WO2025026598A1 - Compact powder without talc and without free mica, based on perlite, at least one spherical filler, non-volatile oils, an amorphous hydrocarbon-based block copolymer and a particulate dye - Google Patents

Abstract

The present invention relates to a compact powder containing at least: a) an oily phase in an amount of at least 10% by weight relative to the total weight of the composition, said oily phase comprising at least one non-volatile oil; and b) a pulverulent phase in an amount of at least 40% by weight relative to the total weight of the composition, said pulverulent phase comprising at least: i) perlite; and ii) at least one spherical filler chosen from mineral fillers, organic fillers of natural origin, and mixtures thereof; and iii) at least one particulate colouring agent; and c) at least one amorphous hydrocarbon-based block copolymer; and d) at least one pigment; said composition containing no talc particle or particle of mica in free form and said composition being obtainable via a process comprising the following steps: 1) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and 2) the slurry is injected into a container and it is formed by compacting, in particular pressing and/or suction?

Description

Compact powder without talc and without free mica, based on perlite, at least one spherical filler, non-volatile oils, an amorphous hydrocarbon-based block copolymer and a particulate dye

The present invention relates to a solid composition in the form of a compact powder, in particular comprising a physiologically acceptable medium, in particular for coating keratin materials, more particularly for making up and/or caring for keratin materials, such as the skin, said compact powder being prepared via a wet process.

Skin care and/or makeup compositions are generally used to give the skin, such as the face, an attractive colour, but also to hide skin imperfections, such as redness, marks, wrinkles and fine lines.

The function of the abovementioned powders is mainly to give colour, matteness, and even, for those more particularly intended for facial skin, to improve the staying power of a foundation or, if used alone, to give coverage (foundation powder, eyeshadow, face powder). These presentation forms are particularly appreciated by users with regard to their lightness, softness, tack-free aspect or non-greasy feel.

In general, these compositions combine a pulverulent phase that is generally predominant with a binder phase usually featured by a liquid fatty phase. The pulverulent phase is formed essentially of fillers combined with pigments, the amount of these pigments being modified to afford the desired makeup effect, generally a colour effect.

To obtain a composition in solid, compacted form, it is known from the prior art to use compacted makeup powders formed by a mixture of powders with a fatty binder, which are put in form, for example, by compression.

However, these compact powders in particular have the drawback of being fragile. Thus, when the percentage of pigments increases in the product, its manufacture and its compacting become complicated or even impossible to perform at an industrial level given the quality and productivity requirements. Furthermore, large amounts of pulverulent phase in the compact powder do not give satisfactory sensory properties when the powder is picked up from its packaging and/or when it is applied to the surface of the skin to be made up. It is furthermore difficult for a formulator to obtain good staying power of the product on the skin. To overcome these drawbacks, if the amount of fatty binder is increased, this composition will have a tendency to become waxy, i.e. to harden during use to the point that it cannot be picked up.

Among the qualities desired for compact makeup powders, mention may be made of:

- good cohesion and homogenization of the composition,

- good impact strength,

- a good texture,

- suitable hardness,

- good adhesion to the skin,

- good uptake irrespective of the applicator (in terms of sufficient amount of product),

- comfort on application without a drying-out effect on the skin,

- good staying-power properties of the powder,

- good sensory properties at the time of pick-up,

- good sensory properties at the time of application of the product.

It is known practice from the prior art for the manufacture of such compositions to use volatile organic solvents (isododecane or isopropanol) used in a wet preparation process, known as a Wet Process, so as to inject one or more given foundation powders into a respective cup. These solvents allow fluidization of the powder and the formation of a “slurry” and forming thereof in a cup, and then evaporate off.

Compact powders obtained by this wet process technique have already been proposed in patent EP 2928448B1; said powders comprising:

- an oily phase in an amount of greater than or equal to 20% by weight relative to the total weight of the composition,

- a pulverulent phase greater than or equal to 40% by weight, relative to the total weight of the composition, comprising at least one spherical filler and at least one lamellar filler; the spherical filler(s) and the lamellar filler(s) being present in a respective total weight content such that the weight ratio of the spherical filler(s) to the lamellar filler(s) is greater than or equal to 0.01, preferably between 0.02 and 15.

Patent application EP3595620 also proposes a compact powder containing at least:

- an oily phase in an amount of at least 20% by weight relative to the total weight of the composition, said oily phase comprising at least one non-volatile non-phenyl silicone oil; and

- a pulverulent phase in an amount of at least 40% by weight relative to the total weight of the composition, said pulverulent phase comprising at least mica particles; and

- at least one amorphous hydrocarbon-based block copolymer, said composition containing no particle of untreated silicone talc and being obtainable via a wet preparation process comprising at least the following steps:

(i) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and

(ii) the slurry is injected into a container (cup or mould) and it is formed by compacting, in particular pressing and/or suction, to obtain the composition in powder form.

These compositions obtained via a wet process comprise a high amount of lamellar fillers comprising mica in free form and talc in order to maintain good injectability in the production process and, after evaporation of the volatile solvent, to obtain a satisfactory product deposit, satisfactory cohesion and satisfactory impact strength. The presence of talc in combination with mica in free form tends to give compact powders having glossy or satin effects. In the course of its research, the applicant found that the reduction or removal of talc and/or mica in free form from these compact powders in order to obtain matteness affected deposition, cohesion and/or sensoriality properties.

There is still a need to find new compact powders obtained via the wet process without talc and without mica in free form, having both good injectability in the wet production process and, after evaporation of the volatile solvent, good product deposition, good cohesion, good matteness and good sensoriality.

The applicant has discovered, unexpectedly, that these objectives can be achieved with a solid composition in the form of a compact powder, in particular comprising a physiologically acceptable medium and containing at least:

a) an oily phase in an amount of at least 10.0% by weight relative to the total weight of the composition, said oily phase comprising at least one non-volatile oil; and

b) a pulverulent phase in an amount of at least 40% by weight relative to the total weight of the composition, said pulverulent phase comprising at least:

i) perlite; and

ii) at least one spherical filler chosen from mineral fillers, organic fillers of natural origin, and mixtures thereof; and

iii) at least one particulate colouring agent; and

c) at least one amorphous hydrocarbon-based block copolymer; and

d) at least one pigment; said composition containing no talc particle or particle of mica in free form and said composition being obtainable via a wet preparation process comprising at least the following steps:

1) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and

2) the slurry is injected into a container and it is formed by compacting, in particular pressing and/or suction, to obtain the composition in compact powder form.

This discovery forms the basis of the invention.

Subjects of the invention

Thus, a first subject of the present invention is a solid composition in the form of a compact powder, in particular comprising a physiologically acceptable medium and containing at least:

a) an oily phase in an amount of at least 10% by weight relative to the total weight of the composition, said oily phase comprising at least one non-volatile oil; and

b) a pulverulent phase in an amount of at least 40% by weight relative to the total weight of the composition, said pulverulent phase comprising at least:

i) perlite; and

ii) at least one spherical filler chosen from mineral fillers, organic fillers of natural origin, and mixtures thereof; and

iii) at least one particulate colouring agent; and

c) at least one amorphous hydrocarbon-based block copolymer; and

d) at least one pigment; said composition containing no talc particle or particle of mica in free form and said composition being obtainable via a wet preparation process comprising at least the following steps:

1) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and

2) the slurry is injected into a container and it is formed by compacting, in particular pressing and/or suction, to obtain the composition in compact powder form.

A second subject of the present invention is a process for coating keratin materials, in particular the skin, and more particularly a process for making up and/or caring for said keratin materials, comprising the application thereto of the composition as defined above.

Definitions

In the context of the present invention, the term “keratin material” notably means the skin (face, cheeks, eyelids).

The term “physiologically acceptable” is understood to mean compatible with the skin and/or its integuments, which exhibits a pleasant colour, odour and feel and which does not cause unacceptable discomfort (stinging, tautness) liable to dissuade the consumer from using this composition.

The term “talc particle” refers to hydroxylated magnesium silicate particles of molecular formula Mg₃Si₄O₁₀(OH)₂ known as talc and belonging to the chemical family of phyllosilicates. Said talc particle can be untreated or surface-treated, i.e. uncoated or surface-coated, such as for example a surface treatment agent chosen from silicones, amino acids, fluoro derivatives or any other substance promoting the dispersion and compatibility of the filler in the composition.

