a shampoo, for example. In fact, the ingredient will be able to settle by friction on the hair and adhere to it. The deposit is therefore uniform on the surface of the hair and resists rinsing with water.

[0019] Ainsi, la présente invention est particulièrement intéressante dans le domaine capillaire, et can also be used in the field of personal hygiene as well as makeup.

[0020] La présente invention concerne donc une composition cosmétique comprenant des microspheres according to the invention and a physiologically acceptable medium.

[0021] Enfin, les inventeurs ont comparé un shampoing solide fait à partir de syndet comprenant uncosmetic ingredient as commercially available (i.e., without being formulated in the form of microspheres) to a solid shampoo made from syndet comprising the microspheres of cosmetic ingredient according to the invention. It has been demonstrated during a consumer test that the shaping of the cosmetic ingredient in the form of microspheres makes it possible to improve its properties during its application (improvement of obtaining foam, sensoriality during application and improvement of rinsing) but also from a cosmetic point of view (improvement of detangling, protection of the hair, cleaning of shine, styling, softness, character).

[0022] Une autre étude comparative démontre clairement les bénéfices apportés par la formulationof a moisturizing active ingredient in the form of microspheres according to the invention compared to the active ingredient alone. At equal concentration (0.3%), the active ingredient in microspheres has a significantly higher moisturizing efficacy. It is particularly notable that even by tripling the concentration of the active ingredient alone (1%), it does not consistently achieve the efficacy of the active ingredient formulated according to the invention. These results confirm the substantial improvement in moisturizing efficacy provided by the microsphere technology according to the invention.

[0023] Ainsi, la présente invention a pour objet l’utilisation des microsphères selon l’invention pour improve the performance of said cosmetic ingredient. Brief description of the drawings

[0024] D’autres caractéristiques, détails et avantages apparaîtront à la lecture de la description detailed below, and to the analysis of the attached drawings, on which: Fig.1

[0025] [Fig.1] montre en microscopie optique réalisée sur microscope Paralux L110 S2 Trino 1600X equipped with a DinoEye eyepiece camera, a microsphere according to the invention of the Cosmegreen surfactant on a hair fiber. Fig.2

[0026] [Fig.2] montre en microscopie optique réalisée sur microscope Paralux L110 S2 Trino 1600Xequipped with a DinoEye eye camera, the clusters of the Cosmegreen surfactant when formulated in its commercial form in a solid shampoo.

[0027] [Fig.3] montre en microscopie optique réalisée sur microscope Paralux L110 S2 Trino 1600X equipped with a DinoEye eyepiece camera, the presence of Cosmegreen microspheres after solubilization of the solid shampoo in water. Fig.4

[0028] [Fig.4] montre en microscopie optique réalisée sur microscope Paralux L110 S2 Trino 1600X equipped with a DinoEye eye camera, the presence of Cosmegreen microspheres on a hair before rinsing. Fig.5

[0029] [Fig.5] montre, en microscopie optique réalisée sur microscope Paralux L110 S2 Trino 1600X equipped with a DinoEye eye camera, the presence of Cosmegreen microspheres on a hair after rinsing. Fig.6

[0030] [Fig. 6] est un graphique illustrant l’évolution de l'hydratation cutanée après applications repeated – Evaluation of the moisturizing effect of an active ingredient in the form of microspheres according to the invention (n=4). Fig.7

[0031] [Fig.7] représente la comparaison de l'efficacité hydratante entre l'actif sous forme de microspheres according to the invention and the active ingredient alone at different concentrations (Figure 7A, comparison at equal concentration, Figure 7B, comparison with tripled concentration of the active ingredient alone). Detailed description

[0032] Microsphères d’ingrédient cosmétique

[0033] Selon un mode de réalisation, la présente invention concerne des microsphères d’ingrédientcosmetic, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, more preferably between 2 and 8 µm, the cosmetic ingredient having a melting point above 30°C, and in which: - when the cosmetic ingredient is other than a wax, it represents at least 80% by mass of said microspheres, and - when the cosmetic ingredient is a wax, it represents at least 95% by mass of said microspheres.

[0034] Selon ce mode de réalisation, chaque microsphère d’ingrédient cosmétique est composée mostly cosmetic ingredient, whether it is a wax or not.

[0035] L’ingrédient cosmétique est différent d’une cire

[0036] Selon un mode de réalisation, la présente invention concerne des microsphères d’ingrédient cosmetic, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, preferably between 2 and 8 µm, preferably between 2 and 5 µm, said cosmetic ingredient having a melting point above 30°C and being different from a wax, and representing at least 80% by mass of said microspheres.

[0037] Lorsque l’ingrédient cosmétique est différent d’une cire, on entend par microsphèrecomposed mainly of the cosmetic ingredient, a microsphere composed of at least 80% by mass of said cosmetic ingredient, relative to the total mass of the microsphere, preferably at least 81%, preferably at least 82%, preferably at least 83%, preferably at least 84%, preferably at least 85%, preferably at least 86%, preferably at least 87%, preferably at least 88%, preferably at least 89% by mass of said cosmetic ingredient, preferably at least 90% by mass, relative to the total mass of the microsphere, preferably at least 91%, preferably at least 92%, preferably at least 93%, preferably at least 94%, preferably at least 95%, preferably at least 96%, preferably at least 97%, preferably at least 98%, preferably at least 99% by mass of said cosmetic ingredient, relative to the total mass of the microsphere.Preferably again, the microsphere is composed of 100% by mass of said cosmetic ingredient, relative to the total mass of the microsphere.

[0038] Selon un mode de réalisation, l’ingrédient cosmétique peut être un mélange d’ingrédient cosmetic, each cosmetic ingredient having a melting point above 30°C and each cosmetic ingredient not being a wax.

[0039] Selon ce mode de réalisation, les microsphères d’ingrédient cosmétique ne comprennent pas of waxes.

[0040] La microsphère d’ingrédient cosmétique peut comprendre de manière minoritaire, un ou several of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process. They are to be distinguished from the cosmetic ingredient(s) forming the microsphere.

[0041] Ainsi, selon ce mode de réalisation, chaque microsphère d’ingrédient cosmétique comprenda content of less than 20% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere, preferably, a content of less than 19%, preferably less than 18%, preferably less than 17%, preferably less than 16%, preferably less than 15%, preferably less than 14%, preferably less than 13%, preferably less than 12%, preferably less than 11% by mass, preferably less than 10% by mass, relative to the total mass of the microsphere, preferably, a content of less than 9%, preferably less than 8%, preferably less than 7%, preferably less than 6%, preferably less than 5%, preferably less than 4%, preferably less than 3%, preferably less than 2%, preferably less than 1% by mass of at least one surfactant and / or at least one colloid ... minus one colloid,relative to the total mass of the microsphere.,

[0042] Ainsi, selon ce mode de réalisation, chaque microsphère est composée d’au moins un cosmetic ingredient which is not a wax, and possibly at least one surfactant and / or least one colloid. This means that each microsphere does not contain any amphiphilic product, waxes, stabilizer or other additives that are not the cosmetic ingredient or a mixture of cosmetic ingredients and possibly one or more surfactants and / or colloids.

[0043] Selon un mode de réalisation, chaque microsphère pourra comprendre en outre, un actif qui is not a cosmetic ingredient within the meaning of the present invention and which is chosen from a vegetable oil or a sunscreen. According to this embodiment, each cosmetic ingredient microsphere comprises an active ingredient content of between 0 and 20%, preferably between 1 and 15%, preferably between 2 and 10%.

[0044] Lorsque l’ingrédient cosmétique est une cire

[0045] Selon un mode de réalisation, la présente invention concerne des microsphères d’ingrédientcosmetic, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, more preferably between 2 and 8 µm, said ingredient being a wax, and represents at least 95% by mass of said microspheres.

[0046] Lorsque l’ingrédient cosmétique est une cire, on entend par microsphère composée predominantly of the cosmetic ingredient, a microsphere composed of at least 95% by mass of said cosmetic ingredient, relative to the total mass of the microsphere, preferably at least 96%, preferably at least 97%, preferably at least 98%, preferably at least 99% by mass of said cosmetic ingredient, relative to the total mass of the microsphere. Preferably again, the microsphere is composed of 100% by mass of said cosmetic ingredient, relative to the total mass of the microsphere.

[0047] Selon un mode de réalisation, l’ingrédient cosmétique peut être un mélange de cires.

[0048] La microsphère d’ingrédient cosmétique peut comprendre de manière minoritaire, un ou several of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process.

[0049] Ainsi, selon ce mode de réalisation, chaque microsphère d’ingrédient cosmétique comprenda content of less than 5% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere, preferably less than 4%, preferably less than 3%, preferably less than 2%, preferably less than 1% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere.

[0050] Ainsi, selon ce mode de réalisation, chaque microsphère est composée d’au moins un cosmetic ingredient which is a wax, and possibly at least one surfactant and / or at least one colloid. This means that each microsphere does not contain any amphiphilic product, destabilizer or other additives which are not a wax or a mixture of waxes and possibly one or more surfactants and / or colloids.

[0051] Les microsphères selon l’invention, que l’ingrédient cosmétique soit une cire ou non, ne sont not microspheres composed of a core of active material and a coating, i.e., the microspheres according to the invention do not have a core-shell structure.

[0052] En effet, les microsphères d’ingrédient cosmétique selon l’invention sont pleines et le ou lescosmetic ingredients, are distributed over the entire volume of the microsphere, including its periphery, without distinction between core and shell. In other words, the cosmetic ingredient(s) are present both at the periphery and in the volume of the microsphere. Preferably, the cosmetic ingredient(s) are distributed uniformly over the entire volume of the microsphere, including its periphery.

[0053] Lorsque les microsphères d’ingrédient cosmétique comprennent de manière minoritaire unor more of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process (and not surfactants qualified as cosmetic ingredients within the meaning of the present invention), the liposoluble surfactants will be equally distributed over the entire volume of the microsphere including its periphery, without distinction between core and shell. The water-soluble surfactants and the colloids will be present at the periphery and / or at the interface. However, and even in the presence in a minority manner of one or more of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process, the microspheres do not have a core / shell structure.

[0054] Ainsi, selon un mode de réalisation, les microsphères ne présentent pas une structureheart / bark. According to one embodiment, each microsphere may further comprise an active ingredient which is not a cosmetic ingredient within the meaning of the present invention and which is chosen from a vegetable oil or a sunscreen. According to this embodiment, each cosmetic ingredient microsphere comprises an active ingredient content of between 0 and 5%, preferably between 1 and 4%, preferably between 2 and 3%.

[0055] Microsphères d’ingrédient cosmétique et de cire

[0056] Selon un autre mode de réalisation, chaque microsphère comprend au moins une cire et au at least one cosmetic ingredient, said at least one cosmetic ingredient having a melting point above 30°C and not being a wax.

[0057] Ainsi, la présente invention concerne également des microsphères, de diamètre en volume d(50) between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient and at least one wax, said cosmetic ingredient having a melting point above 30°C and is different from a wax.

[0058] De la même façon que précédemment, chaque microsphère peut comprendre de manièreminority, one or more of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process. They are to be distinguished from the cosmetic ingredient(s) forming the microsphere.

[0059] Ainsi, selon un mode de réalisation, une microsphère comprend une teneur inférieure à 20% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere, preferably, a content of less than 19%, preferably less than 18%, preferably less than 17%, preferably less than 16%, preferably less than 15%, preferably less than 14%, preferably less than 13%, preferably less than 12%, preferably less than 11% by mass, preferably less than 10% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere, preferably, a content of less than 9%, preferably less than 8%, preferably less than 7%, preferably less than 6%, preferably less than 5%, preferably less than 4%, preferably less than 3%, preferably less than 2%, preferably less than 1% by mass of at least one surfactant and / or at least one colloid, relative to the total mass of the microsphere.

[0060] Selon un mode de réalisation, chaque microsphère comprend de 1 à 10% en masse d’auat least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 90 to 99% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0061] Selon un mode de réalisation, chaque microsphère comprend de 10 à 20% en masse d’au at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 80 to 90% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0062] Selon un mode de réalisation, chaque microsphère comprend de 20 à 30% en masse d’au at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 70 to 80% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0063] Selon un mode de réalisation, chaque microsphère est composée de 30 à 40% en masse of at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 70 to 80% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0064] Selon un mode de réalisation, chaque microsphère est composée de 40 à 50% en masseof at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 50 to 60% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0065] Selon un mode de réalisation, chaque microsphère est composée de 50 à 60% en masse of at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 40 to 50% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0066] Selon un mode de réalisation, chaque microsphère est composée de 60 à 70% en masse of at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 30 to 40% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0067] Selon un mode de réalisation, chaque microsphère est composée de 70 à 80% en masse of at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 20 to 30% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0068] Selon un mode de réalisation, chaque microsphère est composée de 80 à 90% en masseof at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 20 to 10% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0069] Selon un mode de réalisation, chaque microsphère est composée de 90 à 99% en masse of at least one cosmetic ingredient having a melting point above 30°C and not being a wax, from 1 to 10% by mass of at least one wax and from 0 to 20% by mass of at least one surfactant and / or at least one colloid.

[0070] Selon ce mode de réalisation, chaque microsphère est composée d’au moins un ingrédient cosmetic having a melting point above 30°C and which is not a wax, at least one wax and optionally at least one surfactant and / or at least one colloid. This means that each microsphere does not contain an amphiphilic product, stabilizer or other additives which are not the wax or a mixture of waxes, the cosmetic ingredient or a mixture of cosmetic ingredients and optionally one or more surfactants and / or colloids.

[0071] Les microsphères selon l’invention ne sont pas des microsphères composées d’un cœur deactive material and a coating, i.e., the microspheres according to the invention do not have a core-shell structure.

[0072] En effet, les microsphères d’ingrédient cosmétique selon l’invention sont pleines et le ou les cosmetic ingredients, the wax(es) and any colloids or surfactants, are distributed over the entire volume of the microsphere, including its periphery, without distinction between core and shell. In other words, the cosmetic ingredient(s), the wax(es) are present both at the periphery and in the volume of the microsphere. Thus, and preferably, the cosmetic ingredient(s), the wax(es) are distributed uniformly over the entire volume of the microsphere, including its periphery.

[0073] Lorsque les microsphères d’ingrédient cosmétique comprennent de manière minoritaire unor more of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process (and not surfactants qualified as cosmetic ingredients within the meaning of the present invention), the liposoluble surfactants will be equally distributed over the entire volume of the microsphere including its periphery, without distinction between core and shell. The water-soluble surfactants and the colloids will be present at the periphery and / or at the interface. However, and even in the presence in a minority manner of one or more of the surfactants and / or one or more of the colloids used during the microsphere manufacturing process, the microspheres do not have a core / shell structure.

[0074] Selon un mode de réalisation, chaque microsphère pourra comprendre en outre, un actif quiis not a cosmetic ingredient within the meaning of the present invention and which is chosen from a vegetable oil or a sunscreen. According to this embodiment, each microsphere of cosmetic ingredient comprises an active ingredient content of between 0 and 5%, preferably between 1 and 4%, preferably between 2 and 3%.

[0075] Les microsphères selon l’invention sont à distinguer de particules décrites dans l’art antérieur.A particle, in general, refers to a fragment of matter such as a cosmetic ingredient having finite dimensions and any shape. It is a generic term that encompasses any small body, whether regular or irregular, natural or manufactured, without any particular specification regarding its internal structure or composition. Particles can be obtained by various processes, such as fragmentation, precipitation, crystallization or agglomeration, and can have very different characteristics in terms of shape, size, density and structural organization. They can be homogeneous or heterogeneous, solid or hollow, smooth or rough, and their composition can be uniform or layered.

[0076] Cette définition générale s'oppose fondamentalement aux microsphères telles que définiesin the present invention, which have specific structural and compositional characteristics: they are solid, spherical in shape, and the ingredient is distributed uniformly over their entire volume, including at the periphery, without distinction between a core and a shell. This particular structural organization and this homogeneous distribution constitute important distinctive characteristics which differentiate the microspheres from a simple particle, the latter not necessarily implying such a defined internal organization.

[0077] Distribution granulométrique en volume

[0078] Le diamètre en volume d(50) se réfère au diamètre médian de particules dans la distribution granulometric. According to the commonly accepted definition, the median diameter corresponds to the theoretical opening of a sieve such that 50% of the particles, by volume, have a diameter greater than and 50% a diameter less than d(50).