Mica is the name of a family of minerals, of the group of silicates, subgroup of phyllosilicates, formed mainly from potassium aluminium silicate. It is characterized by its laminated structure (phyllosilicates). It is characterized by its laminated structure (phyllosilicates) most often giving shape to flakes and its metallic lustre.

The term “mica in free form” is understood to mean any natural or synthetic mica not bonded to one or more chemical compounds in a composite structure, such as pearlescent agents comprising mica as substrate onto which are coated metal oxides such as titanium dioxide, iron oxides, tin oxides.

The term “composition containing no talc particle” refers to any composition containing less than 1.0% by weight relative to the total weight of the composition, or even less than 0.5% by weight, or even less than 0.1% by weight, of particles of talc, or which is free of particles of talc.

The term “composition containing no particle of mica in free form” is understood to mean any composition containing less than 1.0% by weight relative to the total weight of the composition, or even less than 0.5% by weight, or even less than 0.1% by weight, of particles of mica in free form, or which is free of particles of mica in free form.

For the purposes of the present invention, the following definitions apply:

- “solid” means the state of the composition at ambient temperature (25°C) and at atmospheric pressure (760 mmHg), i.e. a composition of high consistency, which conserves its form during storage. In contrast to “fluid” compositions, it does not flow under its own weight. It is advantageously characterized by a hardness as defined below.

- “compact powder” means a mass of product of which the cohesion is at least partly provided by compacting or, preferably, pressing during the manufacture. In particular, by taking a measurement using a TA.XT.plus Texture Analyser® texturometer sold by Stable Micro Systems, the compact powder according to the invention may advantageously have a pressure resistance of between 0.1 and 1 kg and especially between 0.2 and 0.8 kg, relative to the surface area of the spindle used (in the present case 7.07 mm²). The measurement of this resistance is performed by moving an SMS P/3 flat-headed cylindrical spindle in contact with the powder over a distance of 2 mm and at a speed of 0.5 mm/second; more generally, this powder may be obtained by compacting or, preferably, by pressing.

The composition according to the invention advantageously comprises a solids content of greater than or equal to 95%, better still 98%, or even equal to 100%.

For the purposes of the present invention, the term “solids content” denotes the content of non-volatile matter.

The amount of solids content (abbreviated as SC) of a composition according to the invention is measured using a Halogen Moisture Analyzer HR 73® commercial halogen desiccator from Mettler Toledo. The measurement is performed on the basis of the weight loss of a sample dried by halogen heating and thus represents the percentage of residual matter once the water and the volatile matter have evaporated off. This technique is fully described in the machine documentation supplied by Mettler Toledo.

The measurement protocol is as follows:

Approximately 2 g of the composition, referred to hereinbelow as the sample, are spread out on a metal crucible, which is placed in the halogen desiccator mentioned above. The sample is then subjected to a temperature of 105°C until a constant weight is obtained. The wet mass of the sample, corresponding to its initial mass, and the dry mass of the sample, corresponding to its mass after halogen heating, are measured using a precision balance.

The experimental error associated with the measurement is of the order of plus or minus 2%. The solids content is calculated in the following manner:

Solids content (expressed as weight percentage) = 100 × (dry weight/wet weight).

Pulverulent phase

The pulverulent phase comprises at least:

i) perlite; and

ii) at least one spherical filler chosen from mineral fillers, organic fillers of natural origin; and

iii) at least one particulate colouring agent.

A solid composition according to the invention has a pulverulent phase content greater than or equal to 40% by weight, and more particularly ranging from 50% to 85% by weight, better still from 60% to 80% by weight, relative to the total weight of the composition.

Perlite

The perlites that may be used according to the invention are generally aluminosilicates of volcanic origin and have the composition:

- 70.0%-75.0% by weight of silica SiO₂

- 12.0%-15.0% by weight of aluminium oxide Al₂O₃

- 3.0%-5.0% of sodium oxide Na₂O

- 3.0%-5.0% of potassium oxide K₂O

- 0.5%-2% of iron oxide Fe₂O₃

- 0.2%-0.7% of magnesium oxide MgO

- 0.5%-1.5% of calcium oxide CaO

- 0.05%-0.15% of titanium oxide TiO₂.

Preferably, the perlite is milled, dried and then calibrated in a first step. The product obtained, known as perlite ore, is grey-coloured and has a size of the order of 100 µm. The perlite ore is subsequently expanded (1000°C/2 seconds) to give 30 more or less white particles. When the temperature reaches 850-900°C, the water trapped in the structure of the material evaporates and brings about the expansion of the material, relative to its original volume.

The expanded perlite particles in accordance with the invention may be obtained via the expansion process described in patent US 5 002 698. 

Preferably, the perlite particles used will be milled; in this case, they are known as Expanded Milled Perlite (EMP).

They preferably have a particle size defined by a median diameter D50 ranging from 0.5 to 50 µm and preferably from 0.5 to 40 µm.

Preferably, the perlite particles used have an untamped apparent density at 25°C ranging from 10 to 400 kg/m³ (standard DIN 53468) and preferably from 10 to 300 kg/m³.

Preferably, the perlite sold by Miyoshi Kasei under the trade name Perlite-M SZ12® is used.

Preferably, the composition of the invention comprises perlite in a content ranging from 5% to 45% by weight, and more preferentially ranging from 25% to 35% by weight relative to the total weight of the composition.

Spherical filler

A composition in accordance with the invention comprises one or more spherical filler(s) chosen from inorganic fillers and organic fillers of natural origin.

The term “organic filler of natural origin” means any filler originating from a plant and having undergone one or more chemical modifications, for example by synthesis reaction.

For the purposes of the present invention, the term “fillers” should be understood as meaning colourless or white, mineral or organic, natural or synthetic solid particles of any form, which are in an insoluble and dispersed form in the medium of the composition.

The term “spherical” is understood to mean that the particle has a sphericity index, i.e. the ratio between its largest diameter and its smallest diameter, of less than 1.2.

According to a particular form of the invention, the mean diameter of the spherical filler(s) in accordance with the invention may range from 1 to 100 µm, preferentially from 1 to 50 µm, in particular less than 30 µm, and more particularly ranging from 1 to 25 µm.

The term “mean diameter” of the particles is understood to mean the mean diameter over 50% by volume of the particles (D[0.5]) obtained using a laser diffraction particle size analyser (e.g. Mastersizer 2000® from Malvern).

The spherical fillers of the present invention may be porous or non-porous, and hollow or solid.

An inorganic spherical filler in accordance with the invention may be chosen from the group constituted of glass microbeads; silica microbeads, in particular amorphous porous silica microbeads, and mixtures thereof.

Among the glass microbeads, mention may be made of:

- those with the INCI name: Glass Beads, such as the commercial product P2015SL®

(9-11 µm) by Prizmalite;

- hollow microspheres with the INCI name: Calcium Aluminium Borosilicate, such as the commercial product Luxsil Cosmetic Microspheres® (9-13 µm) by Potters.

By way of example of spherical particles of amorphous silica, the following commercial products may be used: Silica Beads SB-150®, SB-300® or SB 700®, preferentially SB 300® from Miyoshi Kasei; the Sunsphere® or Solasphere® range from Asahi Glass AGC Si-Tech, especially Sunsphere H-51® or else Sunsphere 12L®, Sunsphere H-201®, H-52 and Sunsphere® or Solasphere H-53®; Sunsil 1308® from Sunjin; Spherica P-1500® from Ikeda Corporation; Sylosphere® from Fuji Silysia; the Silica Pearl® and Satinier® ranges from JGC Catalysts and Chemicals, more particularly Satinier M13® and Satinier M16® silicas, the MSS-500® silicas from Kobo, and more particularly MSS-500-20N®, and also Silica Shells® from Kobo.

The organic spherical fillers of natural origin may be chosen from spherical cellulose beads and/or microcrystalline celluloses in the form of spheres, and mixtures thereof. The cellulose beads which can be used are not limited by the type of cellulose, such as cellulose I, cellulose II or the like.