[0079] Le diamètre en volume d(50) est mesuré par granulométrie par diffraction laser. Pour cela,The sample to be analyzed is first diluted in water with the addition of a non-ionic dispersant. An optical microscopy observation is carried out beforehand to ensure the deagglomeration of the particles. The measurement is carried out on a Fritsch Analysette 22 NeXT Nano granulometer with an obscuration of between 5 and 15%. The results are interpreted using Mie theory.

[0080] Selon un mode de réalisation, le diamètre en volume d(50) est compris entre 1 et 10µm et de preferably, between 2 and 8 µm, and even more preferably between 2 and 7 µm. This embodiment is particularly advantageous in hair applications.

[0081] Selon un mode de réalisation, et lorsque l’ingrédient cosmétique est le Cosmegreen, les diameters d(10) and d(90), also measured by laser diffraction granulometry, are as follows:- diameter d(10) is between 0.1 and 2.5µm, preferably less than 1µm- diameter d(90) is between 8 and 20 µm, preferably less than 10 µm.

[0082] Les termes d(10) et d(90) font également référence à des paramètres dans la distributiongranulometric. D(10) corresponds to the theoretical opening of a sieve such that 10% of the particles, by volume, have a diameter less than d(10), and that d(90) corresponds to the theoretical opening of a sieve such that 90% of the particles, by volume, have a diameter less than d(90).

[0083] Ingrédient cosmétique

[0084] Les microsphères pourront être composées d’un seul et même ingrédient ou d’un mélange of two or more ingredients.

[0085] Selon un mode de réalisation, l’ingrédient cosmétique selon l’invention possède un point de melting above 30°C and is not a wax.

[0086] Préférentiellement, l’ingrédient cosmétique possède un point de fusion supérieur à 40°C, preferably greater than 50°C, preferably greater than 60°C, preferably greater than 70°C, preferably greater than 73°C.

[0087] Le point de fusion sera mesuré par toute technique connue de l’homme du métier.

[0088] De façon générale, le point de fusion de l’ingrédient cosmétique peut être mesuré à l’aide a differential scanning calorimeter (DS C), for example the calorimeter sold under the name DSC 30 by the METTLER Company.

[0089] Selon un mode de réalisation, l’ingrédient cosmétique n’est pas hydrosoluble.

[0090] Lorsque l’ingrédient cosmétique possède un point de fusion supérieur à 30°C et n’est pas a wax, the cosmetic ingredient is chosen from surfactants, butters, oils and their mixtures, preferably surfactants and mixtures of at least one butter and at least one oil.

[0091] Tensioactifs

[0092] Selon un mode de réalisation, l’ingrédient cosmétique est un tensioactif. Préférentiellement,the surfactant is an anionic or cationic surfactant, and preferably still a cationic surfactant.

[0093] Selon un mode de réalisation préféré, le tensioactif est choisi parmi les dérivés de glycine betaine, Cetrimonium chloride, Behenoyl PG-Trimonium chloride, Polyglyceryl-10Stearate, Distearoylethyl Hydroxyethylmonium Methosulfate, Cetearyl Alcohol, Distearoylethyl Dimonium Chloride, Distearoylethyl Dimonium Chloride Cetearyl Alcohol, Behentrimonium Methosulfate, BrassicylIsoleucinateEsylate(and) Brassica Alcoholand mixtures thereof

[0094] Selon un mode de réalisation, le tensioactif est choisi parmi les dérivés de glycine bétaïne, le Distearoylethyl Dimonium Chloride Cetearyl Alcohol, Brassicyl Isoleucinate Esylate (and) Brassica Alcohol and mixtures thereof. Glycine betaine derivatives are described in application FR3099058.

[0095] Selon un mode de réalisation, les dérivés de glycine bétaïne sont des sels d’ester ou d’amide glycine betaine containing 14 to 24 carbon atoms.

[0096] Selon un mode de réalisation, les dérivés de glycine bétaïne sont de formule[Chem 1]Xn-[(CH3)3N+-CH2-COZ-R]n where: Z denotes an oxygen atom or an -NH group, R is a linear or branched, saturated or unsaturated alkyl group comprising from 14 to 24 carbon atoms, preferably, the radical R is chosen from the groups myristyl (C14:0), cetyl (C16:0), palmitoleyl (C16:1), stearyl (C18:0), oleyl (C18:1), linoleyl (C18:2), linolenyl (C18:3), arachidyl (C20:0), arachidonyl (C20:4), behenyl (C22:0), 2-hexyldecyl, 2-octyldodecyl and 2-decyltetradecyl, and preferably the radical R is chosen from the groups arachidyl (C20:0) or behenyl (C22:0).X is an organic or inorganic anion, preferably, the anion X is chosen from a chloride, a sulfate, a perchlorate, an alkyl sulfate ion, in particular decyl sulfate or lauryl sulfate, an arylsulfonate ion, in particular benzene sulfonate, paratoluene sulfonate, an alkylsulfonate ion, in particular triflate, methanesulfonate, ethanesulfonate, decylsulfonate, laurylsulfonate, camphorsulfonate, or a sulfosuccinate ion, preferably from alkylsulfonates and arylsulfonates, more particularly from methanesulfonate, triflate, paratoluenesulfonate and camphorsulfonate ions, better still, X is the methanesulfonate ion. and n is 1 or 2.

[0097] Selon un mode de réalisation les dérivés de glycine bétaïne sont sous forme d’unecomposition comprising:(a) at least one glycine betaine ester salt of formula [Chem 2]Xn-[(CH3)3N+-CH2-COO-R]n where R is a linear or branched, saturated or unsaturated alkyl group comprising from 14 to 24 carbon atoms and preferably from 18 to 22 carbon atoms, (b) at least one fatty alcohol of formula R-OH, (c) an organic or inorganic acid of formula XH, and (d) a glycine betaine salt of formula [Chem 3] X n -[(CH3)3N + -CH2-COOH]n, where X is an organic or inorganic anion and n is 1 or 2.

[0098] Selon ce mode de réalisation, les dérivés de glycine bétaïne sous forme de composition contains: (a) from 15 to 45% by weight, preferably from 20 to 30%, more preferably from 25 to 30% by weight, of glycine betaine ester salt, (b) from 55 to 70% by weight, for example from 60 to 65% or from 65 to 70% by weight, of fatty alcohol, (c) from 0 to 5% by weight, for example from 0 to 1% by weight of organic or inorganic acid, (d) from 0 to 3% by weight, for example from 0 to 1% by weight, of glycine betaine salt, (e) from 0 to 15% by weight, for example from 2 to 10% by weight, of dialkyl ether.

[0099] Selon un mode de réalisation, les dérivés de glycine bétaïne sont sous forme d’une composition comprising:(a) one or more glycine betaine amide salt(s) of formula [Chem 4] X n -[(CH3)3N + -CH2-CONH-R]n where R is a linear or branched, saturated or unsaturated alkyl group comprising from 14 to 24 carbon atoms and preferably from 16 to 22 carbon atoms; (b) one or more alkylammonium salt(s) of formula [Chem 5]Xn- [NH3+R]n where R is a linear or branched, saturated or unsaturated alkyl group comprising from 14 to 24 carbon atoms and preferably from 16 to 22 carbon atoms; (c) one or more glycine betaine ester salts of formula [Chem 6] X n -[(CH3)3N + -CH2-COOR']n where R' is a linear or branched, saturated or unsaturated alkyl radical containing from 4 to 8 carbon atoms; and (d) glycine betaine of formula [Chem 7] (CH3)3N+ -CH2-COO-; where X is an organic or inorganic anion and n is 1 or 2.

[0100] A titre illustratif, les dérivés de glycine bétaïne tels que ci-avant définis sont le CosmeGreen™ ES1822+ and CosmeGreen™ MB1618 marketed by the company SurfactGreen. These cationic surfactants are in the form of granules and correspond, in the present application, to the name “Cosmegreen” or “Cosmegreen in its commercial form”, i.e., in the form of granules and not in the form of microspheres according to the present invention.

[0101] Beurres

[0102] On entend par « beurre »,un composé lipophile, solide à température ambiante (25°C), à reversible solid / liquid state change, either by melting, glass transition or softening between 25°C and 40°C.

[0103] On entend par « solide » un objet caractérisé à l'échelle macroscopique par un volume et une determined forms, constant in the absence of any external force or extreme condition.

[0104] Parmi les beurres, on citera le beurre de karité, le beurre de mangue, le beurre de cacao, le cupuaçu butter, pracaxi butter, murumuru butter, Shorea robusta butter (Sal Butter).

[0105] Huiles

[0106] Par « huile », on entend un composé lipophile, liquide à température ambiante (25°C), composed mainly of triglycerides or esters, with varying degrees of viscosity, which does not undergo no phase transition to solid state under normal atmospheric pressure until cooled below 25°C. Oils provide immediate and penetrating emollient effects.

[0107] Dans un mode de réalisation, l'huile est sélectionnée parmi les huiles naturelles telles que les vegetable oils, mineral oils, synthetic oils and their mixtures.

[0108] Huiles naturelles :

[0109] Les huiles naturelles sont dérivées de diverses parties des plantes, y compris les graines, les nuts and fruits.

[0110] Les huiles naturelles peuvent être choisies parmi l’Huile de lin (huile riche en omega 3), lesoils extracted from microalgae such as Schizochytium sp. Oil. (DHA rich oil), Argan Oil, Almond Oil, Avocado Oil, Jojoba Oil, Coconut Oil, Olive Oil, Grape Seed Oil, Sunflower Oil, Rosehip Oil, Evening Primrose Oil, Marula Oil, Macadamia Oil, Hemp Oil, Sea Buckthorn Oil, Camellia Oil, Pomegranate Seed Oil, Safflower Oil, Castor Oil, Baobab Oil, Moringa Oil, Meadowfoam Seed Oil, Neem Oil, Tamanu Oil, Black Cumin Seed Oil, Walnut Oil Kukui, Camelina Oil, Chia Oil, Borage Oil, Olive Squalane and their blends.

[0111] Huiles minérales :

[0112] Les huiles minérales sont dérivées du pétrole et sont hautement raffinées pour un usage cosmetic.

[0113] Des exemples courants d'ingrédients d'origine minérale utilisés dans les formulations Cosmetics include Mineral Oil, Petrolatum, Paraffin Oil, and Polyisobutene.

[0114] Huiles synthétiques :

[0115] Les huiles synthétiques peuvent être des huiles de silicone, des huiles d'ester ou des huiles of hydrocarbons.

[0116] Les huiles de silicone peuvent être choisies parmi la Diméthicone (Polydiméthylsiloxane), laCyclopentasiloxane (Decamethylcyclopentasiloxane), Phenyl Trimethicone (Trimethylsiloxyphenyl Dimethicone), Isopropyl Myristate, Hydrogenated Polyisobutene, Polyisobutene, Ethylhexyl Palmitate, Caprylic / Capric Triglyceride, C12-15 Alkyl Benzoate, Pentaerythrityl Tetraisostearate, Isododecane, Squalane (Synthetic), Octyldodecanol, Isopropyl Palmitate, Tridecyl Trimellitate, Diisostearyl Malate, Isononyl Isononanoate, Neopentyl Glycol Diheptanoate, Diisopropyl Sebacate, Triethylhexanoin, and PPG-15 Stearyl Ether Dicaprylyl Carbonate, Dicaprylyl Carbonate, C13-14 Isoparaffin, Cetearyl Ethylhexanoate, Isostearyl Isostearate, Lauryl Lactate, Cetyl Ethylhexanoate, Octyldodecyl Neopentanoate, Lauryl Methacrylate / Glycol Dimethacrylate Crosspolymer, PPG-3 Benzyl Ether Myristate, C18-21 Alkane, Cetearyl Isononanoate,Hydrogenated Polydecene, Polydecene, Methyl Trimethicone, Dimethiconol, Alkyl Benzoate (and) Propanediol Dicaprylate / Dicaprate, Isostearate, Isocetyl Stearoyl Triglyceride (Caprylic / Capric / Myristic / Stearic), Diisopropyl Dimer Dilinoleate, Caprylic / Capric / Succinic Triglyceride, PPG-20 Methyl Glucose Ether, and mixtures thereof.

[0117] Selon un mode de réalisation préféré, l’huile est choisie parmi l’Huile de lin (huile riche en omega 3), oils extracted from microalgae such as Schizochytium sp. Oil (DHA-rich oil) and their mixtures.

[0118] Mélanges

[0119] Selon un mode de réalisation, l’ingrédient cosmétique est choisi parmi les tensioactifs, preferentially cationic and anionic, butters, oils and their mixtures.

[0120] Dans ce contexte, l'expression "et leurs mélanges" signifie que l'ingrédient cosmétique peutbe made up not only of a single type of compound among those mentioned (cationic or anionic surfactants, butters, oils), but also of a combination of several of these compounds. For example, a cosmetic formulation could contain both surfactants and oils, or a mixture of different types of butters and oils.

[0121] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi les tensioactifs cationic.

[0122] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi les tensioactifs anionic.

[0123] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi les beurres.

[0124] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi les huiles.

[0125] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants and anionic surfactants.

[0126] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants and butters.

[0127] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants and oils.

[0128] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de anionic surfactants and butters.

[0129] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de anionic surfactants and oils.

[0130] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de beurres and oils.

[0131] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants, anionic surfactants and butters.

[0132] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants, anionic surfactants and oils.

[0133] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants, butters and oils.

[0134] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange deanionic surfactants, butters and oils.

[0135] Selon un mode de réalisation, l'ingrédient cosmétique est choisi parmi un mélange de cationic surfactants, anionic surfactants, butters and oils.

[0136] Selon un mode de réalisation, l’ingrédient cosmétique est choisi parmi un mélange d’huile et butter, and more specifically a mixture of sunflower oil, shea butter and an oily macerate of Aloe Vera.

[0137] Cires

[0138] Par « cire », on entend un composé lipophile, solide à température ambiante (25°C), à reversible solid / liquid state change, either by melting, glass transition or by softening between 40°C and 120°C.

[0139] Selon un mode de réalisation les cires ont un point de fusion supérieur à 40 °C.

[0140] Selon un mode de réalisation, les cires ont un point de fusion inférieur à 70°C.

[0141] Selon un mode de réalisation, les cires ont un point de fusion compris entre 40°C et strictly less than 70°C.

[0142] Selon un mode de réalisation, les cires peuvent être choisies parmi (i) les cires hydrocarbons, optionally substituted, in particular hydroxylated, (ii) fluorinated waxes, (iii) silicone waxes and their mixtures.

[0143] Parmi les cires hydrocarbonées, on peut citer les cires hydrocarbonées dont le point de fusion is advantageously greater than 40°C, for example greater than 55°C.

[0144] De façon générale, le point de fusion de la cire peut être mesuré à l’aide d’un calorimètre à differential scanning (DS C), for example the calorimeter sold under the name DSC 30 by the METTLER Company.

[0145] En tant que cires hydrocarbonées, on peut citer par exemple les cires hydrocarbonéeslinear or esters of primary, secondary or tertiary fatty acids. Hydrocarbon waxes can be chosen from linear hydrocarbon waxes. Examples of linear hydrocarbon waxes include: substituted linear alkanes, unsubstituted linear alkanes, unsubstituted linear alkenes, substituted linear alkenes. An unsubstituted compound is composed only of carbon and hydrogen and the substituents do not contain carbon atoms. Linear hydrocarbon waxes include linear paraffin waxes, such as S&P® 206, S&P® 173 and S&P® 434 paraffins from Strahl & Pitsch.

[0146] Les cires hydrocarbonées peuvent être choisies parmi les esters d’acides gras, saturés ou unsaturated, or derived from unsaturated fatty acids that have been previously hydrogenated to become saturated.

[0147] La cire peut ainsi être choisie parmi les esters :- capric acid (C10), lauric acid (C12), myristic acid (C14), palmitic acid (C16), stearic acid (C18), arachidic acid (C20), palmitoleic acid (C16), oleic acid (C18), linoleic acid (C18), linolenic acid (C18), arachidonic acid (C20); and- fatty alcohols, primary, secondary (such as ethylene glycol) or tertiary (such as glycerol), C2 to C22, advantageously C6 to C18, - ricinoleic acid (C18) or hydrogenated ricinoleic acid;- fatty alcohols, primary, secondary (such as ethylene glycol) or tertiary (such as glycerol), C2 to C22, advantageously C6 to C22, better still C16 to C22 and mixtures thereof.