Among the cellulose microbeads, mention may be made of the commercial products Cellulose Beads USF® (4-7 µm), Cellulose Beads D-10® (<15 µm), Cellulose Beads D-30® (<30 µm) and Cellulose Beads D-100® (<100 µm) sold by Daito.

More particularly, the composition comprises at least one spherical filler chosen from the glass microbeads with the INCI name: Calcium Aluminium Borosilicate, porous amorphous silica microbeads, and mixtures thereof.

Preferably, the composition of the invention comprises the spherical fillers(s) in a total amount ranging from 0.5% to 10% by weight, and more preferentially ranging from 1% to 5% by weight relative to the total weight of the composition.

Additional fillers

According to one particular form, the composition may comprise at least one additional filler.

In particular, the additional fillers may be chosen from powders of N-(C₈-C₂₂)acyl amino acid, boron nitride, magnesium stearate and mixtures thereof.

Among the N-(C₈-C₂₂)acyl amino acid powders, use will preferably be made of N-lauroyl lysine, such as the commercial product Amihope LL® sold by Ajinomoto.

Boron nitride

There are a plurality of polymorphic forms of boron nitride:

- hexagonal-form boron nitrides (denoted h-BN),

- rhombohedral-form boron nitrides (denoted r-BN),

- amorphous-form boron nitrides (denoted a-BN),

- turbostratic boron nitrides (denoted t-BN),

- cubic-form boron nitrides (denoted c-BN), and

- wurtzite-type hexagonal-form boron nitrides (denoted w-BN).

Hexagonal-form boron nitride h-BN has a “hexagon sheet” structure, formed by the ABAB-type stacking of BN planes which are perfectly superimposed from one plane to another by virtue of the difference in chemical nature of the elements B and N.

According to a particular form of the invention, use will be made of boron nitride particles having a platelet shape and a hexagonal form (denoted h-BN).

Preferentially, the boron nitride particles have an average particle size ranging from 0.1 to 25 µm, preferably from 0.3 to 15 µm.

The particle size is measured according to a method of distribution by laser scattering with a machine such as a Microtrac® machine from Nikkiso or a 3042407 16 Mastersizer® machine from Malvern, in particular by measuring the D[10], D[50] and D[90] values. D[10] represents the maximum size exhibited by 10% by volume of the particles. D[50] represents the maximum size exhibited by 50% by volume of the particles. D[90] represents the maximum size exhibited by 90% by volume of the particles.

The boron nitride particles in accordance with the invention may be chosen from the following commercial products: RonaFlair Boroneige SQ-6® sold by Merck, SP2® and SP8® sold by Saint Gobain Ceramics, the Softouch Boron Nitride CC6657®, CC6058®, CC6059® products sold by Momentive Performance Materials.

Preferably, the composition of the invention comprises the additional filler(s) in a total amount ranging from 0.5% to 10% by weight, and more preferentially ranging from 1% to 5% by weight relative to the total weight of the composition.

Residual volatile solvent

Preferentially, the composition of the invention comprises less than 0.5% by weight of residual volatile solvent(s) derived from the wet preparation process, better still less than 0.1% by weight relative to the total weight of the composition.

The volatile solvents can be chosen from water, C₂-C₄ monoalcohols, for instance ethanol or isopropanol, ethers such as dicaprylyl ether, cyclic or linear volatile silicone oils and volatile hydrocarbon-based oils, for instance C₈-C₁₆ isoparaffins such as isododecane. Preferentially, isoparaffins such as isododecane will be used.

Oily phase

The composition of the invention comprises an oily phase. Said phase is liquid (in the absence of structuring agent) at ambient temperature (20-25°C). It is organic and water-immiscible.

The oily phase (or fatty phase) of the compositions according to the invention comprises at least one non-volatile oil and optionally additional oils, and also ingredients that are soluble or miscible in oils. It may be constituted of a single oil or of a mixture of several oils.

The term “hydrocarbon-based oil” refers to an oil mainly containing carbon and hydrogen atoms and possibly one or more functions chosen from hydroxyl, ester, ether and carboxylic functions.

The term “oil” refers to any fatty substance that is in liquid form at ambient temperature (20-25°C) and at atmospheric pressure. These oils may be of plant, mineral or synthetic origin.

For the purposes of the present invention, the term “silicone oil” is understood to mean an oil comprising at least one Si-O group, particularly organosiloxane.

The non-volatile oils may be chosen from the group constituted of non-volatile hydrocarbon-based oils, non-volatile silicone oils, and mixtures thereof.

The additional oils may be chosen from the group constituted of volatile hydrocarbon-based oils, volatile silicone oils, and mixtures thereof.

For the purposes of the invention, the term “volatile oil” is understood to mean any oil capable of evaporating on contact with the skin in less than one hour, at ambient temperature and atmospheric pressure. The volatile oil is a volatile cosmetic compound, which is liquid at ambient temperature, having in particular a non-zero vapour pressure, at ambient temperature and atmospheric pressure, in particular having a vapour pressure ranging from 2.66 Pa to 40 000 Pa, especially ranging from 2.66 Pa to 13 000 Pa, and more particularly ranging from 2.66 Pa to 1300 Pa.

The term “non-volatile oil” refers to an oil that remains on the skin or the keratin fibre at ambient temperature and atmospheric pressure for at least several hours and that notably has a vapour pressure of less than 2.66 Pa, preferably less than 0.13 Pa. By way of example, the vapour pressure may be measured via the static method or via the effusion method by isothermal thermogravimetry, depending on the vapour pressure (OECD standard 104).

The oily phase is present in the composition of the invention in an amount of at least 10.0% by weight, preferably ranging from 10% to 30% by weight relative to the total weight of the composition.

Non-volatile hydrocarbon-based oils

As examples of non-volatile hydrocarbon-based oils that may be used in the invention, mention may be made of:

- hydrocarbon-based oils of animal origin, such as perhydrosqualene;

- linear or branched hydrocarbons, of mineral or synthetic origin, such as liquid paraffins and derivatives thereof, petroleum jelly, polydecenes, polybutenes, polyisobutenes, which are optionally hydrogenated such as Parleam, or squalane;

- synthetic ethers containing from 10 to 40 carbon atoms, such as dicaprylyl ether;

- triglycerides constituted of fatty acid esters of glycerol, the fatty acids of which may in particular have chain lengths ranging from C₄ to C₃₆, and notably from C₁₈ to C₃₆, these oils possibly being linear or branched, and saturated or unsaturated; these oils may notably be heptanoic or octanoic triglycerides, wheatgerm oil, sunflower oil, grapeseed oil, sesame seed oil (820.6 g/mol), corn oil, apricot oil, castor oil, shea oil, avocado oil, olive oil, soybean oil, sweet almond oil, palm oil, rapeseed oil, cottonseed oil, hazelnut oil, macadamia oil, jojoba oil, alfalfa oil, poppy oil, pumpkin oil, marrow oil, blackcurrant oil, evening primrose oil, millet oil, barley oil, quinoa oil, rye oil, safflower oil, candlenut oil, passionflower oil or musk rose oil; shea oil; or alternatively caprylic/capric acid triglycerides, for instance those sold by Stéarinerie Dubois or those sold under the names Miglyol 810®, 812® and 818® by Dynamit Nobel;

- linear aliphatic hydrocarbon esters of the formula RCOOR’ in which RCOO is a carboxylic acid residue containing from 2 to 40 carbon atoms and R’ is a hydrocarbon chain containing from 1 to 40 carbon atoms, such as cetostearyl octanoate, esters of isopropyl alcohol such as isopropyl myristate, isopropyl palmitate, ethyl palmitate, 2-ethylhexyl palmitate, isopropyl stearate or isostearate, isostearyl isostearate, octyl stearate, diisopropyl adipate, heptanoates, and in particular isostearyl heptanoate, octanoates, decanoates or ricinoleates of alcohols or polyalcohols such as propylene glycol dioctanoate, cetyl octanoate, tridecyl octanoate, 4-diheptanoate and 2-hexyl ethyl palmitate, C₁₂-C₁₅ alkyl benzoate, hexyl laurate, neopentanoic acid esters such as isodecyl neopentanoate, isotridecyl neopentanoate, isostearyl neopentanoate, octyl-2-docecyl neopentanoate, isononanoic acid esters such as isononyl isononanoate, isotridecyl isononanoate, octyl isononanoate, oleyl erucate, lauroyl isopropyl sarcosinate, diisopropyl sebacate, isocetyl stearate, isodecyl neopentanoate, isostearyl behenate;

- polyesters obtained by condensation of unsaturated fatty acid dimer and/or trimer and of diol, such as those described in patent application FR 0 853 634, in particular such as of dilinoleic acid and of 1,4-butanediol. Mention may notably be made in this respect of the polymer sold by Biosynthis under the name Viscoplast 14436H® (INCI name: Dilinoleic Acid/Butanediol Copolymer) or else copolymers of polyols and of diacid dimers, and esters thereof, such as Hailuscent ISDA®,

- dialkyl carbonates, the two alkyl chains possibly being identical or different, such as dicaprylyl carbonate sold under the name

Cetiol CC® by Cognis;

- esters of linear fatty acids having a total carbon number ranging from 35 to 70, such as pentaerythrityl tetrapelargonate,

- aromatic esters, such as tridecyl trimellitate, C₁₂-C₁₅ alkyl benzoates, the 2-phenylethyl ester of benzoic acid, or butyloctyl salicylate,

- esters and polyesters of diol dimer and of monocarboxylic or dicarboxylic acid, such as esters of diol dimer and of fatty acid and esters of diol dimer and of dicarboxylic acid dimer, such as Lusplan DD-DA5® and Lusplan DD-DA7® sold by Nippon Fine Chemical and described in patent application US 2004-175 338, the content of which is incorporated into the present application by reference;

- fatty alcohols containing from 12 to 26 carbon atoms, for instance octyldodecanol, 2-butyloctanol, 2-hexyldecanol, 2-undecylpentadecanol and oleyl alcohol;

- dialkyl carbonates, the two alkyl chains possibly being identical or different, such as dicaprylyl carbonate sold under the name

Cetiol CC® by Cognis;

- and mixtures thereof.

Non-volatile silicone oils

As examples of non-volatile hydrocarbon-based oils that may be used in the invention, mention may be made of:

- phenyl silicone oils, for instance phenyl trimethicones, phenyl dimethicones, phenyltrimethylsiloxydiphenylsiloxanes, diphenyl dimethicones, diphenylmethyldiphenyltrisiloxanes and 2-phenylethyl trimethyl-siloxysilicates; and

- polydimethylsiloxanes (INCI name: Dimethicone) with a viscosity at 25°C from 50 to 500 mm²/s (cSt), especially 100 cSt, such as the commercial products sold under the names Belsil DM 100® from Wacker, Dowsil SH 200 Fluid® 100 cSt and Xiameter PMX-200 Silicone Fluid® 100 CS® from Dow Corning;

- mixtures thereof.

According to a particular form, the non-volatile oil(s) is (are) chosen from polydimethylsiloxanes with a viscosity at 25°C ranging from 50 to 500 mm²/s, hydrogenated polyisobutenes, C₁₂-C₁₅ alkyl benzoate, and mixtures thereof.

According to one particular form, the non-volatile oil(s) is (are) present in the composition of the invention in an amount of at least 10.0% by weight, preferably ranging from 10% to 30% by weight relative to the total weight of the composition.

Volatile additional oils

The composition according to the invention may additionally comprise at least one volatile oil in an amount of less than or equal to 0.5% by weight, preferably less than or equal to 0.1% by weight relative to the total weight of the composition.

In particular, the volatile oil(s) present in the composition of the invention are residual and are derived from the wet process for production of the composition.

The volatile oils may be chosen from hydrocarbon-based volatile oils and silicone volatile oils, and mixtures thereof.

By way of example of a volatile hydrocarbon-based oil that can be used in the invention, mention may be made of volatile hydrocarbon-based oils chosen from hydrocarbon-based oils containing from 8 to 16 carbon atoms, and especially C₈-C₁₆ isoalkanes of petroleum origin (also known as isoparaffins), for instance isododecane (also known as 2,2,4,4,6-pentamethylheptane), isodecane and isohexadecane, for example the oils sold under the trade names Isopar or Permethyl, branched C₈-C₁₆ esters, isohexyl neopentanoate, and mixtures thereof. Other volatile hydrocarbon-based oils, such as petroleum distillates, in particular those sold under the name Shell Solt by Shell, can also be used; volatile linear alkanes, such as those described in the patent application DE10 2008 012 457 from Cognis.

Mention may be made, as volatile silicone oils, of volatile linear or cyclic silicone oils, in particular those having a viscosity ≤ 8 centistokes (8 mm²/s) and having in particular from 2 to 7 silicon atoms, these silicones optionally comprising alkyl or alkoxy groups having from 1 to 10 carbon atoms. As volatile silicone oils that may be used in the invention, mention may notably be made of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, heptamethylhexyltrisiloxane, heptamethyloctyltrisiloxane, hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetrasiloxane and dodecamethylpentasiloxane, and mixtures thereof.

Preferably, the composition according to the invention comprises isododecane in an amount of less than or equal to 0.5% by weight, preferably less than or equal to 0.1% by weight relative to the total weight of the composition.

Amorphous hydrocarbon-based block copolymer

The composition according to the invention comprises at least one amorphous hydrocarbon-based block copolymer, preferably a block copolymer that is soluble or dispersible in the oily phase.

Such a copolymer may thus serve as gelling agent for this oily phase.

The hydrocarbon-based block copolymer may especially be a diblock, triblock, multiblock, radial or star copolymer, or mixtures thereof.

Such hydrocarbon-based block copolymers are described in patent application US-A-2002/005 562 and in patent US-A-5 221 534.

The copolymer can exhibit at least one block, the glass transition temperature of which is preferably less than 20°C, preferably less than or equal to 0°C, preferably less than or equal to -20°C and more preferably less than or equal to -40°C. The glass transition temperature of said block can be between -150°C and 20°C, in particular between -100°C and 0°C.

The hydrocarbon-based block copolymer present in the composition according to the invention is preferably an amorphous copolymer formed by polymerization of an olefin. The olefin can in particular be an ethylenically unsaturated monomer.

Mention may be made, as examples of olefins, of ethylenic carbide monomers, having in particular one or two ethylenic unsaturations and having from 2 to 5 carbon atoms, such as ethylene, propylene, butadiene, isoprene or pentadiene.

Advantageously, the hydrocarbon-based block copolymer is an amorphous block copolymer of styrene and of olefin.

Block copolymers comprising at least one styrene block and at least one block comprising units chosen from butadiene, ethylene, propylene, butylene and isoprene or a mixture thereof are notably preferred.

According to a preferred embodiment, the hydrocarbon-based block copolymer is hydrogenated to reduce the residual ethylenic unsaturations after the polymerization of the monomers.

In particular, the hydrocarbon-based block copolymer is a copolymer, optionally hydrogenated, containing styrene blocks and ethylene/C3-C4 alkylene blocks.

Mention may be made, as diblock copolymers, which are preferably hydrogenated, of styrene-ethylene/propylene copolymers, styrene-ethylene/butadiene copolymers or styrene-ethylene/butylene copolymers. Diblock polymers are notably sold under the name Kraton® G1701E by Kraton Polymers.

Mention may be made, as triblock copolymers, which are preferably hydrogenated, of styrene-ethylene/propylene-styrene copolymers, styrene-ethylene/butadiene-styrene copolymers, styrene-ethylene/butylene-styrene copolymers, styrene-isoprene-styrene copolymers or styrene-butadiene-styrene copolymers. Triblock polymers are sold in particular under the names Kraton® G1650, Kraton® G1652, Kraton® G1657®, Kraton® D1101, Kraton® D1102, Kraton® D1160 by Kraton Polymers.

According to a preferred embodiment of the present invention, the hydrocarbon-based block copolymer is a hydrogenated styrene-ethylene/butylene-styrene triblock copolymer with the INCI name: Hydrogenated Styrene/Butadiene Copolymer such as the commercial product Ellamera TER-SET 503® sold by Kraton Polymers.

Preferably, a composition according to the invention comprises a content of from 0.5% to 5% by weight and better still from 0.5% to 2% by weight of active material of hydrocarbon-based block copolymer(s) relative to the total weight of the composition.