[0148] Ces esters présentent des points de fusion qui peuvent varier en fonction de l’alcool incorporé from 23°C to 85°C. The waxes selected according to the present invention will be those having a melting point above 40°C.

[0149] On peut citer les esters (i) d’acide myristique et d’éthylène glycol ou de glycérol (ii) d’acidestearic acid and primary and linear C6 fatty alcohols or ethylene glycol or glycerol, (iii) esters of stearic acid and primary and linear C8 fatty alcohols, (iv) esters of stearic acid and primary and linear C10 fatty alcohols, (v) esters of stearic acid and primary and linear C12 fatty alcohols, (vi) esters of stearic acid and primary and linear C14 fatty alcohols, (vii) esters of stearic acid and primary and linear C16 fatty alcohols, (viii) esters of stearic acid and primary and linear C18 fatty alcohols, (ix) esters of ricinoleic acid, hydrogenated or not, and primary and linear C16 fatty alcohols or ethylene glycol or glycerol, (x) esters of ricinoleic acid, hydrogenated or not, and primary and linear C18 fatty alcohols and (xi) esters of ricinoleic acid, hydrogenated or not, and primary and linear C22 fatty alcohols.

[0150] Selon un mode de réalisation, la cire est choisie parmi les esters d’acide myristique etof ethylene glycol or glycerol, esters of stearic acid and primary and linear C18 fatty alcohols or of ethylene glycol or glycerol, esters of ricinoleic acid, hydrogenated or not, and primary and linear C22 fatty alcohols or of ethylene glycol or glycerol, hydrogenated palm oil. Advantageously, mention may be made of glycerol tristearate and glycerol trimyristate.

[0151] On peut citer l’ester d’acide stéarique et d’alcool gras primaire et linéaire en C16 avec une Tf between 52 and 57°C, the ester of stearic acid and primary and linear C18 fatty alcohol with a Tm between 54 and 60°C, the esters of hydrogenated ricinoleic acid and primary and linear C16 fatty alcohols with a Tm between 62 and 66°C, the esters of hydrogenated ricinoleic acid and primary and linear fatty alcohols linear C18 with a Tm between 67 and 71°C, the esters of hydrogenated ricinoleic acid and primary and linear C22 fatty alcohols with a Tm between 71 and 75°C.

[0152] On pourra citer cires particulièrement avantageuses pour l’invention les cires du tableau 1 below :

[0153] [Tableau 1]Name Chemical name INCI Chemical name Number as or description CAS Hydrogenated Castor 22L73 Castor oil - Behenyl esters Hydrogenated Castor oil hydrogenated Castor oil 16L64 castor oil cetyl esters Dynasan 118 Tristearin2,3-di(octadecanoyloxy)propyl 555-43- octadecenoate, C57H110O6 1 Hydrogenated Olive 18L.57 olive oilHydrogenated olive oil cetearyl esters Hydrogenated Olive 10L.40 olive oil Hydrogenated olive oil decyl esters68514- Dynasan P60F 74-9 / Hydrogenated 8033- PaHydrogenated palm oil (29-2 Vegetable oil lm Hydrogenated oil Softisan 154 Shellac SSB 63 Shellac Shellac9000- 59-3 1,3-di(tetradecanoyloxy)propan-2-yl Dynasan 114 Trimyristintetradecanoate 555-45- (Glycerol trimyristate),C45H86O6 3 L ipoxol 6000 PEG-135 Polyethylene glycol,HO- 25322- (CH2CH2O)135-H 68-3 CoperniciaWax from Ca8015- cerifera cera rnauba 86-9 EUPHORBIA CERIFERA 8006 or Can Wax- C ERA dellila44-8 Candelilla wax Cera alba Cire d'abeille8012- 89-3 Octadecanoic ac Imwitor 960 K Glyceryl id, reaction produc 11099- Stearate SE ts with 1,2,3-propanetriol (1:1), neutralized 07-3 Glycéryl monostearate, Imwitor 49 Glyceryl Octadecanoic acid, 31566- stearate monoester with 1,2,3-propanetriol, 31-1 C21H42O4 Oryza Sativa Cera / Oryza Sative Bran Cire de riz Wax Huile de coco hydrogenate Macadamia Integrifolia Wax Cire de macadamia Rhus Succedanea Cire de Sumac Fruit Cera Rhus Verniciflua Peel Cera Cire de baies de SumacHydrogenated jojoba wax ou hydrogenated Huile de jojoba hydrogénée jojoba oil Hydrogenated sunflower seed Huile de tournesol hydrogénée oil Helianthus Annuus Seed Cire de tournesol cera Citrus Aurantium Dulcis Peel Cire d'écorce d'orange Cera Acacia Decurrens Cire de mimosa Flower Cera Jasminum Grandiflorum Cire de jasmin Flower Cera Rosa Damascena Cire de rose de Damas Flower Cera Myrica Pubescens Fruit Cire de baie de Myrica Cera Camellia Sinensis Leaf Cire de feuilles de thé vert Wax Lanolin Cera Cire de lanoline

[0154] Selon un mode de réalisation, les cires sont choisies parmi l’huile de ricin hydrogénée, le 2,3-di(octadecanoyloxy)propyloctadecenoate, hydrogenated olive oil, hydrogenated palm oil, shellac, 1,3-di(tetradecanoyloxy)propan-2-yl, carnauba wax, candelilla wax, beeswax, Glyceryl Stearate SE, Glyceryl Stearate, rice wax, hydrogenated coconut oil, macadamia ternifolia wax, sumac wax, sumac berry wax, hydrogenated jojoba oil, hydrogenated sunflower oil, sunflower wax, orange peel wax, mimosa wax, jasmine wax, rose damascena wax, myrica berry wax, green tea leaf wax, lanolin wax, and mixtures thereof.

[0155] Selon un mode de réalisation, les cires sont choisies parmi l’huile d’olive hydrogénée, l’huile hydrogenated castor oil, 2,3-di(octadecanoyloxy)propyloctadecenoate, rice wax, macadamia wax, candelilla wax, carnauba wax, hydrogenated jojoba oil, and mixtures thereof.

[0156] Selon un mode de réalisation préférée, les cires sont choisies parmi l’huile d’olive hydrogénée and hydrogenated castor oil, and mixtures thereof.

[0157] Microsphères comprenant majoritairement au moins un ingrédient cosmétique choisi among cationic surfactants

[0158] Selon un mode de réalisation, la présente invention concerne des microsphères decationic or anionic surfactants, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, preferably between 2 and 8 µm, preferably between 2 and 5 µm representing at least 80% by mass of said microspheres, preferably at least 90% by mass of said microspheres, and preferably 100%.

[0159] Selon un mode de réalisation, la présente invention concerne des microsphères de cationic surfactants, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, preferably between 2 and 8 µm, preferably between 2 and 5 µm, representing at least 80% by mass of said microspheres, preferably at least 90% by mass of said microspheres.

[0160] Selon un mode de réalisation, la présente invention concerne des microsphères decationic surfactants chosen from glycine betaine derivatives, preferably Cosmegreen with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, preferably between 2 and 8 µm, preferably between 2 and 5 µm representing at least 80% by mass of said microspheres, preferably at least 90% by mass of said microspheres.

[0161] Selon un mode de réalisation, la présente invention concerne des microsphères de BrassicylIsoleucinateEsylate(and) Brassica Alcohol with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 15 µm, preferably between 2 and 12µm, representing at least 80% by mass of said microspheres, preferably at least 90% by mass of said microspheres.

[0162] Selon ces modes de réalisation (lorsque les microsphères comprennent majoritairement au at least one cosmetic ingredient chosen from cationic surfactants), the microspheres may further comprise at least one colloid and at least one residual surfactant resulting from the process.

[0163] Selon ce mode de réalisation, la présente invention concerne un composé qui comprend :- between 80% and 95% by mass of cationic surfactant, preferably between 85% and 93%, more preferably between 88% and 92% by mass of said compound; and - between 5% and 20% by mass of colloid and / or surfactant, preferably between 7% and 15%, more preferably between 8% and 12% by mass of said compound.

[0164] Microsphères comprenant majoritairement au moins une cire

[0165] Selon un mode de réalisation, la présente invention concerne des microsphères de cires, de volume diameter d(50) between 0.5 and 20 µm, preferably between 1 and 15 µm, preferably between 2 and 12 µm, and representing at least 95% by mass of said microspheres.

[0166] Selon un mode de réalisation, la présente invention concerne des microsphères de cires chosen from hydrogenated castor oil, hydrogenated olive oil and their mixtures, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 15 µm, preferably between 2 and 12 µm, and representing at least 95% by mass of said microspheres.

[0167] Selon ces modes de réalisation (lorsque les microsphères comprennent majoritairement au less one wax), the microspheres may further comprise at least one colloid and at least one residual surfactant resulting from the process.

[0168] Selon ce mode de réalisation, la présente invention concerne un composé qui comprend :- between 80% and 95% by mass of cationic surfactant, preferably between 85% and 93%, more preferably between 88% and 92% by mass of said compound; and - between 5% and 20% by mass of colloid and / or surfactant, preferably between 7% and 15%, more preferably between 8% and 12% by mass of said compound.

[0169] Microsphères comprenant au moins un tensioactif et au moins une cire

[0170] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, said microspheres comprising at least one ingredient chosen from surfactants and at least one wax.

[0171] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, said microspheres comprising at least one ingredient chosen from cationic or anionic surfactants and at least one wax.

[0172] Selon un mode de réalisation, la présente invention concerne également des microsphères,with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient chosen from cationic surfactants and at least one wax.

[0173] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one ingredient chosen from cationic surfactants, preferably chosen from glycine betaine derivatives, Distearoylethyl Dimonium Chloride Cetearyl Alcohol and mixtures thereof, and at least one wax.

[0174] Selon un mode de réalisation, la présente invention concerne également des microsphères,with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient chosen from cationic surfactants chosen from glycine betaine derivatives, preferably Cosmegreen, and at least one wax.

[0175] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient chosen from cationic surfactants chosen from glycine betaine derivatives, preferably Cosmegreen, and at least one wax chosen from hydrogenated olive oil, hydrogenated castor oil and mixtures thereof.

[0176] Selon un mode de réalisation, la présente invention concerne également des microsphères,with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one Distearoylethyl Dimonium Chloride Cetearyl Alcohol and at least one wax.

[0177] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one Distearoylethyl Dimonium Chloride Cetearyl Alcohol and at least one wax chosen from hydrogenated olive oil, hydrogenated castor oil and mixtures thereof.

[0178] Selon ces modes de réalisation (lorsque les microsphères comprennent au moins un surfactant, at least one wax), the microspheres may further comprise a residual colloid used in the process.

[0179] Ainsi, selon ces modes de réalisation, les microsphères comprennent :- between 4% and 30% by mass of cationic surfactant, preferably between 4% and 28%, more preferably between 5% and 28% by mass of said compound; - between 60% and 80% by mass of wax, preferably between 64% and 78.5%, more preferably between 65% and 78.5% by mass of said compound and - between 5% and 20% by mass of residual colloid used during the process, preferably between 7% and 18.5%, more preferably between 7.5% and 18% by mass of said compound.

[0180] Selon un premier mode de réalisation, lors que le tensioactif cationique est au moins un dérivéof glycine betaine, preferably Cosmegreen, the microspheres comprise: - between 3% and 6% by mass of cationic surfactant, preferably between 3.5% and 5%, more preferably between 4% and 4.5% by mass of said compound; - between 75% and 80% by mass of wax, preferably between 76% and 79%, more preferably between 77% and 78.5% by mass of said compound; - between 15% and 20% by mass of residual colloid used during the process, preferably between 16% and 19%, more preferably between 17% and 18% by mass of said compound.

[0181] Selon un second mode de réalisation, lorsque le tensioactif cationique est au moins unDistearoylethyl Dimonium Chloride Cetearyl Alcohol the microspheres comprise:- between 25% and 30% by mass of cationic surfactant, preferably between 26% and 29%, more preferably between 27% and 28% by mass of said compound; and - between 60% and 70% by mass of wax, preferably between 62% and 67%, more preferably between 64% and 65% by mass of said compound. - between 5% and 10% by mass of residual colloid used during the process, preferably between 6% and 9%, more preferably between 7% and 8% by mass of said compound.

[0182] Microsphères comprenant au moins une huile et au moins une cire

[0183] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one ingredient chosen from oils and at least one wax.

[0184] Selon un mode de réalisation, la présente invention concerne également des microsphères,with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one ingredient chosen from oils preferably chosen from oils rich in omega 3 such as linseed oil and in DHA such as linseed oil and mixtures thereof and at least one wax.

[0185] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, preferably between 2 and 5 µm, said microspheres comprising at least one ingredient chosen from oils preferably chosen from oils rich in omega 3 and DHA and their mixtures and at least one wax, said wax being 2,3-di(octadecanoyloxy)propyl octadecenoate.

[0186] Selon ce mode de réalisation, lorsque la microsphère comprend au moins un ingrédient choisiamong the oils and at least one wax, the oil / wax ratio is between 40:100 and 80:100, preferably between 60:100 and 75:100 and preferably around 68:100.

[0187] Selon ces modes de réalisation (lorsque les microsphères comprennent au moins une huile and at least one wax), the microspheres may further comprise a residual colloid used in the process.

[0188] Selon ce mode de réalisation, les microsphères comprennent - Between 40% and 60% by mass of wax, preferably between 45% and 55%, more preferably between 48% and 52% by mass of said compound; - Between 25% and 40% by mass of oils, preferably between 30% and 37%, more preferably between 32% and 35% by mass of said compound; and - Between 10% and 25% by mass of residual colloid used in the process, preferably between 12% and 20%, more preferably between 14% and 18% by mass of said compound.

[0189] Microsphères comprenant au moins un ingrédient et au moins une cire, l’ingrédient being a mixture of at least one oil and at least one butter.

[0190] Selon un mode de réalisation, la présente invention concerne également des microsphères,with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient and at least one wax, the ingredient being a mixture of at least one oil and at least one butter.

[0191] Selon un mode de réalisation, la présente invention concerne également des microsphères, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8µm, preferably between 2 and 5µm, said microspheres comprising at least one ingredient and at least one wax, the ingredient being a mixture of sunflower oil, shea butter and an oily macerate of Aloe Vera.

[0192] Selon ces modes de réalisation (lorsque les microsphères comprennent au moins un ingredient and at least one wax, the ingredient being a mixture of at least one oil and at least one butter, at least one wax), the microspheres may further comprise a residual colloid used in the process.

[0193] Selon ce mode de réalisation, les microsphères comprennent :- between 40% and 55% by mass of wax, preferably between 42% and 52%, more preferably between 45% and 50% by mass of said compound; - between 30% and 45% by mass of a mixture of at least one oil and one butter, preferably between 32% and 40%, more preferably between 33% and 37% by mass of said compound; and - between 2% and 10% by mass of residual colloid used in the process, preferably between 3% and 8%, more preferably between 4% and 6% by mass of said compound.

[0194] Procédé d’obtention des microsphères selon l’invention

[0195] Les microsphères selon l’invention pourront être obtenues par le procédé tel que décrit dans patent EP2894978.

[0196] Selon un mode de réalisation, le procédé pour l’obtention des microsphères selon la présenteinvention, comprises the following steps:(I) Heating a fatty phase comprising (i) at least one wax, and / or (ii) at least one cosmetic ingredient having a melting point above 30°C and not being a wax, to a reaction temperature above the melting temperature of said at least one wax and / or said at least one cosmetic ingredient; (II) Heating a first aqueous phase comprising at least one water-soluble surfactant and at least one protective colloid, to said reaction temperature implemented in step (I), with mechanical stirring;(III) Incorporating said fatty phase into said first aqueous phase while maintaining the reaction temperature, with mechanical stirring, so as to form a stable oil-in-water emulsion;(IV) Adding dropwise, with mechanical stirring, said emulsion previously formed into a second aqueous phase comprising at least one water-soluble surfactant and / or at least one protective colloid, the temperature of said second phase being lower than the melting temperature of said wax and / or said cosmetic ingredient.

[0197] L’ingrédient cosmétique et la cire sont tels que ci-avant définis.