Particulate colouring agent

The particulate colouring agent according to the invention is preferably chosen from pigments, pearlescent agents, reflective particles, and mixtures thereof.

A composition according to the invention may comprise a total content of particulate colouring agent(s) ranging from 5% to 40% by weight, preferably ranging from 10% to 30% by weight relative to the total weight of the composition.

Pigments

The term “pigments” should be understood as meaning white or coloured, mineral or organic particles of any shape, which are insoluble in the physiological medium, and which are intended to colour the composition.

The pigments may be white or coloured, and mineral and/or organic.

Among the mineral pigments, mention may be made of titanium dioxide, optionally surface-treated, zirconium oxide or cerium oxide, and also zinc oxide, (black, yellow or red) iron oxide or chromium oxide, manganese violet, ultramarine blue, chromium hydrate and ferric blue, and metal powders, for instance aluminium powder and copper powder.

The organic pigments may be chosen from the materials below, and mixtures thereof:

- cochineal carmine,

- organic pigments of azo dyes, anthraquinone dyes, indigoid dyes, xanthene dyes, pyrene dyes, quinoline dyes, triphenylmethane dyes or fluoran dyes.

Among the organic pigments, mention may be made in particular of the D&C certified pigments known under the following names: D&C Blue No. 4, D&C Brown No. 1, D&C Green No. 5, D&C Green No. 6, D&C Orange No. 4, D&C Orange No. 5, D&C Orange No. 10, D&C Orange No. 11, D&C Red No. 6, D&C Red No. 7, D&C Red No. 17, D&C Red No. 21, D&C Red No. 22, D&C Red No. 27, D&C Red No. 28, D&C Red No. 30, D&C Red No. 31, D&C Red No. 33, D&C Red No. 34, D&C Red No. 36, D&C Violet No. 2, D&C Yellow No. 7, D&C Yellow No. 8, D&C Yellow No. 10, D&C Yellow No. 11, FD&C Blue No. 1, FD&C Green No. 3, FD&C Red No. 40, FD&C Yellow No. 5, FD&C Yellow No. 6.

The chemical materials corresponding to each of the organic dyestuffs mentioned previously are mentioned in the International Cosmetic Ingredient Dictionary and Handbook, 1997 edition, pages 371 to 386 and 524 to 528, published by The Cosmetic, Toiletry and Fragrance Association, the content of which is incorporated into the present patent application by reference.

Use will preferably be made of pigments chosen from

- titanium dioxides (CI 77891) such as the commercial product Hombitan FF Pharma® sold by Venator,

- red iron oxides (CI 77491) such as the commercial product Sunpuro Red Iron oxide C33-8001® sold by Sun,

- yellow iron oxides (CI 77492) such as the commercial product Sunpuro Yellow Iron oxide C33-9001® sold by Sun,

- black iron oxides (CI 77499) such as the commercial product Sunpuro Black Iron oxide C33-7001® sold by Sun, and

- mixtures thereof, such as the mixture of red and black iron oxides sold under the trade name Unipure Red LC 383® by Sensient.

Pearlescent agents

The term “pearlescent agents” should be understood as meaning coloured particles of any form, which may or may not be iridescent, notably produced by certain molluscs in their shell, or alternatively synthesized, and which have a colour effect via optical interference.

Examples of pearlescent agents that may be mentioned include pearlescent pigments such as titanium mica coated with an iron oxide, mica coated with bismuth oxychloride, titanium mica coated with chromium oxide, and pearlescent pigments based on bismuth oxychloride. They may also be mica particles, at the surface of which are superposed at least two successive layers of metal oxides and/or of organic dyestuffs.

The pearlescent agents may more particularly have a yellow, pink, red, bronze, orangey, brown, green, blue, violet and/or coppery colour or glint.

As illustrations of pearlescent agents that may be introduced into the composition, mention may be made of the gold-coloured pearlescent agents sold especially by Engelhard under the name Brilliant Gold 212G® (Timica), Gold 222C® (Cloisonne), Sparkle Gold® (Timica), Gold 4504® (Chromalite) and Monarch gold 233X (Cloisonne); the bronze pearlescent agents sold especially by Merck under the name Bronze Fine® (17384) (Colorona) and Bronze® (17353) (Colorona) and by Engelhard under the name Super bronze (Cloisonne); the orange pearlescent agents sold especially by Engelhard under the name Orange 363C® (Cloisonne) and Orange MCR® 101 (Cosmica) and by Merck under the name Passion orange (Colorona) and Matte Orange® (17449) (Microna); the brown pearlescent agents sold especially by Engelhard under the name Nu-Antique Copper 340XB® (Cloisonne) and Brown CL4509® (Chromalite); the pearlescent agents with a copper glint sold especially by Engelhard under the name Copper 340A® (Timica); the pearlescent agents with a red glint sold especially by Merck under the name Sienna Fine® (17386) (Colorona); the pearlescent agents with a yellow glint sold especially by Engelhard under the name Yellow® (4502) (Chromalite); the red pearlescent agents with a gold glint sold especially by Engelhard under the name Sunstone G012® (Gemtone); the pink pearlescent agents sold especially by Engelhard under the name Tan Opale G005® (Gemtone); the black pearlescent agents with a gold glint sold especially by Engelhard under the name Nu Antique Bronze 240 AB® (Timica); the blue pearlescent agents sold especially by Merck under the name Matte Blue® (17433) (Microna), the white pearlescent agents with a silvery glint sold especially by Merck under the name Xirona Silver®, and the golden-green pink-orange pearlescent agents sold especially by Merck under the name Indian Summer® (Xirona), and mixtures thereof.

Still as examples of pearlescent agents, mention may also be made of particles including a borosilicate substrate coated with titanium oxide.

Particles having a glass substrate coated with titanium oxide are sold in particular under the name Metashine MC1080RY® by Toyal.

Finally, mention may be made, among the examples of pearlescent agents that may also be mentioned, of polyethylene terephthalate flakes, in particular those sold by Meadowbrook Inventions under the name Silver 1P 0.004X0.004® (silver flakes).

A composition according to the invention may comprise a pearlescent content ranging from 0% to 50% by weight, preferably ranging from 0% to 20% by weight relative to the total weight of the composition.

Emulsifying non-ionic surfactants

According to a preferential form, the composition according to the invention comprises at least one emulsifying non-ionic surfactant with an HLB of less than or equal to 8.

For the purposes of the present invention, the term “emulsifying surfactant” is understood to mean an amphiphilic surface-active compound, that is to say one exhibiting two parts of different polarities. Generally, one is lipophilic (soluble or dispersible in an oily phase). The other is hydrophilic (soluble or dispersible in water). Emulsifying surfactants are characterized by the value of their HLB (Hydrophilic Lipophilic Balance), the HLB being the ratio of the hydrophilic part to the lipophilic part in the molecule. The term “HLB” is well known to a person skilled in the art and is described, for example, in “The HLB System. A Time-Saving Guide to Emulsifier Selection” (published by ICI Americas Inc.; 1984). For the non-ionic emulsifying surfactants that can be used according to the invention, the HLB will generally range from 3 to 8. The HLB of the surfactant(s) used according to the invention can be determined by the Griffin method or the Davies method.

The emulsifying surfactant(s) may be present in a content ranging from 0.05% to 5% by weight, in particular from 0.05% to 1% by weight relative to the total weight of the composition.