[0198] Selon un mode de réalisation, la température de chauffe de la phase grasse est supérieure at 30°C.

[0199] On entend par « stable » une émulsion dont la granulométrie n'évolue pas dans le temps du process, or the time required for transfer into the aqueous phase.

[0200] Ainsi, le procédé permet l’obtention de microsphères selon l’invention i.e., d’un diamètre en volume d(50) between 0.5 and 10µm, and composed of either:- predominantly at least one cosmetic ingredient having a melting point above 30°C and not being a wax;- predominantly at least one wax;- at least one wax and at least one cosmetic ingredient having a melting point above 30°C and not being a wax.

[0201] Ces microsphères sont telles que ci-avant définies et sont en suspension dans ladite second aqueous phase.

[0202] Le seul fait que l’émulsion obtenue à l’étape (III) soit ajoutée goutte à goutte permet d’obtenirthe microspheres according to the invention. The use of a protective colloid in the 1st aqueous phase combined with the dropwise addition of the emulsion makes it possible to further improve the formation of the microspheres, whereas the sole presence of a protective colloid without dropwise addition does not make it possible to produce microspheres.

[0203] Phase grasse

[0204] La phase grasse du procédé est constituée par soit : - a wax or a mixture of waxes, or- a cosmetic ingredient or a mixture of cosmetic ingredients, each of the cosmetic ingredients having a melting point above 30°C and not being a wax, or- (i) at least one wax and (ii) at least one cosmetic ingredient having a melting point above 30°C and not being a wax.

[0205] Cela signifie que ladite phase grasse ne comporte pas de produit amphiphile, de stabilisant, of surfactant or co-surfactant, or other additives which are not the wax and / or the cosmetic ingredient.

[0206] Les proportions de ladite au moins une cire et dudit au moins un ingrédient actif pourrontvary depending on the desired contents of said at least one wax and said at least one active ingredient within the fatty phase. A person skilled in the art is able to determine the proportions.

[0207] Les cires sont telles que ci-avant décrit.

[0208] Selon un mode de réalisation du procédé, la température réactionnelle est supérieure d’au minus 10°C at the melting temperature of said at least one wax and / or said at least one cosmetic ingredient.

[0209] Première et seconde phase aqueuse

[0210] Selon un mode de réalisation du procédé, le ou les tensioactif(s) de la première phase aqueous phase and / or the second aqueous phase is or are chosen from non-ionic surfactants, cationic surfactants and anionic surfactants.

[0211] Selon un mode de réalisation, le ou les tensioactif(s) de la première phase aqueuse et / ou de the second aqueous phase is or are chosen from polyoxyethylene stearyl ethers, sodium lauryl sulfonate, polyoxyethylene polyoxypropylene copolymers (AB, ABA, BAB form), sorbitan esters and Potassium Cetyl Phosphate.

[0212] On peut citer comme tensioactif(s) de la première phase aqueuse et / ou de la seconde phase aqueous steareth 21, Pluronic®, Tween® and Span® soluble in water and capable of forming an oil-in-water emulsion, and Synperonic®.

[0213] Ces tensioactifs sont bien connus de l’homme du métier.

[0214] Ainsi le stéareth 21 est un polyoxyéthylène stearyl éther comprenant 21 unités oxydeof ethylene per molecule whose CAS number is 9005-00-9. It is commercially available from BASF under the brand name Eumulgin S 21®.

[0215] Pluronic® est la marque sous laquelle BASF commercialise des copolymères polyoxyethylene polyoxypropylene also called poloxamers.

[0216] Tween® et Span® sont les marques sous lesquelles Croda commercialisent des esters oxyethylenated sorbitan fatty acids. Synperonic® is the brand under which Croda markets polyethylene polypropylene glycol copolymers.

[0217] Amphisol K® est la marque sous laquelle DSM commercialise le Potassium Cetyl Phosphate.

[0218] La première phase aqueuse comme la deuxième phase aqueuse conforme à l’invention peut comprise from 0.1 to 2.5% by mass, relative to the total mass of said aqueous phase, of at least one surfactant in accordance with the invention, preferably from 0.1 to 1% by mass, and more particularly from 0.25 to 0.5% by mass relative to the total mass of said aqueous phase.

[0219] Selon un mode de réalisation du procédé, le colloïde protecteur est choisi parmi les maltodextrins, polyvinylpyrrolidone, xanthan gum, carboxymethylcellulose, pectin, starches and its derivatives, guar gum, acacia gum and polyvinyl alcohol (PVA).

[0220] Selon un mode de réalisation du procédé, le colloïde protecteur est choisi parmi la gomme acacia and polyvinyl alcohol (PVA).

[0221] La première phase aqueuse comme la deuxième phase aqueuse conforme à l’invention peutcomprise from 0 to 5% by mass, relative to the total mass of said aqueous phase, of at least one colloid in accordance with the invention, preferably from 0.05 to 2.5% by mass, and more particularly from 0.1 to 2% by mass relative to the total mass of said aqueous phase.

[0222] Selon un mode de réalisation, la seconde phase aqueuse ne comporte pas de solvant additional other than those previously described, which allows the use of the least possible additives and the most ecological microspheres possible.

[0223] Selon un mode de réalisation, la température de la seconde phase est de 10°C à 5°C lower than the crystallization temperature of said at least one wax and / or said at least one cosmetic ingredient.

[0224] La vitesse d’agitation dans l’étape III est fonction de la quantité d’émulsion à réaliser et de la desired particle size and the person skilled in the art will be able to determine it based on his general knowledge. Thus, for batches of approximately 1 to 5 kg, the speed is 1500-2000 rpm for a particle size d(50) of 15-20 µm and 5000-6000 rpm for a particle size d(50) of less than 10 µm.

[0225] Selon un mode de réalisation du procédé, la vitesse d’agitation dans l’étape III est de 1500– 6,000 rpm, preferably between 2,000 and 5,000 rpm with the IKA® EurostarPower control-visc 6000 mixer equipped with a 45 mm diameter deflocculating blade.

[0226] Le débit de transfert « goutte à goutte » dans l’étape IV du procédé est fonction de la quantité of dispersion to be prepared and the person skilled in the art will be able to determine it based on his general knowledge. Thus, for batches of approximately 0.5 to 1 kg of second aqueous phase, the flow rate is between 10 and 40 ml / min and for batches of approximately 50 kg, the flow rate can go up to 10 liters / min.

[0227] Microsphères obtenues par le procédé

[0228] La présente invention concerne également des microsphères obtenues selon le procédé previously described.

[0229] Suspension de microsphères selon l’invention

[0230] Le procédé d’obtention ci-avant décrit permet l’obtention d’une suspension aqueuse comprising at least 25% by mass of microspheres relative to the total mass of the suspension. Preferably, the suspension comprises at least 30% by mass of microspheres, relative to the total mass of the suspension.

[0231] Ceci est réalisé en ajoutant au minimum une part et au maximum deux parts de l’émulsion obtained in step (III) in a part of the second aqueous phase.

[0232] La présente invention concerne également une suspension de microsphère obtenu selon le process previously described.

[0233] Poudre

[0234] Selon un mode de réalisation, les microsphères selon l’invention sont sous une forme sèche, such as a powder.

[0235] Selon un mode de réalisation, la forme sèche est obtenue par lyophilisation ou atomisation,preferentially by lyophilization of the suspension of microspheres previously obtained.

[0236] Selon un mode de réalisation, la forme sèche comprend les microsphères selon l’invention in a content of at least 90% by mass relative to the total mass of the dry form.

[0237]

[0238] La poudre peut comprendre, outre les microsphères, un ou plusieurs ingrédients choisis among preservatives, stabilizers, buffers, anti-caking agents, flow agents and their mixtures.

[0239] Composition cosmétique

[0240] La présente demande concerne également une composition cosmétique comprenant des cosmetic ingredient microspheres according to the present invention, and a physiologically acceptable medium.

[0241] Le milieu physiologiquement acceptable est de préférence cosmétiquement ou dermatologically acceptable. A "physiologically acceptable" or "cosmetically acceptable" or "dermatologically acceptable" medium means any medium that does not present harmful side effects and in particular does not produce redness, inflammation, heating, tightness or stinging unacceptable to a user of cosmetic or dermatological products. The medium is thus compatible with human keratin materials.

[0242] Matières kératiniques

[0243] Les matières kératiniques seront la peau, les muqueuses, le cuir chevelu, les cheveux, le hair system, eyelashes, eyebrows, lips, nails.

[0244] Galénique

[0245] Avantageusement, les microsphères selon l’invention, sous forme de suspension ou sous dry form can be used in any type of galenic such as liquid galenics or solid galenics.

[0246] Selon un mode de réalisation, la composition cosmétique se présente sous forme liquide ou solid, preferably solid.

[0247] A titre illustratif, pour les galéniques liquides, on citera les solutions aqueuses, hydroalcoholic or oily emulsions, microemulsions, nanoemulsions, suspensions, lotions, creams, aqueous or hydroalcoholic gels, foams, serums, solutions or dispersions for aerosol, dispersions of lipid vesicles.

[0248] A titre illustratif, pour les galéniques solides, on citera les savons, les syndets, les shampoings solids or solid shower gels made preferably from soap or syndet, the balms, solid or semi-solid sticks, powders or powders to be reconstituted for the formation of a cosmetic product (whether the powder is in any form such as granules, microbeads, glitter, etc.).

[0249] Selon un mode de réalisation préféré, la composition cosmétique est sous forme de solid shampoo, preferably obtained from syndet.

[0250] Ces galéniques solides pourront être obtenues par toutes les méthodes connues de l’hommeof the art for the preparation of solid galenics. It has in fact been advantageously demonstrated that the microspheres according to the invention (with or without waxes) could be incorporated into solid galenics without modification of the process for obtaining the solid galenic or deterioration of the microspheres.

[0251] Typiquement, les galéniques solides pourront être obtenues par extrusion ou par coulage à hot.

[0252] Avantageusement, la forme sphérique et la granulométrie en volume d(50) entre 0.5 et 20 µm, preferably between 1 and 10µm, preferably between 2 and 8µm allow easy mechanical adhesion to hair from 30 µm (fine hair) to 70 µm (thick hair) as illustrated in Figure 1. The particle size / hair size ratio acts in favor of the adhesion of the particle to the hair. This adhesion allows better resistance to washing of the particles when rinsing a shampoo for example.

[0253] Ainsi, la composition selon la présente invention est de préférence utile pour formuler des hygiene and care products for the scalp and / or hair as well as coloring products for the scalp and / or hair

[0254] Hygiène, soins et coloration du cuir chevelu et / ou des cheveux

[0255] Les compositions convenant à l’hygiène, aux soins et à la coloration du cuir chevelu et / ouhair can be presented in all forms suitable in the field, such as soaps, syndets, liquid or solid shampoos, dry shampoos, hair masks, syndets, serums, mousses, balms, creams, sprays, conditioners, detanglers, hair creams, lotions, gels, serums, sprays, rinse aids and coloring products, powder shampoos to be reconstituted.

[0256] Selon un mode de réalisation, la composition est sous forme d’un shampoing solide, preferentially obtained from syndet.

[0257] Selon un mode de réalisation, le shampoing solide est obtenu par extrusion.

[0258] Selon un mode de réalisation, l’ingrédient cosmétique est un tensioactif, de préférence un cationic surfactant, preferably chosen from glycine betaine derivatives as defined above, preferably CosmeGreen™ ES1822+ and CosmeGreen™ MB1618 from the company SurfactGreen.

[0259] Selon un mode de réalisation, l’ingrédient cosmétique n’est pas hydrosoluble.

[0260] L’invention a également pour objet un procédé de soin et / ou d’hygiène ou un procédé decoloring of keratin materials, in particular the scalp and / or hair, consisting of applying to said keratin materials, in particular the scalp and / or hair, a cosmetic composition comprising the microspheres of active ingredients according to the invention.

[0261] Visage et corps : Hygiène

[0262] La composition selon l’invention est également utile pour formuler des produits d’hygiène du face and body. For example, galenic forms suitable for hygiene and / or care of the face and / or body include serums, roll-ons, liquid or solid soaps, shower gels, syndets, gels, micellar waters, lotions, scrubs, deodorants, creams, skin masks, shaving creams, foams, aftershave products, milks, balms, grain scrubs, cleansing creams, milks, facial cleansers in milk form, aqueous serums, shaving powders, shower gels, powders to be reconstituted.

[0263] Selon un mode de réalisation, l’ingrédient cosmétique n’est pas hydrosoluble.

[0264] L’invention a également pour objet un procédé de nettoyage et / ou de démaquillage ou unprocess for caring for keratin materials, in particular the skin, consisting of applying to said keratin materials, in particular the skin, a cosmetic composition comprising the microspheres of active ingredients according to the invention.

[0265] Visage et corps : Maquillage

[0266] La composition selon l’invention est également utile pour formuler des produits de maquillage of the face and body. For example, galenic forms suitable for face and body makeup include foundation powders, loose powders, bronzing powders, compact foundations, eye shadows, eye shadows, lip balms, body balms, lipsticks, eye pencils, eyebrow pencils, lip pencils, and nail polishes.

[0267] Selon un mode de réalisation, l’ingrédient cosmétique est une cire.

[0268] Selon un mode de réalisation, la composition est sous forme de poudre, telle qu’une poudre loose, compact, compressed or a powder to be reconstituted.

[0269] L’invention a également pour objet un procédé de maquillage des matières kératiniques, en in particular the skin, consisting of applying to said keratin materials, in particular the skin, a cosmetic composition comprising the microspheres of active ingredients according to the invention.

[0270] La composition cosmétique selon l’invention peut également comprendre, en outre desmicrospheres according to the invention, at least one additive usual in the field, such as for example at least one compound chosen from an emollient or humectant agent, a gelling and / or thickening agent, a surfactant, an oil, an active agent, a colorant, a preservative, an antioxidant agent, an active agent, an organic or inorganic powder, a sunscreen and a perfume.

[0271] L’homme du métier est en mesure de choisir, parmi l’ensemble de ces éventuels additifs, both the nature and the quantity of those which will be added to the composition, so that it retains all of its properties.

[0272] Procédé d’obtention du shampoing solide

[0273] La présente invention concerne également un procédé d’obtention d’un shampoing solide, comprising:- the mixture of raw syndet and microspheres according to the invention to obtain a paste,- the extrusion of the previously obtained paste,- the cutting and / or molding of said paste if necessary.

[0274] Selon un mode de réalisation, le syndet brut dans l’étape de mélange est sous forme deshavings. In addition to the raw syndet and the microspheres according to the invention, any type of ingredient conventionally used in the manufacture of a solid shampoo by extrusion may be incorporated into the mixture. Examples include conditioners, surfactants, perfumes, colorants, etc.

[0275] Utilisation

[0276] Les inventeurs ont démontré que la formulation d’ingrédient cosmétique sous forme de microspheres according to the invention make it possible to improve the performance of the cosmetic ingredient, both during its application and for its cosmetic properties.

[0277] En effet, les inventeurs ont comparé un shampoing solide préparé à partir de syndet etcomprising a cosmetic ingredient as commercially available (i.e., without being formulated in the form of microspheres) to a solid shampoo prepared from syndet and comprising the cosmetic ingredient microspheres according to the invention. It has been demonstrated during a consumer test that the shaping of the cosmetic ingredient in the form of microspheres makes it possible to improve its properties during its application (improvement in obtaining foam, sensoriality during application and improvement in rinsing) but also from a cosmetic point of view (improvement in detangling, hair protection, cleaning, shine, styling, softness, character).

[0278] Plus particulièrement, il a été démontré que :- Foam production is improved;- Sensoriality during application is improved: (the product is considered more pleasant to use, easier to apply and provides a finer foam);- Rinsing is improved;- Detangling is improved;- The product does not dry out the hair;- Hair protection is improved;- Cleaning is improved;- Shine is improved;- Styling is improved;- Softness is improved;- Nourishing is improved.

[0279] Les inventeurs ont également démontré les bénéfices apportés par la formulation d’un actifmoisturizing agent in the form of microspheres according to the invention compared to the active ingredient alone. At equal concentration (0.3%), the active ingredient in microspheres has significantly higher moisturizing efficacy. It is particularly notable that even by tripling the concentration of the active ingredient alone (1%), it does not consistently achieve the efficacy of the active ingredient formulated according to the invention. These results confirm the substantial improvement in moisturizing efficacy provided by the microsphere technology according to the invention.

[0280] Ainsi, la présente invention concerne également l’utilisation des microsphères selon the invention to improve the cosmetic performance of said cosmetic ingredient.

[0281] Selon un mode de réalisation, les performances cosmétiques sont choisies parmi l’obtention foam, sensoriality, rinsing, detangling, hair protection, cleansing, shine, styling, softness, nourishing character, hydration of keratin materials, preferably of the skin.

[0282] Selon un mode de réalisation, les performances cosmétiques sont choisies parmi l’obtentionfoam, sensoriality, rinsing, detangling, hair protection, cleansing, shine, styling, softness, nourishing character.

[0283] Selon un mode de réalisation, la performance cosmétique est l’hydratation.

[0284] L’invention est illustrée de manière non limitative par les exemples ci-dessous. ExamplesExample 1: Microspheres according to the invention comprising at least one cosmetic ingredient having a melting point above 30°C and not being a wax and at least one wax.

[0285] Les procédés tel que décrits à l’exemple 1 permet d’obtenir des microsphères comprenant at least one cosmetic ingredient having a melting point above 30°C and not being a wax and at least one wax.

[0286] Exemple 1A : Microsphères selon l’invention comprenant un tensioactif cationique (CosmeGreen ES1822+) and a wax (hydrogenated olive oil)

[0287] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0288] [Tableau 2] Emuls 1 ère ion aqueous phase Fatty phase 2nd aqueous phase90% Demineralized water95% Phytowax 10L40 (oil95% Demineralized water 10% INAVEA Hydrogenated olive oil) ***5% INAVEA ORIGINAL(acacia gum)** 5% CosmeGreen ES1822+* ORIGINAL(acacia gum)** *Surfactant; **Protective colloid; *** Wax

[0289] Le CosmeGreen ES1822+*est un dérivé de glycine bétaïne.

[0290] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 40 / 60.

[0291] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 60 / 40.

[0292] Le débit de transfert d’émulsion en « goutte à goutte » est de 300ml / min.

[0293] Le diamètre D(50) des microsphères produites est de 15µm.

[0294] Matériel utilisé

[0295] [Tableau 3]Reactors Agitators SpeedReactor 1: 2.5 L stainless steel Mixer IKA® Eurostar 1300 rpmPower control-visc 6000, deflocculating blade D 45 mm Reactor 2: 2.5 L stainless steel Mixer RS ​​Lab, propeller at 4800-1000 rpm inclined blades

[0296] Protocole

[0297] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0298] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 65°C.

[0299] 2 / Préparation de la phase grasse en faisant fondre à 70°C la cire et en y ajoutant ensuite le CosmeGreen™ ES1822+.

[0300] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute, with stirring in an IKA Eurostar stirrer at 1300 rpm, then for 7 minutes.

[0301] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiqués above, stirring with an RS Lab stirrer, at speed 800 rpm.

[0302] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 1000 rpm.

[0303] 6 / Obtention d’une suspension de microsphères de taille 15 µm, à laquelle on ajoute 1% de Euxyl K712 preservative by mass relative to the total mass of the suspension.

[0304] Ce procédé permet l’obtention des suspensions de microsphères suivantes

[0305] Suspension 1

[0306] [Tableau 4] Trade name INCI %- Aqua 68.61Phytowax 10L40 Hydrogenated Olive Oil Decyl Ester 23.72INAVEA Original Acacia Senegal Gum 5.42Behenyl Alcohol CosmeGreen ES1822+ Arachidyl Alcohol 1.25 Betaine Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0307] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenantin addition a preservative (Euxyl K 712). The aqueous suspension contains 30.39% by mass of microspheres relative to the total mass of the suspension.

[0308] Chaque microsphère comprend : - 78.06% by mass of wax, relative to the total mass of the microsphere, the wax being a hydrogenated olive wax;- 4.11% by mass of the cationic surfactant CosmeGreen ES1822+, relative to the total mass of the microsphere;- 17.83% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process.

[0309] Une autre suspension a été obtenue par le procédé ci-avant décrit, la phase grasse étant composed of an equal mixture of hydrogenated olive oil and hydrogenated castor oil. The suspension is described below.

[0310] Suspension 2

[0311] [Tableau 5]Trade name INCI %- Aqua 68.61Phytowax 18L57 Hydrogenated Olive Oil Stearyl Ester 11.86Phytowax 22L73 Hydrogenated Castor Oil Behenyl Ester 11.86INAVEA Original Acacia Senegal Gum 5.42Behenyl Alcohol CosmeGreen ES1822+ Arachidyl Alcohol 1.25 Betaine Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0312] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant furthermore a preservative (Euxyl K 712). The aqueous suspension comprises 30.39% by mass of microspheres relative to the total mass of the suspension.

[0313] Chaque microsphère comprend : - 78.06% by mass of waxes, relative to the total mass of the microsphere, the waxes being a mixture of a hydrogenated olive oil and a hydrogenated castor oil;- 4.11% by mass of the cationic surfactant CosmeGreen ES1822+, relative to the total mass of the microsphere;- 17.83% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process.

[0314] Exemple 1B : Microsphères selon l’invention comprenant un tensioactif cationique (VarisoftEQ 65 MB) and a wax (hydrogenated olive oil)

[0315] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0316] [Tableau 6]Emulsi 1 ère on aqueous phase Fatty phase 2nd aqueous phase 100% Demineralized water 70% Phytowax Olive 18L5795% Demineralized water (hydrogenated olive oil) *** 5% INAVEA 30% VarisoftEQ 65 MB* ORIGINAL (acacia gum)** *Surfactant (cosmetic ingredient) **Protective colloid; *** Wax

[0317] Le VarisoftEQ 65 MB et un tensioactif cationique.

[0318] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 30 / 70.

[0319] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 65 / 35.

[0320] Le débit de transfert d’émulsion en « goutte à goutte » est de 13ml / min.

[0321] Le diamètre D(50) des microsphères produites est de 1.34µm.

[0322] Matériel utilisé

[0323] [Tableau 7] Reactors Agitators SpeedReactor 1: 2.5 L stainless steel Mixer IKA® Eurostar6000 rpm Power control-visc 6000, deflocculating blade D 45 mm Reactor 2: 2.5 L stainless steel Mixer RS ​​Lab, propeller at 4,800 rpm inclined blades

[0324] Protocole

[0325] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0326] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 80°C.

[0327] 2 / Préparation de la phase grasse en faisant fondre à 88°C la cire et en y ajoutant ensuite le VarisoftEQ 65 MB.

[0328] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute, with stirring in an IKA Eurostar stirrer at 4000 rpm, then for 10 minutes at 6000 rpm.

[0329] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiqués above, stirring with an RS Lab stirrer, at speed 800 rpm.

[0330] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 800 rpm.

[0331] 6 / Obtention d’une suspension de microsphères de taille 1.34 µm, à laquelle on ajoute 1% deEuxyl K712 preservative by mass relative to the total mass of the suspension.

[0332] Ce procédé permet l’obtention des suspensions de microsphères suivantes

[0333] Suspension 3

[0334] [Tableau 8] Trade name INCI %- Aqua 77.3Phytowax Olive 18L57 Hydrogenated Olive Oil Decyl Ester 14INAVEA Original Acacia Senegal Gum 1.7VarisoftEQ 65 MB DistearoylethylDimoniumChloride; CetearylAlcohol 6 Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0335] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant in addition a preservative (Euxyl K 712). The aqueous suspension contains 21.7% by mass of microspheres relative to the total mass of the suspension.

[0336] Chaque microsphère comprend : - 64.5% by mass of wax, relative to the total mass of the microsphere, the wax being a hydrogenated olive wax;- 27.6% by mass of the cationic surfactant VarisoftEQ 65 MB relative to the total mass of the microsphere;- 7.8% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process.

[0337] Exemple 1C : Microsphères selon l’invention comprenant une huile riche en oméga 3(linseed oil) and a wax (high melting point (approximately 73°C) C18 fatty acid monobasic triglyceride)

[0338] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0339] [Tableau 9] ère Emulsion 1 aqueous phase Fatty phase 2nd aqueous phase93% Demineralized water60% Dynasan 11893% Demineralized water 7% INAVEA (Tristearin)) *** 7% INAVEA ORIGINAL (acacia gum)**39% Oil rich in omega 3*ORIGINAL (acacia gum)** 1% tocopheryl acetate* *Cosmetic ingredient; **Protective colloid; *** Wax

[0340] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 40 / 60.

[0341] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 70 / 30.

[0342] Le débit de transfert d’émulsion en « goutte à goutte » est de 38ml / min.

[0343] Le diamètre D(50) des microsphères produites est de 3.4µm.

[0344] Matériel utilisé

[0345] [Tableau 10] Reactors Agitators SpeedReactor 1: 2.5 L stainless steel Ultra-Turrax IKA mixer 6000 rpm T50, S50N-G45F rod Reactor 2: 2.5 L stainless steel RS Lab mixer, 4500 rpm propeller inclined blades

[0346] Protocole

[0347] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0348] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 80°C.

[0349] 2 / Préparation de la phase grasse en faisant fondre à 80°C la cire et en y ajoutant ensuite oil rich in omega 3 and tocopheryl acetate.

[0350] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 5 minute, under agitation in an Ultra-Turrax IKA T50 agitator, S50N-G45F shaft at 6000 rpm.

[0351] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiquésabove, under stirring with an RS Lab stirrer, at speed 500 rpm.

[0352] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous moderate speed 500 rpm.

[0353] 6 / Obtention d’une suspension de microsphères de taille 3.4 µm, à laquelle on ajoute 1% de Euxyl K712 preservative by mass relative to the total mass of the suspension.

[0354] Ce procédé permet l’obtention des suspensions de microsphères suivantes

[0355] Suspension 4

[0356] [Tableau 11] Trade name INCI %- Aqua 65.84 Dynasan 118 Tristearin 16.63 INAVEA Original Acacia Senegal Gum 5.16 Oil rich in Omega 3 Linseed oil 11.03 Tocopheryl acetate 0.34 Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0357] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant in addition (Tocopheryl acetate). The aqueous suspension contains 33.16% by mass of microspheres relative to the total mass of the suspension.

[0358] Chaque microsphère comprend :- 50.2% by mass of wax, relative to the total mass of the microsphere, the wax being a monoacid triglyceride based on a C18 fatty acid with a high melting point (approximately 73°C). ;- 33.3% by mass of an oil rich in omega 3 relative to the total mass of the microsphere;- 15.6% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process- 1% by mass of antioxidant (tocopheryl acetate), relative to the total mass of the microsphere.

[0359] Exemple 1D : Microsphères selon l’invention comprenant un actif hydratant Hydrosmart and two waxes (hydrogenated olive oil and hydrogenated castor oil).

[0360] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0361] [Tableau 12] è Emulsion 1st aqueous phase Fatty phase 2nd aqueous phase90% Demineralized water27.4% Phytowax Olive99% Demineralized water 10% INAVEA 18L57*** 1% INAVEA ORIGINAL(acacia gum)** 27.4% Phytowax Ricin ORIGINAL(acacia gum)** 22L73*** 40% Hydrosmart*5.2%Cosmegreen ** Cosmetic ingredient; ** Protective colloid; *** Wax

[0362] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 40 / 60.

[0363] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 60 / 40.

[0364] Le débit de transfert d’émulsion en « goutte à goutte » est de 500ml / min.

[0365] Le diamètre D(50) des microsphères produites est de 12.3µm.

[0366] Matériel utilisé

[0367] [Tableau 13] Reactors Agitators SpeedReactor 1: 2.5 L stainless steel Mixer IKA® Eurostar2100 rpm Power control-visc 6000, deflocculating blade D 45 mm Reactor 2: 2.5 L stainless steel Mixer RS ​​Lab, propeller at 4800-1000 rpm inclined blades

[0368] Protocole

[0369] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0370] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 80°C.

[0371] 2 / Préparation de la phase grasse en faisant fondre à 85°C les cires et en y ajoutant ensuite Hydrosmart and Cosmegreen

[0372] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute, with stirring in an IKA Eurostar stirrer at 1000 rpm, then for 8 minutes at 2100 rpm.

[0373] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiqués above, stirring with an RS Lab stirrer, at speed 800 rpm.

[0374] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 1000 rpm.

[0375] 6 / Obtention d’une suspension de microsphères de taille 12.34 µm, à laquelle on ajoute 1% of Euxyl K712 preservative by mass relative to the total mass of the suspension.

[0376] Ce procédé permet l’obtention des suspensions de microsphères suivantes

[0377] Suspension 5

[0378] [Tableau 14] Trade name INCI % Eau 70.16 Phytowax Olive 18L57 Hydrogenated Olive Oil6.85 P hytowax Ricin 22L73 Decyl Ester 6.85Hydrosmart 10Inavea Original Acacia Senegal Gum 3.84Behenyl Alcohol CosmeGreen ES1822+ CH Arachidyl Alcohol 1.3 Betaine Aqua Euxyl K712 Sodium benzoate 1 Potassium sorbate 100

[0379] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant in addition a preservative (Euxyl K712). The aqueous suspension contains 28.84% by mass of microspheres relative to the total mass of the suspension.

[0380] Chaque microsphère comprend : - 47.50% by mass of wax, relative to the total mass of the microsphere, the wax being a mixture of hydrogenated olive oil and hydrogenated castor oil;- 34.67% by mass of hydrosmart relative to the total mass of the microsphere;- 4.52% by mass of cosmegreen relative to the total mass of the microsphere- 13.31% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process.

[0381] Exemple 2 : Procédé d’obtention d’une dispersion de microsphères selon l’invention composed mainly of cosmetic ingredients

[0382] Dans ces exemples, des microsphères d’ingrédient cosmétique ont été obtenues, les microspheres being composed mainly of a cosmetic ingredient which is not a wax.

[0383] Exemple 2A : Procédé d’obtention d’une dispersion de microsphères selon l’inventioncomposed mainly (at least 90%) of Cosmegreen ES1822+ (cationic surfactant)

[0384] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0385] [Tableau 15] 1ère Aqueous phase emulsion Fatty phase 2nd aqueous phase 99% Demineralized water 100% CosmeGreen ES1822+* 95% Demineralized water 1% PVA* 5% INAVEA Buffer solution qsp pH 4.3 ORIGINAL (acacia gum)** Buffer solution qsp pH 4.3 *Surfactant; **Protective colloid; *** Active ingredient

[0386] Le CosmeGreen ES1822+ est un dérivé de glycine bétaïne.

[0387] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 30:70.

[0388] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 65:35.

[0389] Le débit de transfert d’émulsion en « goutte à goutte » est de 400ml / min. L’extrait sec de la dispersion obtained in example 2 is 21.5%.

[0390] Le diamètre D(50) des microsphères produites est de 3,1µm. La D(10) est de 0.6µm et la D(90) of 8.5µm.

[0391] Matériel utilisé

[0392] [Tableau 16] Reactors Agitators SpeedReactor 1: 5 L stainless steel Mixer IKA® Eurostar 600 rpmPower control-visc 6000, deflocculating blade D 45 mm Reactor 2: 5 L stainless steel Ultra-Turrax IKA T50, rod10000 rpm S50N-G45F

[0393] Protocole

[0394] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0395] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 85°C.

[0396] 2 / Préparation de la phase grasse en faisant fondre à 90°C le CosmeGreen™ ES1822+.

[0397] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute with stirring in an Ultra-Turrax IKA T50 at 3000 rpm, then for 5 minutes at 10000 rpm.

[0398] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiquésabove, stirring with an IKA Eurostar stirrer, at speed 600 rpm.

[0399] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 600rpm.

[0400] 6 / Obtention d’une suspension de microsphères de Cosmegreen de taille 3,1µm telle que ci- described below, to which 1% of Euxyl K712 preservative is added by mass relative to the total mass of the suspension.

[0401] Suspension 6

[0402] [Tableau 17] Trade name INCI %- Aqua 75.8Behenyl Alcohol CosmeGreen ES1822+ Arachidyl Alcohol 19.85 Betaine INAVEA Original Acacia Senegal Gum 1.77Aqua Buffer solution Sodium Lactate 1.15 Lactic acid Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate Kuraray-Poval 4-88 LV Polyvinyl alcohol 0.43

[0403] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant furthermore a preservative (Euxyl K 712) and a buffer solution. The aqueous suspension comprises 22.05% by mass of microspheres relative to the total mass of the suspension 6.