The surfactants preferentially used in the composition according to the invention are chosen from:

- saccharide esters and ethers such as sucrose stearate, sucrose cocoate, sorbitan stearate, sorbitan monoisostearate, sorbitan tristearate, sorbitan oleate, sorbitan sesquioleate, methylglucose isostearate, sucrose (poly)palmitostearate, sucrose laurate, sucrose palmitate, sucrose tribehenate, sucrose oleate, sucrose distearate, sucrose polylaurate, sucrose laurate and sucrose hexaerucate, and mixtures thereof, for example Arlatone 2121® sold by ICI or Span 65V® from Uniqema;

- esters of fatty acids, especially of C₈-C₂₄ and preferably of C₁₆-C₂₂, and of polyol, especially of glycerol or sorbitol, such as glyceryl stearate, sold, for example, under the name Tegin M® by Goldschmidt, polyglyceryl diisostearate, polyglyceryl isostearate, polyglyceryl monostearate, diglyceryl tetraisostearate, polyethylene glycol diisostearate, polyglyceryl-10 pentastearate, glyceryl monooleate, glyceryl laurate, such as the product sold under the name Imwitor 312® by Hüls, diethylene glycol (di)laurate, decaglyceryl pentaoleate, decaglyceryl pentadiisostearate, glyceryl caprate/caprylate, polyglyceryl-2 (iso)stearate and glyceryl (poly)ricinoleate;

- oxyalkylenated alcohols, in particular oxyethylenated and/or oxypropylenated alcohols, which may comprise from 1 to 15 oxyethylene and/or oxypropylene units, in particular ethoxylated C₈-C₂₄ and preferably C₁₂-C₁₈ fatty alcohols such as stearyl alcohol ethoxylated with 2 oxyethylene units (CTFA name: Steareth-2) such as Brij 72® sold by Uniqema, or oxyethylenated oleyl alcohol;

- fatty alcohols such as cetylstearyl alcohol;

- oxyethylenated and/or oxyproprylenated silicone compounds having, for example, from 3 to 20 oxyalkylene units and in particular oxyethylenated and/or oxyproprylenated elastomeric or non-elastomeric dimethicones; and mixtures thereof.

According to a particular form, the emulsifying non-ionic surfactant with an HLB of less than or equal to 8 is sorbitan isostearate with the INCI name: Sorbitan Isostearate such as the commercial product Span® 120 sold by Croda.

Preparation process (wet process)

The cosmetic composition according to the invention is obtained via a wet process comprising the following steps:

- the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry;

- said slurry is injected into and then formed in a container by compacting, in particular pressing and/or suction, to obtain the final compact powder.

Preferentially, a step of drying the slurry moulded in the container is also performed.

Mixing step

In this step, the components of the oily phase, the components of the pulverulent phase and the volatile solvent(s) are mixed to prepare the slurry, which is a thick suspension of the pulverulent materials in the liquid formed by the oily phase and the volatile solvent(s).

According to a first variant, the components of the pulverulent phase and those of the oily phase are premixed and, in a second step, the volatile solvent(s) will then be added to the mixture obtained.

According to a second variant, the components of the oily phase and the volatile solvent(s) are premixed and, in a second step, the components of the pulverulent phase are then added to the mixture obtained.

According to a particular form of the invention, the amount of oily phase and the amount of pulverulent phase are such that the oily phase/pulverulent phase weight ratio ranges from 20/80 to 45/55, preferably from 25/75 to 40/60.

The volatile organic solvents can be chosen from water, C₂-C₄ monoalcohols, for instance ethanol or isopropanol, ethers such as dicaprylyl ether, cyclic or linear volatile silicone oils and hydrocarbons, for instance isoparaffins such as isododecane. Preferentially, isoparaffins such as isododecane will be used.

According to the present invention, the mixing with the pulverulent phase may be performed with any type of mixer such as a Lodige mixer.

According to a particular form of the invention, the mixed powder may also undergo milling, for example with an Alpine pin mill or a cutting processor.

According to a particular form of the invention, the mixing of the volatile solvents may be performed in any suitable container such as a bowl. It may be performed in a planetary mixer. The dispersion time required is not limited and may depend on certain factors such as the type of mixer. For example, if a planetary mixer is used, the dispersion time may range from 15 to 20 minutes.

The total amount of oily phase, of pulverulent phase and of volatile solvent is not limited. According to a particular form of the invention, the weight ratio of the total amount of oily phase and pulverulent phase/amount of volatile solvent(s) may be 5/1, preferably 3/1 and more preferentially 2/1.

If necessary, degassing may be performed during the mixing step. The oily phase, the pulverulent phase and the volatile solvent(s) may be mixed in a vacuum chamber. The degassing time may depend on certain factors such as the pressure in the vacuum chamber. It may range from 15 to 20 minutes. It is preferable to stir the slurry for efficient degassing.

Forming step

In this step, the slurry is injected into and then formed in a container such as a cup or a mould by compacting, in particular pressing and/or suction. Use is preferably made of

A crucible or a cuvette may be used as container. The container may have small orifices which allow only the solvent to escape by suction.

As methods for pouring the slurry into the container, mention may be made of those by injection via the top of the container (top injection) or by injection via the rear of the container (back injection).

In the “top injection” method, the slurry is poured into the container from above the container. This method is particularly suitable for preparing multi-coloured compact powders.

In the “back injection” method, the slurry is injected via the base of the container by means of a suitable mechanism for introducing it into the container. In particular, a Pilot Back Injection machine sold by Nanyo Co. Ltd. is used.

This injection method is suitable for a wide range of compact makeup powders and is particularly suitable for obtaining a compact powder of complex form. The slurry introduced into the container is moulded by compression and/or suction. Preferably, the compression and suction are performed simultaneously.

Compacting, in particular pressing, may be performed by exerting pressure on the slurry in the container via mechanical means such as a press having a surface that may or may not be flat (possibility of relief). Suction may be performed, for example, by reducing the pressure in the container by vacuum. The compacting, in particular pressing, and suction may be repeated several times. If necessary, vibration may be applied to the container and/or the press.

Drying step

In this step, the moulded slurry is dried to obtain a compact powder free of volatile solvent or containing a very small amount of volatile solvent. By drying, the remaining volatile solvent(s) may be totally removed. The drying temperature and time depend on several factors such as the components of the composition and the type of volatile solvent used. For example, drying may be performed at a temperature of from 60 to 100°C for a time of 1 to 12 hours.

Cosmetic process

The invention also relates to a process for coating keratin materials, more particularly for making up and/or caring for keratin materials such as the skin, in particular the face or the eyelids, characterized in that it comprises the application to said keratin materials of a composition as defined previously.

Preferentially, the cosmetic composition according to the invention may be a powder, a foundation powder, a face powder or an eyeshadow.

The cosmetic composition according to the invention may be applied by means of any applicator suitable for compact powders intended to be applied to the face or to the eyelids, such as a powder puff or a brush.

Such compositions are in particular prepared according to the general knowledge of a person skilled in the art.

Assembly

According to another aspect, the invention also relates to a cosmetic assembly or kit comprising:

i) a container delimiting one or more compartment(s), said container being closed by a closing member and optionally not being leaktight; and

ii) a makeup and/or care composition in accordance with the invention, placed inside said compartment(s).

The container can, for example, be in the form of a pot or a case. The closing member may be in the form of a lid comprising a cap mounted so as to be able to move by translation or by pivoting relative to the container housing said makeup and/or care composition(s).

Said cosmetic assembly may be combined with an applicator such as a powder puff, a foam applicator or a brush.

Cosmetic additives

The composition may contain conventional cosmetic additives such as liposoluble dyestuffs, preservatives, fragrances, antioxidants, moisturizers, lipophilic active ingredients such as vitamins, lipophilic UV-screening agents.

Of course, a person skilled in the art will take care to choose the optional additional additives and/or the amount thereof such that the advantageous properties of the composition according to the invention are not, or are not substantially, adversely affected by the envisaged addition.

Liposoluble dyestuffs

A composition according to the invention may comprise at least one liposoluble dyestuff, preferably in a proportion of at least 0.01% by weight relative to the total weight of the composition.

For obvious reasons, this amount is liable to vary significantly with regard to the intensity of the desired colour effect and of the colour intensity afforded by the dyestuffs under consideration, and its adjustment clearly falls within the competence of a person skilled in the art.

For the purposes of the invention, the term “liposoluble dyestuff” means any natural or synthetic, generally organic compound, which is soluble in an oily phase or in solvents that are miscible with a fatty substance, and which is capable of imparting colour.

As liposoluble dyes that are suitable for use in the invention, mention may notably be made of synthetic or natural liposoluble dyes, for instance DC Red 17, DC Red 21, DC Red 27, DC Green 6, DC Yellow 11, DC Violet 2, DC Orange 5, Sudan red, carotenes (β-carotene, lycopene), xanthophylls (capsanthin, capsorubin, lutein), palm oil, Sudan brown, quinoline yellow, annatto and curcumin.

Cosmetic applications

The composition used according to the invention may be a composition for caring for and/or making up keratin materials, in particular the skin, the cheeks and the eyelids.