[0404] Chaque microsphère comprend :- 90.02% by mass of the cationic surfactant CosmeGreen ES1822+, relative to the total mass of the microsphere;- 8.03% by mass of the colloid (acacia gum) and 1.95% by mass of the surfactant (PVA), relative to the total mass of the microsphere, the colloid and the surfactant being the residual colloid and surfactant used in the process.

[0405] Exemple 2B : Procédé d’obtention d’une dispersion de microsphères selon l’invention composed mainly (100%) of Emulsense™ HC (cationic surfactant)

[0406] Les ingrédients et proportions utilisés dans le procédé sont décrits dans le tableau ci-après.

[0407] [Tableau 18] èr Emulsion 1st aqueous phase Fatty phase 2nd aqueous phase99% Demineralized water100% Emulsense™ HC*** 95% Demineralized water1% PVA* 5% INAVEA ORIGINAL(acacia gum)** *Surfactant; **Protective colloid; *** Active ingredient

[0408] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 30 / 70.

[0409] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 65 / 35.

[0410] Le débit de transfert d’émulsion en « goutte à goutte » est de 33ml / min. L’extrait sec de la dispersion obtained in example 2B is 21.4%.

[0411] Le diamètre D(50) des microsphères produites est de 11.25 µm.

[0412] Matériel utilisé

[0413] [Tableau 19]Reactors Agitators SpeedReactor 1: 5 L stainless steel IKA® Eurostar mixer4000 rpm Power control-visc 6000, deflocculating blade D 45 mm Reactor 2: 5 L stainless steel IKA® Eurostar mixer 1800 rpmPower control-visc 6000, deflocculating blade D 40 mm

[0414] Protocole

[0415] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0416] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 80°C.

[0417] 2 / Préparation de la phase grasse en faisant fondre à 80°C le Emulsense™ HC.

[0418] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute stirred in an IKA Eurostar stirrer at 3000 rpm, then for 10 minutes at 4000 rpm.

[0419] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiqués above, stirring with an IKA Eurostar stirrer, at speed 600 rpm.

[0420] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 1800rpm, at a flow rate of 33ml / min.

[0421] 6 / Obtention d’une suspension de microsphères de Emulsense™ HC de taille (D50) 11.25µm as described below, to which 1% of Euxyl K712 preservative is added by mass relative to the total mass of the suspension.

[0422] Suspension 7

[0423] [Tableau 20]Trade name INCI %- Aqua 76.85Emulsense™ HC BrassicylIsoleucinateEsylate(and) Brassica20.00 Alcohol INAVEA Original Acacia Senegal Gum 1.70Aqua Euxyl K 712 Sodium benzoate 1.00 Potassium sorbate Kuraray-Poval 4-88 LV Polyvinyl alcohol 0.45

[0424] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant furthermore a preservative (Euxyl K 712). The aqueous suspension comprises 20.00% by mass of microspheres relative to the total mass of the suspension 3.

[0425] Chaque microsphère comprend : - 90.3% by mass of the cationic surfactant Emulsense™ HC, relative to the total mass of the microsphere;- 7.7% by mass of the colloid (acacia gum) and 2% by mass of the surfactant (PVA), relative to the total mass of the microsphere, the colloid and the surfactant being the residual colloid and surfactant used in the process.Example 3: Process for obtaining a dispersion of microspheres according to the invention, mainly comprising a wax.

[0426] Dans cet exemple, des microsphères d’ingrédient cosmétique ont été obtenues, lesmicrospheres being composed mainly of a mixture of waxes (hydrogenated olive oil and hydrogenated castor oil).

[0427] Les réactifs utilisés dans le procédé sont tels que ci-après décrits.

[0428] [Tableau 21] è Emulsion 1st aqueous phase Fatty phase 2nd aqueous phase91.6% Demineralized water50% Phytowax18L57 50%***98.03% Demineralized water 7.2% Maltodextrin** Phytowax22L73 *** 1.3% Amphisol K* 1.2% Amphisol K* 0.67% Euxyl K712 *Surfactant; **Protective colloid; *** Waxes:

[0429] Le ratio volumique entre la phase grasse et la première phase aqueuse dans l’émulsion est 50:50.

[0430] Le ratio volumique entre l’émulsion et la seconde phase aqueuse dans la dispersion est 50:50.

[0431] Le débit de transfert d’émulsion en « goutte à goutte » est de 300ml / min.

[0432] Le diamètre D(50) des microsphères produites est de 13.4µm.

[0433] Matériel utilisé

[0434] [Tableau 22] Reactor Agitator SpeedReactor 1: 5 L stainless steel Mixer IKA® Eurostar 2000 rpmPower control-visc 6000, deflocculating blade D 45 mm Reactor 2: 5 L stainless steel Mixer RS ​​Lab, blade 1300 rpm cross-type mixing

[0435] Protocole

[0436] La suspension de microsphères est fabriquée selon les étapes successives 1- 6 suivantes :

[0437] 1 / Chargement du réacteur 1 avec les ingrédients de la première phase aqueuse indiqués ci- above at a temperature of 90°C.

[0438] 2 / Préparation de la phase grasse en faisant fondre à 80°C les cires.

[0439] 3 / Ajout de la phase grasse préalablement fondue dans ledit réacteur 1, pendant 1 minute with stirring in an IKA® Eurostar stirrer at 2000 rpm, for 4 minutes.

[0440] 4 / Fabrication de la seconde phase aqueuse dans le réacteur 2 avec les ingrédients indiquésabove, stirring with an RS Lab stirrer, at speed 600 rpm, at 90°C then cool to 4°C.

[0441] 5 / Ajout au goutte à goutte de l’émulsion présente dans le réacteur 1 dans le réacteur 2 sous high speed 1300rpm.

[0442] 6 / Obtention d’une suspension de microsphères comprenant majoritairement des cires.

[0443] La suspension de microsphères a ensuite été lyophilisées, dans un lyophilisateur pilote de CRYOTEC benchtop, for obtaining microsphere powder. A person skilled in the art will be able to determine the cycle necessary for drying the suspensions obtained. The composition of the microsphere powder is described below:

[0444] Forme sèche, poudre de microsphères 1

[0445] [Tableau 23] Phytowax 18L57 Hydrogenated Olive Oil Stearyl Ester 44.57 Phytowax 22L73 Hydrogenated Castor Oil Behenyl Ester 44.57 Glucidex 6D Maltodextrin 6.46 Amphisol K Potassium Cetyl Phosphate 3.40 Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0446] Les microsphères sont sous forme de poudre, la poudre comprenant 92.54 % en masse de microspheres relative to the total mass of the powder 2. The powder includes, in addition to the microspheres, Glucidex 6D which stabilizes the powder and prevents the particles from clumping together during drying and a preservative (Euxyl K 712).

[0447] Chaque microsphère comprend :- 96.33% by mass of wax, relative to the total mass of the microsphere, the wax being a mixture of hydrogenated olive oil and hydrogenated castor oil,- 3.67% by mass of surfactant (Amphisol K), relative to the total mass of the microsphere, the surfactant being the residual surfactant used in the process.

[0448] Exemple 4 : Microsphères sous forme de poudre.

[0449] D’autres formes sèches ont été obtenues par un procédé de lyophilisation et sont décrites ci- After.

[0450] Forme sèche, poudre de microsphères 2

[0451] [Tableau 24] Trade name INCI %Phytowax 10L40 Hydrogenated Olive Oil Decyl Ester 89.14Glucidex 6D Maltodextrin 6.46Amphisol K Potassium Cetyl Phosphate 3.40Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0452] Les microsphères sont sous forme de poudre, la poudre comprenant 92.54 % en masse de microspheres relative to the total mass of the powder 1. The powder includes, in addition to the microspheres, Glucidex 6D which stabilizes the powder and prevents the particles from clumping together during drying and a preservative (Euxyl K 712).

[0453] Chaque microsphère comprend :- 96.33% by mass of wax, relative to the total mass of the microsphere, the wax being a hydrogenated olive oil - 3.67% by mass of surfactant (Amphisol K), relative to the total mass of the microsphere, the surfactant being the residual surfactant used in the process.

[0454] Forme sèche, poudre de microsphères 3

[0455] [Tableau 25] Trade name INCI %Behenyl Alcohol CosmeGreen ES1822+ Arachidyl Alcohol 85.80 Betaine INAVEA Original Acacia Senegal Gum 7.21Sodium Lactate Buffer 2.87 Lactic acid Kuraray-Poval 4-88 LV Polyvinyl alcohol 1.91Aqua Euxyl K712 Sodium benzoate 2.12 Potassium sorbate

[0456] Les microsphères sont sous forme de poudre, la poudre comprenant 94.92 % en masse de microspheres relative to the total mass of the powder 3. The powder includes, in addition to the microspheres, a buffer and a preservative.

[0457] Chaque microsphère comprend :- 90.39% by mass of the surfactant CosmeGreen ES1822+, relative to the total mass of the microsphere;- 7.59% by mass of the colloid (acacia gum) and 2.01% by mass of the surfactant (PVA), relative to the total mass of the microsphere, the colloid and the surfactant being the residual colloid and surfactant used in the process.Example 5: Solid shampoo comprising a surfactant in the form of microspheres

[0458] Un shampoing solide obtenu à partir de syndet comprenant en tant que tensioactif un dérivé of glycine betaine, and more particularly CosmeGreen ES1822+ CH was manufactured, the surfactant CosmeGreen ES1822+ CH being in the form of a suspension of microspheres according to the invention and as obtained by the process described in Example 2. The suspension of microspheres used in this example is suspension 6 as obtained by the process described in Example 2 and more particularly described in Table 17.

[0459] Le CosmeGreen ES1822+ CH sous sa forme commercialement disponible se présente sous the shape of pellets of a few millimeters.

[0460] Le syndet brut se présente sous la forme de copeaux qui sont introduits dans le mélangeur.These shavings are the product of a saponification or neutralization reaction.

[0461] Dans le mélangeur sont ensuite ajoutés la suspension de microsphères selon l’invention, le perfume and possibly a coloring.

[0462] Le mélangeur est un mélangeur à double bras en Z qui permet un travail mécanique à room temperature.

[0463] Le mélange obtenu est homogène et granuleux.

[0464] L’étape suivante est une étape d’affinage durant laquelle le mélange préalablement obtenu is passed through a refiner which will compact it into lumps.

[0465] L’affinage est réalisé par une machine à double vis, équipée de refroidissement pour keep the product at a constant temperature, approximately at room temperature.

[0466] Les bondillons obtenus à l’étape précédente sont broyés par des calandreuses multicylindres. The spacing of the grinders is between 0 and 5 mm, and the person skilled in the art knows how to adapt the spacing according to the product to be obtained.

[0467] A cette étape, la préparation est homogène avec une texture souple.

[0468] L’étape suivante est une étape d’extrusion, au travers d’une boudineuse qui va compacter le soap by forcing it through a die, being pushed by an endless screw.

[0469] La boudineuse est une boudineuse duplex, c’est-à-dire 2 étages avec 2 vis, est équipée d’une vacuum bell. The extruder is also cooled by a liquid refrigerant circuit between 5 and 15°C. At its end is the extrusion cone (and the die), the only part of the machine that is heated, between 50 and 70°C, to ensure the sliding and smoothing of the soap through the die.

[0470] Ainsi extrudé, le syndet est coupé en bondons par une coupeuse à guillotine. La forme de la die is defined by the shape of the mold.

[0471] Le bondon est mis en forme par la presse, à l’aide de moules multi empreintes. Les presses are in fact equipped with multi-cavity molds which are cooled (up to 20°C).

[0472] Après l’opération de mise en forme du bondon, le surplus appelé crashs, est enlevé automatically to be recycledExample 6: Comparison of the properties of a solid shampoo comprising the surfactant CosmeGreen ES1822+ as commercially available (i.e., without being formulated in the form of microspheres) with those of a solid shampoo comprising the surfactant CosmeGreen ES1822+ in the form of microspheres according to the invention

[0473] Les propriétés d’un shampoing solide obtenu à partir de syndet et comprenant le tensioactifCosmeGreen ES1822+ as commercially available (i.e., without being formulated in the form of microspheres) were compared with that of a solid shampoo obtained from syndet and comprising the surfactant CosmeGreen ES1822+ in the form of microspheres according to the invention and obtained according to the process as described in Example 2. The solid shampoos (commercial form of Cosmegreen and microspheres of Cosmegreen) were obtained according to the process described in Example 5. The suspension of microspheres used in this example is suspension 6 as obtained by the process described in Example 2 and more particularly described in Table 17. In its current commercial form, Cosmegreen has beneficial properties for hair and skin. These properties are mainly attributed to its mechanical effects.

[0474] Malgré des propriétés indéniables qui contribuent à la qualité des produits cosmétiquesintended for hair and skin, the formulation of Cosmegreen in different cosmetic preparations (liquid or solid) in its current commercial form raises various problems:

[0475] Pour être utilisé dans les galéniques liquides (tels que les shampoings et après-shampoings), Cosmegreen surfactant must be melted at 80°C and mixed with fatty phases at the same temperature, and / or in glycerin to be either emulsified or co-solubilized. The pH must also be adjusted.

[0476] Pour être utilisé dans les galéniques solides coulées à chaud, on retrouve les mêmes temperature constraints regarding mixing with other solids. Crystallization must be controlled to avoid phase separations between the constituents.

[0477] Quant à son utilisation en galéniques solides extrudées, son utilisation est limitée, car la extrusion temperature is lower than the melting temperature of Cosmegreen. Its dispersion in the solid phase is then poor, and its performance as a conditioner of the finished product is poor or even non-existent.

[0478] Les microsphères de tensioactif selon l’invention offrent la possibilité de formuler le surfactant in these various galenic forms without heating constraints.

[0479] Shampoing solide comprenant le tensioactif CosmeGreen ES1822+ tel quecommercially available (i.e., not formulated as microspheres)

[0480] Lors de la fabrication du shampoing solide à partir de syndet, la température d’extrusion est of approximately 65°C. This extrusion temperature is lower than the 80°C melting temperature of Cosmegreen. Thus, Cosmegreen in its commercial form will not be mixed homogeneously but will be dispersed in fairly large clusters (a few tens to hundreds of µm) in the mixture allowing the solid shampoo to be obtained, as seen in Figure 2. These aggregates and this non-homogeneity in the mixture will considerably reduce the effectiveness of the surfactant.

[0481] En effet, lors de l’application du shampoing avec de l’eau, les constituants classiquementpresent in a shampoo dissolve in water, playing their role one by one. The Cosmegreen will be deposited by friction on the surface of the hair in clumps. However, the size of the Cosmegreen clumps is significantly greater than that of a hair, causing them to be eliminated during rinsing. This considerably reduces the presence of Cosmegreen on the surface of the hair, which weakens its performance, which is partly linked to the quantity deposited.

[0482] Shampoing solide comprenant le tensioactif Cosmegreen sous forme de microsphères selon the invention

[0483] Le format microsphères selon l’invention permet une incorporation directe et homogène du Cosmegreen surfactant in the constituents of the mixture for extrusion, and allows the production of a solid shampoo with Cosmegreen uniformly distributed in the mass.

[0484] Avantageusement, le procédé d’extrusion n’altère pas les microsphères qui restent intactes after solubilization of the shampoo in water (Figure 3).

[0485] Lors de l’utilisation par le consommateur, le Cosmegreen se dépose par friction sur le cheveu and adheres. The application is uniform on the surface of the hair (Figure 4), and resists rinsing with water (Figure 5).

[0486] En effet, la forme sphérique et la granulométrie d(50) de 3.1µm permet une accrocheeasy mechanics on hair from 30 µm (fine hair) to 70 µm (thick hair) as illustrated in Figure 1. Thus, the particle size / hair size ratio acts in favor of the adhesion of the particle to the hair. This adhesion allows better resistance to washing of the particles when rinsing a shampoo for example.

[0487] Ainsi, il apparait clairement que le Cosmegreen sous forme de microsphères selon l’invention can easily be incorporated into a solid dosage form such as a solid shampoo, without the need to heat them, unlike its commercial form, while preserving its properties in terms of effectiveness and stability. Advantageously, the microspheres are not altered by the extrusion process.