More especially, the composition according to the invention is a product for caring for and/or making up the skin, in particular the face, the cheeks or the eyelids, and more particularly a foundation powder, a face powder or an eyeshadow.

Such compositions are in particular prepared according to the general knowledge of a person skilled in the art.

Packaging and application assembly or kit

The present invention also relates to an assembly, or kit, for packaging and applying a cosmetic composition for coating keratin materials, comprising:

- a packaging device comprising said cosmetic composition for coating keratin materials as described above,

- an applicator for said composition.

According to another aspect, the invention also relates to a makeup assembly comprising:

i) an applicator

ii) a composition in accordance with the invention placed inside a container.

The container can delimit one or more compartment(s). The container can, for example, be in the form of a tube.

Such an applicator can be integral with a cap reversibly fitted to said container between a position of closure of said container and a makeup position.

In a variant, such an applicator can be irreversibly fitted to said container. Mention may be made, as examples of applicators, of those of felt or brush type which can be constituted of synthetic fibres.

It is understood that, in the context of the present invention, the percentages by weight given for a compound or a family of compounds are always expressed by weight relative to the total weight of the composition.

Throughout the patent application, the term “comprises one” should be understood as meaning “comprising at least one”, unless otherwise specified.

It is understood that the examples which follow are present by way of illustration and that they do not in any way limit the scope of the protection conferred by the present patent application.

Example 1 (invention) and Examples 1a and 1b (outside the invention) of eyeshadows

The following compositions were prepared.

Phase	Ingredients	Ex. 1 (invention)	Ex. 1a (outside the invention)	Ex. 1b (outside the invention)
A	Lauroyl Lysine (Amihope LL® – Ajinomoto)	5	5	5
	Boron nitride (Softouch Boron Nitride CC6058® – Momentive Performance Materials)	3	3	3
	Silica (Solasphere H-53®-Asahi Glass AGC SI-Tech)	3	3	3
	Calcium Aluminium Borosilicate (Luxsil Cosmetic Microspheres® – Potters)	2	2	2
	Magnesium stearate	2	2	2
	Perlite (Perlite-M SZ12® – Miyoshi Kasei	33	0	0
	Mica	0	0	33
	Talc	0	33	0
B	Titanium Dioxide (CI 77891) (Hombitan FF Pharma® – Venator)	2.25	2.25	2.25
	Yellow iron oxides (CI 77492) (Sunpuro Yellow Iron Oxide C33-9001® – Sun)	7.15	7.15	7.15
	Red Iron Oxides (CI 77491) (Sunpuro Red Iron Oxide C33-8001® – Sun)	5.2	5.2	5.2
	Black Iron Oxides (CI 77499) (Sunpuro Red Iron Oxide C33-7001® – Sun)	11	11	11
	Iron Oxides (CI 77491) (and) Iron Oxides (CI 77499) (Unipure Red LC 383® – Sensient)	3.7	3.7	3.7
C	Dimethicone 100 cSt (Belsil DM 100® – Wacker)	7	7	7
	Hydrogenated Polyisobutene	4.5	4.5	4.5
	Sorbitan Isostearate (Span-120® – Croda)	0.1	0.1	0.1
	Caprylyl glycol	0.5	0.5	0.5
	Hydrogenated Styrene/Butadiene Copolymer (Ellamera Ter-SET 503® – Kraton Polymers)	0.9	0.9	0.9
	C12-C15 Alkyl Benzoate (C12/C15 Benzoate (DUB B1215) – Stéarinerie Dubois)	9.6	9.6	9.6
	Isododecane	0.1	0.1	0.1

Protocol for preparation of the compositions 1. Preparation of phases A and B

The ingredients of phase A and the pigments of phase B were weighed in a large stainless steel crucible.

Phase A was milled in a cutting processor: 1 time 15 seconds at 1500 rpm then 3 times 1 minute at 3000 rpm.

2. Incorporation of phase C:

The ingredients of phase C (excluding isododecane) were heated (in a water bath at 75°C). When phase C was melted, it was stirred with a deflocculator until a vortex was formed (about 300 rpm) and then introduced with stirring via the lid of the cutting processor: 1 time 1 minute at 1500 rpm.

The whole mixture was milled in a cutting processor: 1 time 1 minute at 1500 rpm, then 2 times 2 minutes at 3000 rpm and 1 time 1 minute at 3000 rpm.

3. Slurry preparation:

The mixture obtained previously was diluted in a large amount of isododecane in order to obtain the desired viscosity of the powder/solvent mixture. This paste was injected via the base (back injection) into the cups by means of a Pilot Back Injection machine sold by Nanyo Co. Ltd.

4. Slurry injection:

The Back Injection machine made it possible to inject the powder-solvent mixture, or slurry, via the base of the cup and simultaneously suction off part of the dilution solvent. Throughout the injection of the product, the injection mould was placed under vacuum so as to allow the removal of isododecane which was drawn up by suction and recovered in the vacuum trap. Placing under vacuum thus made it possible to promote the filling and homogenization of the cup.

The parts back-injected were then placed in a ventilated oven at 45°C until their weight no longer changed. The product was then considered to be dry.

Examples 1c and 1d obtained by a conventional dry process (outside the invention)

The compositions of Examples 1c and 1d, identical to Compositions 1a and 1b without isododecane, were prepared as follows:

Protocol for preparing Compositions 1c and 1d by a conventional dry process

1. Preparation of phases A and B

The ingredients of phase A and the pigments of phase B were weighed in a large stainless steel crucible.

Phase A was milled in a cutting processor: 1 time 15 seconds at 1500 rpm then 3 times 1 minute at 3000 rpm.

2. Incorporation of phase C:

The ingredients of phase C excluding isododecane were heated (in a water bath at 75°C). When phase C was melted, it was stirred with a deflocculator until a vortex was formed (about 300 rpm) and then introduced with stirring via the lid of the cutting processor: 1 time 1 minute at 1500 rpm.

The whole mixture was milled in a cutting processor: 1 time 1 minute at 1500 rpm, then 2 times 2 minutes at 3000 rpm and 1 time 1 minute at 3000 rpm.

3. Powder compaction by conventional press:

The bulk mixture was loaded respecting a studied weight into a cup, itself placed in a support fitting its size. A cloth was placed on its surface followed by an impression the size of the cup. The assembly thus installed was pressed at a pressure of 40 kgf/cm² to form an eyeshadow in the form of a compacted powder.

This made it possible to obtain Example 1c (Composition 1a with conventional pressing) and Composition 1d (Composition 1b with conventional pressing).

Measurement of the impact strength: Measurement principle

The machine used to perform such a measurement, known as a Package Drop-Test machine sold by Co Pack (Italy), made it possible to perform drop tests on the solid compositions in compact powder form to measure their impact strength. The drop height was 30 cm. By means of a small ruler, the size of the support that holds the compact was set (according to the size of the crucible) and the compact was then dropped by means of compressed air that actuates the aperture of the support. The number of drops required to split the powder was measured.

The test was carried out on 5 crucibles. The drop test was considered satisfactory when the mean of the number of drops was greater than or equal to 10.

Measurement of the pick up/pay off with foam applicator

EQUIPMENT

- Caressa® foam applicator (ref1001486 – Kahn)

- Supplale Support (manufacturer: Idemistupetrochemical; composition: collagen sheet with artificial relief bonded on a fabric)

- powder sample already used at least once and not visually damaged

- Hotplate (ref PCMF400x600 – EKIUM).

Measurement principle

A piece of supplale is placed on the hotplate so as to temper it at 32°C. The product is picked up by performing three times a transverse movement, holding the applicator parallel to the surface of the powder and perpendicular to the direction of movement.

The product was then deposited on the supplale by performing three times a transverse movement, holding the applicator parallel to the surface of the supplale and perpendicular to the direction of movement. The application area was approximately 3.5 cm long and the width of the applicator

The result obtained was then graded on a scale from 0 to 5 according to the intensity relative to pre-established boundaries.

5 equivalent to very good

4 equivalent to good

3 equivalent to moderate

2 equivalent to mediocre

1 equivalent to poor

0 equivalent to impossible.

A difference of 1 is considered as significant.