[0488] Exemple 7 : Comparaison des performances du tensioactif Cosmegreen tel que commercially available (i.e., without being formulated in the form of microspheres) to those of the Cosmegreen surfactant in the form of microspheres according to the invention

[0489] L’objectif du test a été d’évaluer l’acceptabilité, la tolérance et l’efficacité de trois shampoings solids A, B and C. The formulas of these three compositions are reproduced below.

[0490] La méthodologie est ci-après reproduite.

[0491] [Tableau 26]Description of the panel Panel of 24 people 17 women 7 men Average age: 44 years between 28 and 69 years Inclusion criteria Healthy volunteers Female or male volunteers Volunteers aged 18 to 75 years Duration of the test 21 days Instructions Apply at least 3 times a week to the scalp and hair: wet the solid shampoo and hair well then rub, massage thoroughly and rinse

[0492] Le produit A est un shampoing solide, obtenu à partir de syndet et comprenant le Cosmegreen as commercially available (i.e., not formulated as microspheres).

[0493] [Tableau 27] Ingredient % by mass relative to the total mass of the product T ENSIANOL SCI 96 Cosmegreen ES 1822+ 2Glycerin 4811 RSPO MB 2

[0494] La glycérine a été introduite dans la formulation car le Cosmegreen ES1822+ ne se mélange not properly alone. Glycerin improves workability and allows Cosmegreen ES1822+ to be incorporated into the syndet.

[0495] Le produit B est un shampoing solide obtenu à partir de syndet et ne comprenant pas de Cosmegreen.

[0496] [Tableau 28] Ingredient % by mass relative to the total mass of the product T ENSIANOL SCI 100

[0497] Le produit C est un shampoing solide obtenu à partir de syndet et comprenant le Cosmegreenin the form of microspheres according to the invention. The microspheres are in the form of an aqueous suspension. The aqueous suspension of microspheres used in this example is suspension 6 as obtained by the process described in example 2 and more particularly described in table 17.

[0498] [Tableau 29] Ingredient % by mass relative to the total mass of the product T ENSIANOL SCI 90 Aqueous suspension 6 microspheres of 10 Cosmegreen ES 1822+

[0499] Les shampoings solides A, B et C ont été obtenus selon le procédé tel que décrit à l’exemple 5.

[0500] Pour chacune de ces compositions, les critères suivantes ont été évalués :

[0501] [Tableau 30] Criteria Rating Tolerance Mention a sign of intolerance or a feeling of discomfort such as tingling, redness, tightness, etc. Overall satisfaction The overall judgment of the product should be categorized as “very good”, “good”, “bad”, “very bad”. The smell is pleasant The product lathers well when applied The product is easy to apply The product makes detangling easier The product produces a fine lather The product is easy to rinse Volunteers were asked to indicate, for each of these statements, whether they were: The product protects the hair "TOTALLY AGREE" The product gently cleanses the hair "AGREE" The hair is shiny "TOTALLY DISAGREE" The hair is easy to style "DISAGREE" The hair is less oily The scalp seems balanced A weighted average of the scores awarded was then calculated. The product prevents my hair from getting greasy again The hair is soft The product does not weigh down the hair The hair is supple The hair is light The hair is nourished

[0502] Résultats produit A

[0503] [Tableau 31]Criteria Rating Tolerance No signs of intolerance were observed No sensation of discomfort was reported Overall satisfaction Overall judgment of the product: Very good 12.5% ​​B on : 3.5% Bad: 42% Very bad: 8%

[0504] [Tableau 20] NOT ALL NOT ALL AVERAGE D 'ACCORD D'ACCORD AGREE WEIGHTED AGREE The smell is pleasant 4.55 18.18 27.27 50.00 22.73 The product foams well when applied 58.33 12.50 8.33 20.83 70.83 The product is pleasant to use 39.13 30.43 21.74 8.70 69.57 The product is easy to apply 41.67 33.33 20.83 4.17 75.00 The product makes it easier to detangle 22.22 16.67 33.33 27.78 38.89 The product produces a fine foam 29.17 45.83 20.83 4.17 75.00 The product is easy to rinse 47.83 43.48 8.70 0.00 91.30The product does not dry out the hair 12.50 54.17 20.83 12.50 66.67The product protects the hair 13.64 36.36 45.45 4.55 50.00The product gently cleanses the hair 30.43 43.48 26.09 0.00 73.91The hair is shiny 8.70 56.52 26.09 8.70 65.22 Hair is easy to style 25.00 37.50 25.00 12.50 62.50 Hair is less oily 20.83 50.00 25.00 4.17 70.83 Scalp seems balanced 8.33 62.50 25.00 4.17 70.83 Product prevents hair from getting greasy again 17.39 34.78 30.43 17.39 52.17 Hair is soft 25.00 37.50 20.83 16.67 62.50 Product does not weigh hair down 29.17 37.50 25.00 8.33 66.67 Hair is supple 29.17 45.83 12.50 12.50 75.00Hair is light 33.33 41.67 16.67 8.33 75.00Hair is nourished 17.39 43.48 21.74 17.39 60.87

[0505] Conclusions produit A :

[0506] [Tableau 32] Conclusion The product presented: Very good dermatological tolerance Good cosmetic acceptability Significant items (>74%): •The product is easy to apply •The product produces a fine foam •The product is easy to rinse •The hair is supple •The hair is light

[0507] L’acceptabilité du produit A est partagée. Le produit A est considéré comme bon à 50% (sum of “very good” and “good”) and is considered 50% bad (sum of “bad” and “very bad”).

[0508] 29% des volontaires achèteraient le produit, contre 71% qui ne l’achèteraient pas.

[0509] Résultats produit B

[0510] [Tableau 33] Criteria Rating Tolerance No signs of intolerance were observed No sensation of discomfort was reported Overall satisfaction Overall judgment of the product: Very good 8% Bon : 54% Bad: 34% Very bad: 4%

[0511] [Tableau 34] NOT ALL NOT ALL AVERAGE D 'ACCORD D'ACCORD AGREE AGREE WEIGHTED The smell is pleasant 8.33 20.83 41.67 29.17 29.17 The product foams well upon application 29.17 62.50 4.17 4.17 91.67The product is pleasant to use25.00 54.17 16.67 4.17 79.17The product is easy to apply29.17 54.17 12.50 4.17 83.33The product makes detangling easier23.81 47.62 14.29 14.29 71.43The product produces a fine foam 25.00 58.33 12.50 4.17 83.33The product is easy to rinse 33.33 66.67 0.00 0.00 100.00The product does not dry out the hair 30.43 43.48 21.74 4.35 73.91The product protects the hair21.74 39.13 34.78 4.35 60.87The product gently cleanses the hair33.33 58.33 8.33 0.00 91.67The hair is shiny25.00 50.00 25.00 0.00 75.00The hair is easy to style26.09 43.48 26.09 4.35 69.57The hair is less oily18.18 54.55 22.73 4.55 72.73The scalp seems to be balanced16.67 54.17 25.00 4.17 70.83The product prevents my hair from getting greasy again13.04 47.83 30.43 8.70 60.87Hair is soft 25.00 45.83 29.17 0.00 70.83The product does not weigh down the hair 25.00 45.83 25.00 4.17 70.83Hair is supple 25.00 50.00 20.83 4.17 75.00Hair is light 25.00 50.00 20.83 4.17 75.00Hair is nourished 13.04 52.17 26.09 8.70 65.22,

[0512] Conclusions produit B :

[0513] [Tableau 35] Conclusion The product presented: Very good dermatological tolerance Good cosmetic acceptability Significant items (>74%): •The product foams well upon application •The product is pleasant to use •The product is easy to apply •The product produces a fine foam •The product is easy to rinse •The product gently cleanses the hair •The hair is shiny •The hair is supple •The hair is light

[0514] Le produit B est considéré comme bon à 62% (somme de « très bon » et « bon ») et est considered bad at 38% (sum of “bad” and “very bad”).

[0515] 37% des volontaires achèteraient le produit, contre 63% qui ne l’achèteraient pas.

[0516] Résultats produit C

[0517] [Tableau 36] Criteria Rating Tolerance No signs of intolerance were observed 1 feeling of discomfort was reported Overall satisfaction Overall judgment of the product: Very good 42% Bon : 37% Bad: 17% Very bad: 4%

[0518] [Tableau 37] ALL TO D'ACCORD PAS TOUTDONE DONE NOT AVERAGE AGREE AGREE AGREE WEIGHTED The smell is pleasant 4.17 16.67 50.00 29.17 20.83 The product foams well when applied 39.13 43.48 13.04 4.35 82.61 The product is pleasant to use 43.48 39.13 13.04 4.35 82.61 The product is easy to apply 50.00 45.83 0.00 4.17 95.83 The product makes detangling easier 19.05 57.14 19.05 4.76 76.19 The product produces a fine foam 41.67 45.83 8.33 4.17 87.50 The product is easy to rinse 54.17 45.83 0.00 0.00 100.00The product does not dry out the hair 33.33 45.83 12.50 8.33 79.17The product protects the hair 17.39 60.87 17.39 4.35 78.26The product gently cleanses the hair 29.17 62.50 4.17 4.17 91.67The hair is shiny 25.00 50.00 20.83 4.17 75.00The hair is easy to style 45.45 31.82 18.18 4.55 77.27The hair is less oily 16.67 45.83 33.33 4.17 62.50The scalp seems to be balanced 20.83 50.00 20.83 8.33 70.83The product prevents my hair from getting greasy again 8.70 47.83 30.43 13.04 56.52Hair is soft 29.17 54.17 16.67 0.00 83.33The product does not weigh down the hair 21.74 52.17 21.74 4.35 73.91Hair is supple 20.83 54.17 20.83 4.17 75.00Hair is light 20.83 45.83 29.17 4.17 66.67Hair is nourished 17.39 60.87 13.04 8.70 78.26,

[0519] Le produit C est considéré comme bon à 79% (somme de « très bon » et « bon ») et est considered bad at 21% (sum of “bad” and “very bad”).

[0520] 67% des volontaires achèteraient le produit, contre 33% qui ne l’achèteraient pas.

[0521] Tableau

[0038] Conclusion The product presented: Very good dermatological tolerance Good cosmetic acceptability Significant items (>74%): •The product foams well upon application •The product is pleasant to use •The product is easy to apply •The product facilitates detangling •The product produces a fine foam •The product is easy to rinse •The product does not dry out the hair •The product protects the hair •The product gently cleanses the hair •The hair is shiny •The hair is easy to style •The hair is soft •The hair is supple •The hair is nourished

[0522] Ainsi, le produit C possèdent les meilleures performances, comparativement aux produits A and B.

[0523] Tel que démontré par le test consommateur, les microsphères selon l’invention permettent advantageously to improve the qualities and properties of the surfactant.

[0524] En effet, et par comparaison au shampoing solide comprenant le Cosmegreen tel que commercially available (i.e., without being formulated in the form of microspheres), it has been demonstrated in the present consumer test that the shaping of Cosmegreen in the form of microspheres makes it possible to improve the properties of the surfactant, both for its application and for its cosmetic properties, as summarized in table 28 below.

[0525] Une amélioration de l’application et de la sensorialité lors de l’application ont été observed: - Improvement in obtaining foam (weighted average of 70.83 for product A for the criterion “the product foams well on application” vs. 82.61 for product C); - Improvement in sensoriality during application (weighted averages, respectively, of 69.57, 75 and 75 for the criteria “the product is pleasant to use”, “the product is easy to apply” and “the product provides a fine foam” for product A vs. 82.61, 95.83 and 87.50 for product C) ;- Improvement during rinsing (weighted average of 91.30 for product A for the criterion “the product foams well on application” vs 100 for product C).

[0526] Amélioration des propriétés cosmétiques : - Improved detangling (weighted average of 38.89 for product A vs 76.19 for product C);- The product does not dry out the hair (weighted average of 66.67 for product A vs 79.17 for product C);- Improved hair protection (weighted average of 50.00 for product A vs 78.26 for product C);- Improved cleaning (weighted average of 73.91 for product A vs 91.67 for product C)- Improved shine (weighted average of 65.22 for product A vs 75 for product C) ;- Improved styling (weighted average of 91.30 for product A vs 77.27 for product C) - Improved softness (weighted average of 91.30 for product A vs 83.33 for product C); - Improved nourishing character (weighted average of 60.87 for product A vs 78.26 for product C).

[0527] [Tableau 39]Product A Product B Product CThe product is easy to applyThe product is easy to applyThe product is easy to rinseThe product is easy to rinseThe product is easy to rinseThe product provides a fine foamThe product provides a fine foamThe product lathers wellThe product lathers wellThe product lathers well when appliedThe product gently cleanses the hairThe product gently cleanses the hairThe product is pleasant to useThe product is pleasant to useThe hair is softThe hair is softThe hair is shinyThe hair is shinyThe hair is easy to styleThe hair is softThe hair is nourishedThe product facilitates detanglingThe product does not dry out the hairThe product protects the hair

[0528] Exemple 7 : Compositions galéniques

[0529] Sérums aqueux

[0530] Deux sérums aqueux, comprenant des microsphères du tensioactif cationique CosmeGreenES1822+ were prepared, one comprising the microspheres of the cationic surfactant CosmeGreen ES1822+ in the form of suspension 1, the other in the form of suspension 2 as previously described in Tables 4 and 5. The composition of the aqueous sera is described in the table below:

[0531] [Tableau 40] Phase Composition %A Aqua QSP

[0532] La galénique est préparée selon les étapes suivantes : la phase A est préparée par solubilization of xanthan gum in water, with stirring at room temperature, then glycerin and perfume are added. The preservatives of phase B, then the microspheres (phase C) are also incorporated with stirring.

[0533] Shampoings liquides

[0534] Trois shampoings liquides, comprenant trois suspensions aqueuses différentes deMicrospheres of the cationic surfactant CosmeGreen ES1822+ were prepared (suspensions 1, 2 and 6 as described above in tables 4, 5 and 8). The composition of the liquid shampoos is described in the table below:

[0535] [Tableau 41] Composition %Aqua 82.36%Sodium cocoyl isethionate 6.97%Decyl Glucoside 4.00%Microspheres (in the form of suspension 1, 2 or 6) 3.00%Cocamidopropyl betaine 1.87%Sodium Benzoate 1.00%Cyamopsis tetragonoloba (guar) gum 0.50%Guar hydroxypropyltrimonium chloride 0.30%Citric acid Qsp pH 5.5

[0536] La galénique est préparée selon les étapes suivantes : la phase A est préparée parsolubilization of the gum in water, while stirring using a deflocculating paddle at room temperature. Cocamidopropyl betaine is gradually added to phase A, then stirred for 10 minutes. Then decyl glucoside is gradually added to the mixture and stirred for 10 minutes. Finally, Sodium cocoyl isethionate is also gradually added and the mixture is left stirring for a further 15 minutes. Phase B is prepared by solubilization of the gum in water, while stirring using a deflocculating paddle at room temperature. Phases A and B are mixed, then the microspheres (phase C) and the preservative (phase D) are also incorporated while stirring. Finally, the pH is adjusted to 5.5 using citric acid.

[0537] [Tableau 42]Steps Composition %PreparationDemineralized water 41.18%phase ACyamopsis tetragonoloba (guar) gum 0.50%Cocamidopropyl betaine 1.87%Added phase ADecyl Glucoside 4.00%Sodium cocoyl Isethionate 6.97%PreparationDemineralized water 41.18%phase BGuar hydroxypropyltrimonium chloride 0.30%Phase CMicrospheres (in the form of suspension 1, 2 or 6) 3.00% S odium Benzoate 1,00% Phase D Citric acid Qsp pH 5.5

[0538] Gel douche à reconstituer

[0539] Trois gels douche à reconstituer, comprenant des microsphères sous forme sèche ont été prepared (Powders 1, 2, 3 as described above in tables 11, 12 and 13). The composition of the shower gels to be reconstituted is described in the table below:

[0540] [Tableau 43] Composition %Sodium Cocoyl Isethionate 78.84%Instant Fragrance powder perfume 8.76%Microspheres in dry form (Powder 1, 2 or 3) 7.90%Xanthan gum 2.50%Sodium Benzoate 2.00%

[0541] La poudre de gel douche est obtenue par mélange de tous les constituants. La poudre The resulting solution should be reconstituted at 10% in lukewarm water. Shake and let stand for 24 hours before use.