Measurement of the pick up/pay off with brush

EQUIPMENT

- Eyeshadow Brush M® applicator brush – Suqqu

- Supplale® Support (manufacturer: Idemistupetrochemical; composition: collagen sheet with artificial relief bonded on a fabric) preheated on a hotplate to 32°C

- Crucible already used at least once and not visually damaged

Measurement principle

A piece of supplale was placed on the hotplate so as to temper it at 32°C.

The product was picked up by performing three times a transverse movement, holding the brush at an angle of about 45° relative to the surface of the powder and parallel to the direction of movement.

The product was then deposited on the supplale by performing three times a transverse movement, holding the brush at an angle of about 45° relative to the surface of the supplale and parallel to the direction of movement. The application area was about 3.5 cm long and the width of the brush.

The result obtained was then graded on a scale from 0 to 5 according to the intensity relative to pre-established boundaries.

5 equivalent to very good

4 equivalent to good

3 equivalent to moderate

2 equivalent to mediocre

1 equivalent to poor

0 equivalent to impossible.

A difference of 1 is considered as significant.

Evaluation of matteness

A protocol for evaluating matteness was implemented on a panel of 10 experienced individuals. The matteness is evaluated in terms of mass when the product is in its cup, and then on the skin after application.

The panel gives a score of 0 to 5.

0 corresponds to a glossy powder.

5 corresponds to a matte powder.

Evaluation of sensoriality

An evaluation protocol was implemented on a panel of 10 experienced individuals, and the result concerned:

- the texture of the powder,

- the sensoriality and in particular the softness to the touch, creaminess, slipperiness when picked up,

- the application (amount sampled, ease of application, adhesion on application),

- the makeup result: uniformity, powdery effect, coverage, colouring effect, matteness, comfort throughout a day, staying power and ease of removal of makeup of a composition according to the invention evaluated by the same individuals.

Results

The panel gives a score of 0 to 10.

0 corresponds to a powder not satisfying any of the above parameters.

10 corresponds to a powder satisfying all the above parameters.

The results of the comparative tests are shown in the table below:

Evaluations	Ex1	Ex. 1a	Ex. 1b	Ex. 1c	Ex. 1d
Pick up/pay off with foam applicator	5	2	4	1	1
Pick up/pay off with brush	5	1	3	1	1
Impact strength	15	10	10	1	1
Evaluation of matteness	5	4	2	4	2
Sensory evaluation	10	5	6	1	1

The compact powder of Example 1 showed excellent pick up/pay off qualities both with the foam applicator and with a brush, and also good impact strength and excellent matteness.

Claims (25)

1. Solid composition in the form of a compact powder, in particular comprising a physiologically acceptable medium and containing at least:
   a) an oily phase in an amount of at least 10.0% by weight relative to the total weight of the composition, said oily phase comprising at least one non-volatile oil; and
   b) a pulverulent phase in an amount of at least 40% by weight relative to the total weight of the composition, said pulverulent phase comprising at least:
   i) perlite; and
   ii) at least one spherical filler chosen from mineral fillers, organic fillers of natural origin, and mixtures thereof; and
   iii) at least one particulate colouring agent; and
   c) at least one amorphous hydrocarbon-based block copolymer; and
   d) at least one pigment;
   said composition containing no talc particle or particle of mica in free form and
   said composition being obtainable via a wet preparation process comprising the following steps:
   1) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and
   2) the slurry is injected into a container and it is formed by compacting, in particular pressing and/or suction, to obtain the composition in compact powder form.
2. Composition according to Claim 1, in which the content of pulverulent phase ranges from 50% to 85% by weight, better still from 60% to 80% by weight, relative to the total weight of the composition.
3. Composition according to Claim 1 or 2, comprising less than 0.5% by weight of residual volatile solvent(s) derived from the wet preparation process, better still less than 0.1% by weight relative to the total weight of the composition.
4. Composition according to Claim 3, in which the volatile solvent is chosen from water, C₂-C₄ monoalcohols, ethers, cyclic or linear volatile silicone oils, volatile hydrocarbon-based oils, in particular chosen from C₈-C₁₆ isoparaffins, and more particularly isododecane.
5. Composition according to any one of the preceding claims, comprising perlite in a content ranging from 5% to 45% by weight, and more preferentially ranging from 25% to 35% by weight relative to the total weight of the composition.
6. Composition according to any one of the preceding claims, in which the inorganic spherical filler in accordance with the invention is chosen from the group constituted of glass microbeads; silica microbeads, and mixtures thereof.
7. Composition according to any one of the preceding claims, in which the organic spherical filler of natural origin is chosen from spherical cellulose beads and/or microcrystalline celluloses in the form of spheres, and mixtures thereof.
8. Composition according to any one of the preceding claims, comprising the spherical filler(s) in a total amount ranging from 0.5% to 10% by weight, and more preferentially ranging from 1% to 5% by weight relative to the total weight of the composition.
9. Composition according to any one of the preceding claims, comprising at least one additional filler.
10. Composition according to Claim 9, in which the additional filler is chosen from powders of N-(C₈-C₂₂)acyl amino acid, boron nitride, magnesium stearate and mixtures thereof.
11. Composition according to Claim 9 or 10, comprising the additional filler(s) in a total amount ranging from 0.5% to 10% by weight, and more preferentially ranging from 1% to 5% by weight relative to the total weight of the composition.
12. Composition according to any one of the preceding claims, in which the oily phase is present in an amount of at least 10.0% by weight, preferably ranging from 10% to 25% by weight relative to the total weight of the composition.
13. Composition according to any one of the preceding claims, in which the non-volatile oil(s) is (are) chosen from polydimethylsiloxanes with a viscosity at 25°C ranging from 50 to 500 mm²/s, hydrogenated polyisobutenes, C₁₂-C₁₅ alkyl benzoate, and mixtures thereof.
14. Composition according to any one of the preceding claims, in which the non-volatile oil(s) is (are) present in the composition of the invention in an amount of at least 10.0% by weight, preferably ranging from 10% to 30% by weight relative to the total weight of the composition.
15. Composition according to any one of the preceding claims, in which said amorphous hydrocarbon-based block copolymer is an amorphous copolymer formed by polymerization of an olefin.
16. Composition according to any one of the preceding claims, in which said at least one amorphous hydrocarbon-based block copolymer is an amorphous block copolymer of styrene and of olefin.
17. Composition according to any one of the preceding claims, in which said amorphous hydrocarbon-based block copolymer is an optionally hydrogenated copolymer comprising styrene blocks and C₃-C₄ ethylene/alkylene blocks.
18. Composition according to any one of the preceding claims, in which the particulate colouring agent is chosen from pigments, pearlescent agents, and mixtures thereof.
19. Composition according to any one of the preceding claims, comprising a total content of particulate colouring agent(s) ranging from 5% to 40% by weight, preferably ranging from 10% to 30% by weight relative to the total weight of the composition.
20. Composition according to Claim 19, in which the pigments are chosen from
    - titanium dioxides (CI 77891),
    - red iron oxides (CI 77491),
    - yellow iron oxides (CI 77492),
    - black iron oxides (CI 77499), and
    - mixtures thereof.
21. Composition according to any one of the preceding claims, comprising at least one emulsifying non-ionic surfactant with an HLB of less than or equal to 8, in particular sorbitan isostearate with the INCI name: Sorbitan Isostearate.
22. Composition according to any one of the preceding claims, characterized in that it is in the form of a foundation powder, a face powder or an eyeshadow.
23. Cosmetic assembly or kit comprising:
    i) a container delimiting one or more compartment(s), said container being closed by a closing member and optionally not being leaktight; and
    ii) a composition as defined according to any one of Claims 1 to 22, placed inside said compartment(s).
24. Process for coating keratin materials, in particular the skin, comprising the application to said keratin materials of a composition as defined according to any one of Claims 1 to 22.
25. Process for preparing a composition as defined in any one of Claims 1 to 22, characterized in that it comprises at least the following steps:
    1) the oily phase, the amorphous hydrocarbon-based block copolymer, the pulverulent phase and at least one volatile solvent are mixed to form a slurry; and
    2) the slurry is injected into a container and it is formed by compacting, in particular pressing and/or suction, to obtain a compact powder.