[0542] Poudre à raser

[0543] Deux poudres à raser, comprenant des microsphères sous forme sèche ont été préparées(Powders 2 and 3 as described above in Tables 12 and 13). The composition of the shaving powders is described in the table below:

[0544] [Tableau 44] Composition %Xanthan gum (80 mesh) 49%Disodium Lauryl Sulfosuccinate 49%Microspheres in dry form (Powder 2 or 3) 2%

[0545] La poudre à raser est à déposer dans la main. Appliquer quelques gouttes d’eau, mélanger and apply to the face.

[0546] Shampoing poudre à reconstituer

[0547] Deux shampoings poudre à reconstituer, comprenant des microsphères sous forme sèche (Powders 2 and 3 as described above in Tables 12 and 13) were prepared. The composition of the powder shampoos to be reconstituted is described in the table below:

[0548] [Tableau 45] Composition %Sodium Laurylglucosides Hydroxypropylsulfonate 38%Disodium Lauryl Sulfosuccinate 38%Glucomannan 10% Microspheres in dry form (Powder 1 or 3) 10%Instant Fragrance powder perfume 5%

[0549] La poudre de shampoing est à reconstituer à 10% dans l’eau tiède. Agiter et laisser reposer 24 hours before use.

[0550] Poudre compacte

[0551] Une poudre de maquillage compacte, comprenant des microsphères sous forme sèche (Powder 2 as described above in Table 12) was prepared. The composition of the compact powder is described in the table below:

[0552] [Tableau 46]Composition %Magnesium stearate 42.375%Sericite 300S 42.375%Pigment Colorona Oriental Beige 5.85%Glycerin 2%Perfume 0.4%Microspheres in dry form (Powder 1) 7%

[0553] La poudre obtenue après mélange des différents composants est compactée dans une aluminum cup.

[0554] Avantageusement, les microsphères selon l’invention peuvent être intégrées dans un compacted galenic, without loss of their properties. Example 8: Evaluation of the moisturizing effect of cosmetic ingredients formulated in the form of microspheres according to the invention

[0555] Ces études visent à évaluer l'efficacité hydratante et les propriétés sensorielles d’ingrédients cosmetic in the form of microspheres according to the invention (example 8A) and to compare the moisturizing performance of an active ingredient in the form of microspheres according to the invention vs. the non-formulated active ingredient in the form of a microsphere (example 8B).

[0556] Méthodologie d'évaluation

[0557] La mesure de l'hydratation cutanée a été réalisée par cornéométrie, une technique qui quantifies skin hydration by measuring its dielectric constant. This method is based on the principle that the higher the skin hydration, the greater the measured conductivity.

[0558] Caractéristiques de la mesure^ Corneometry allows an evaluation on a thickness of 15 μm^ This low measurement depth does not allow a measurement to be taken immediately after application^ Protocol: measurement before daily application, then measurement after 24 hours of application

[0559] Protocole d'application ^ Continuous application of serums throughout the duration of the study (once a day), including weekends^ Measurements taken daily at approximately constant times, except in exceptional cases

[0560] Design expérimental ^ Panel of 4 volunteers^ Evaluation of 5 serums containing different ingredients^ Continuity of measurements over a minimum of 7 applications per serum

[0561] Exemple 8A : Evaluation de l’effet hydratant et des propriétés sensorielles

[0562] L’objet de l’étude est de déterminer l’efficacité hydratante d’un actif sous forme de microspheres according to the invention as well as the impact of such an ingredient on the sensory properties of the serum.

[0563] Les compositions des sérums A et B sont les suivantes :

[0564] [Tableau 47] Sérum A : Ingredient %Glycerin 0.5Euxyl K712 (water, potassium sorbate, sodium benzoate) G omme xanthane 1.5 Eau 97

[0565] [Tableau 51] Sérum B :Ingredient %Glycerin 0.5Euxyl K712 (water, potassium sorbate, 1 sodium benzoate) G omme xanthane 1.5 CreaskinGlide 3 Eau 97 100

[0566] CreaskinGlide correspond à la suspension 2 décrite au tableau 14, à savoir des microsphères comprising mainly a mixture of hydrogenated olive oil and hydrogenated castor oil:[Table 48] N om commercial INCI % - Aqua 68.61 Phytowax 18L57 Hydrogenated Olive Oil Stearyl Ester 11.86 Phytowax 22L73 Hydrogenated Castor Oil Behenyl Ester 11.86 INAVEA Original Acacia Senegal Gum 5.42 Behenyl Alcohol CosmeGreen ES1822+ Arachidyl Alcohol 1.25 Betaine Aqua Euxyl K 712 Sodium benzoate 1 Potassium sorbate

[0567] Les microsphères sont en suspension dans un milieu aqueux, le milieu aqueux comprenant furthermore a preservative (Euxyl K 712). The aqueous suspension comprises 30.39% by mass of microspheres relative to the total mass of the suspension.

[0568] Chaque microsphère comprend :- 78.06% by mass of waxes, relative to the total mass of the microsphere, the waxes being a mixture of a hydrogenated olive oil and a hydrogenated castor oil;- 4.11% by mass of the cationic surfactant CosmeGreen ES1822+, relative to the total mass of the microsphere;- 17.83% by mass of the colloid, relative to the total mass of the microsphere, the colloid being the residual colloid used in the process.

[0569] La Figure 6 présente une comparaison claire entre deux formulations : ^ Blank Serum A: formulation without CreaskinGlide.^ Serum with ingredient B: formulation comprising the ingredient in the form of microspheres according to the invention, namely CreaskinGlide.

[0570] La Figure 6 permet de démontrer que les microsphères de CreaskinGlide maintiennent systematically a higher hydration rate, with values ​​generally oscillating between 6 and 16, while virgin serum presents more modest values ​​between approximately -1 and 4.

[0571] Par ailleurs les propriétés sensorielles du sérum B ont été comparées à celles du sérum A.Comparing the sensory properties between the two products shows several notable differences. In terms of softness, serum B scores higher (7 / 10) than virgin serum (5 / 10). The stickiness is identical for both products with an average score of 4 / 10. The most significant difference concerns the mattifying effect, where serum B excels with a very high score of 8 / 10, while serum A only scores a low 1 / 10. Regarding the speed of penetration, serum B also shows a better performance (5 / 10) compared to virgin serum A (3 / 10). Finally, both products have an identical spreadability with a good score of 7 / 10.

[0572] L'étude démontre l'efficacité hydratante significative du sérum comprenant l'ingrédientCreaskinGlide in the form of microspheres according to the invention. Beyond the hydration performance, this technology offers two major advantages: -Ease of cold formulation: The formulation of the waxes in the form of microspheres allows them to be incorporated into an aqueous gel at room temperature, which would have been technically impossible with traditional waxes requiring a heating step. -Preservation and improvement of sensory properties: Despite their incorporation into an aqueous formula, the waxes in the form of microspheres retain their beneficial sensory characteristics, providing a distinctive texture and feel to the final product.

[0573] Exemple 8B : Comparaison des performances de l’ingrédient Hydrasmart tel que commercially available (i.e., without being formulated in the form of microspheres) to those in the form of microspheres according to the invention

[0574] Les résultats de cette étude permettront de déterminer si le procédé selon l'invention améliore significantly the moisturizing properties of the ingredient compared to its standard commercial form.

[0575] Les compositions des sérums C, D et E sont les suivantes :

[0576] [Tableau 49] Sérum C :Ingredient %Glycerin 0.5Euxyl K712 (water, potassium sorbate, 1 sodium benzoate) G omme xanthane 1.5 Hydrosmart Microspheres (3% of 3 microspheres = 0.3% active) Eau 94 100

[0577] [Tableau 50] Sérum D : Ingredient %Glycerin 0.5Euxyl K712 (water, potassium sorbate, 1 sodium benzoate) G omme xanthane 1.5 Hydrosmart 0.3 Eau 96.7 100

[0578] Tableau 51] Sérum E : Ingredient %Glycerin 0.5Euxyl K712 (water, potassium sorbate, 1 sodium benzoate) G omme xanthane 1.5 Hydrosmart 1 Eau 96 100

[0579] Les microsphères Hydrosmart ont la composition suivante et ont été obtenues par le procédé as described in Example 1D.

[0580] [Tableau 52] Ingredient % Eau 70.16 Phytowax Olive 18L57 6.85Phytowax Castor 22L73 6.85Hydrosmart 10Inavea Original 3.84 CosmeGreen ES1822+ CH 1.3Euxyl K712 1100

[0581] L’actif Hydrosmart se compose comme suit :

[0582] [Tableau 53] Ingredient %Sunflower oil 36Shea butter 33Aloe vera oil macerate 30Tocopherol 1100

[0583] L’Hydrosmart est donc un mélange d’huile et de beurre, et plus particulièrement un mélange sunflower oil, shea butter and an oily macerate of Aloe Vera.

[0584] La figure 7 présente deux graphiques distincts (A et B) qui démontrent clairement l'avantage Hydrosmart microspheres according to the invention compared to the active ingredient alone:

[0585] Figure 7A - Comparaison à concentration égale (0,3%)

[0586] L'actif sous forme de microsphères montre une efficacité hydratante nettement supérieure àthe active ingredient alone at the same concentration.

[0587] L'actif sous forme de microsphères maintient des valeurs d'hydratation positives (entre +1 et +9) over the study period.

[0588] L'actif seul présente des performances fluctuantes mais généralement inférieures, avec des often negative values ​​(between -3 and +2).

[0589] Le pic d'efficacité observé à la troisième application pour l'actif sous forme de microsphères (+9) is particularly significant.

[0590] Figure 7B - Comparaison avec concentration triplée de l'actif seul

[0591] Même avec une concentration triplée (1% vs 0,3%), l'actif seul ne parvient pas à égaler systematically the effectiveness of the active ingredient in the form of microspheres.

[0592] On observe une instabilité importante de l'efficacité hydratante de l'actif seul, même à high concentration.

[0593] La chute d'efficacité observée à l'application 6 pour l'actif seul (-10) est particulièrement revealing this instability.

[0594] L'actif sous forme de microsphères présente une courbe d'efficacité plus stable et overall superior.

[0595] Conclusion

[0596] Ces résultats démontrent deux avantages majeurs de la technologie des microsphères selon the invention:

[0597] Efficacité supérieure à concentration égale : À concentration identique (0,3%), l'actif sous microsphere form provides significantly greater hydration than the active ingredient alone.

[0598] Économie de matière active : La nécessité d'utiliser trois fois plus d'actif seul (1%) pour attempting to achieve an efficiency comparable to that obtained with the active ingredient in the form of microspheres (0.3%) demonstrates a substantial gain in efficiency thanks to this technology.

[0599] Stabilité des performances : La formulation sous forme de microsphères permet une more consistent and predictable delivery of the active, unlike the active alone which has significant variations in effectiveness.

[0600] Cette étude fournit des preuves convaincantes de l'amélioration significative de l'efficacitémoisturizing provided by the microsphere technology according to the invention, while allowing a substantial reduction in the quantity of active ingredient required.

Claims

Claims

1. Microspheres of cosmetic ingredient, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, the cosmetic ingredient having a melting point above 30°C, and in which:- when the cosmetic ingredient is other than a wax, the latter represents at least 80% by mass of said microspheres, and- when the cosmetic ingredient is a wax, the latter represents at least 95% by mass of said microspheres.

2. Microspheres, with a volume diameter d(50) of between 0.5 and 20 µm, preferably between 1 and 10 µm, and preferably between 2 and 8 µm, said microspheres comprising at least one ingredient and at least one wax, said cosmetic ingredient having a melting point above 30°C and is different from a wax.

3. Microspheres according to claim 1 or 2, characterized in that, when the cosmetic ingredient is other than a wax, the cosmetic ingredient is chosen from surfactants, butters, oils, and mixtures thereof, preferably surfactants and mixtures of at least one butter and at least one oil.

4. Microspheres according to claim 3, characterized in that the surfactant is an anionic or cationic surfactant, preferably cationic, and preferably chosen from glycine betaine derivatives, Cetrimonium chloride, Behenoyl PG-Trimonium chloride, Polyglyceryl-10 Stearate, Distearoylethyl Hydroxyethylmonium Methosulfate, Cetearyl Alcohol, Distearoylethyl Dimonium Chloride, Behentrimonium Methosulfate, Distearoylethyl Dimonium Chloride, Cetearyl Alcohol, Brassicyl Isoleucinate Esylate (and) Brassica Alcohol and mixtures thereof, and in that the butters are chosen from shea butter, mango butter, cocoa butter, cupuaçu butter, pracaxi butter, murumuru butter, Shorearobusta (Sal Butter) and their mixtures.

5. Microspheres according to claim 4, characterized in that the cosmetic ingredient is chosen from glycine betaine derivatives, preferably the glycine betaine derivatives are glycine betaine ester or amide salts, preferably glycine betaine ester or amide salts comprising from 14 to 24 carbon atoms, and preferably the glycine betaine derivatives are derivatives of formula (I) [Chem 1] Xn-[(CH3)3N+-CH2-COZ-R]n where: Z denotes an oxygen atom or an -NH group, R is a linear or branched, saturated or unsaturated alkyl group comprising from 14 to 24 carbon atoms, preferably, the radical R is chosen from myristyl (C14:0), cetyl (C16:0), palmitoleyl groups (C16:1), stearyl (C18:0), oleyl (C18:1), linoleyl (C18:2), linolenyl (C18:3), arachidyl (C20:0), arachidonyl (C20:4), behenyl (C22:0), 2-hexyldecyl, 2-octyldodecyl and 2-decyltetradecyl. X is an organic or inorganic anion. and n is 1 or 2.

6. Microspheres according to claim 1 or 2, characterized in that the cosmetic ingredient is a wax, preferably chosen from hydrogenated castor oil, 2,3-di(octadecanoyloxy)propyloctadecenoate, hydrogenated olive oil, hydrogenated palm oil, shellac, 1,3-di(tetradecanoyloxy)propan-2-yl, carnauba wax, candelilla wax, beeswax, Glyceryl Stearate SE, Glyceryl Stearate, rice wax, hydrogenated coconut oil, macadamia wax, sumac wax, sumac berry wax, hydrogenated jojoba oil, hydrogenated sunflower oil, sunflower wax, orange peel wax, mimosa wax, jasmine wax, damask rose wax, myrica berry wax, green tea leaf wax, lanolin wax and mixtures thereof.

7. A method of manufacturing the microspheres according to any one of claims 1 to 6,characterized in that it comprises the following steps: (I) Heating a fatty phase comprising (i) at least one wax and / or (ii) at least one cosmetic ingredient having a melting point above 30°C and not being a wax, to a reaction temperature above the melting temperature of said at least one wax and / or said at least one cosmetic ingredient; (II) Heating a first aqueous phase comprising at least one water-soluble surfactant and at least one protective colloid, to said reaction temperature implemented in step (I), with mechanical stirring; (III) Incorporating said fatty phase into said first aqueous phase while maintaining the reaction temperature, with mechanical stirring, so as to form a stable oil-in-water emulsion; (IV) Adding dropwise, with mechanical stirring,of said emulsion previously formed in a second aqueous phase comprising at least one water-soluble surfactant and / or at least one protective colloid, the temperature of said second phase being lower than the melting temperature of said wax and / or said cosmetic ingredient.

8. Aqueous suspension of microspheres of cosmetic ingredient according to any one of claims 1 to 6.

9. Microspheres, and preferably aqueous suspension of microspheres of cosmetic ingredient, capable of being obtained by the manufacturing process according to claim 7.

10. Cosmetic composition comprising, in a physiologically acceptable state, microspheres of cosmetic ingredient according to any one of claims 1 to 6.

11. Cosmetic composition according to claim 10, characterized in that it is in liquid or solid form,preferably solid.

12. Cosmetic composition according to claim 10 or 11, characterized in that it is in the form of a solid shampoo.

13. Cosmetic composition according to claim 12, characterized in that the cosmetic ingredient is a surfactant, preferably a cationic surfactant, and preferably from glycine betaine derivatives.

14. Use of the cosmetic ingredient microspheres according to any one of claims 1 to 6, to improve the cosmetic performance of said cosmetic ingredient.

15. Use according to claim 14, characterized in that the cosmetic performance is chosen from obtaining foam, sensoriality, rinsing, detangling, hair protection, cleansing, shine, styling, softness, nourishing character, hydration of keratin materials, preferably of the skin. .,

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