JP2009137900A - Water-in-oil type solid emulsion cosmetic and method for producing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a water-in-oil type solid emulsion cosmetic having light spread in application, a fresh and youthful touch and excellent make-up lasting quality. <P>SOLUTION: The water-in-oil type solid emulsion cosmetic includes powder dispersed in an inner water phase, a powder dispersant for stably dispersing the powder into the water phase and a wax and/or gelling agent for solidifying an outer oil phase. The method for producing the water-in-oil type solid emulsion cosmetic includes (A) a process of mixing the water-phase component with the powder and the powder dispersant and (B) a process, after the process (A), of emulsifying the water-phase component and the oil-phase component added with the wax and/or gelling agent. <P>COPYRIGHT: (C)2009,JPO&amp;INPIT

Description

  The present invention relates to a water-in-oil solid emulsified cosmetic and a method for producing the same, and particularly relates to an improvement in the feeling of use of the cosmetic.

Conventionally used as a type of solid makeup cosmetics, it is generally used from solidified oil type solidified with wax, specific oily solidifying agent, hydrophobized powder, water and lipophilic surfactant There are solid water-in-oil emulsified types, specific wax esters and amphoteric surfactants, oil-in-water solid cosmetics obtained by combining higher fatty acids, etc., which are used depending on the purpose and method of use .
In general, water-in-oil emulsions with an oil phase as the outer phase and an aqueous phase as the inner phase can efficiently spread oil-soluble active ingredients such as emollient oil, oil-soluble drugs, and UV absorbers on the skin. Therefore, it is a dosage form suitable as an external preparation for skin, and is superior to the oil-in-water type in this respect. In addition, in order to improve the makeup feeling, it has been generally practiced to blend a hydrophobic powder into the outer oil phase.
JP-A-1-79104 Japanese Patent Laid-Open No. 2-88511

However, in such a conventional solid water-in-oil emulsified cosmetic, since the hydrophobized powder is dispersed in the oil phase, the powder particles are adsorbed on the solid wax in the oil phase. , May cause aggregation. Due to this agglomerate, the cosmetic material has a problem of heavy spreading during application and reduced freshness. In addition, the hydrophobized powder has a very weak oil absorption due to the treatment, and it cannot sufficiently prevent makeup slippage due to sebum and makeup.
The present invention has been made in view of the above-mentioned problems of the prior art, and provides a water-in-oil solid emulsified cosmetic that is lightly spread during application, has a fresh feel, and is excellent in makeup. Objective.

  As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that a water-in-oil solid emulsified cosmetic with a light and fresh feel can be obtained by dispersing the powder in the inner aqueous phase. It was. Moreover, it discovered that the cosmetics with high makeup with respect to sebum were obtained by mix | blending the powder which has not been hydrophobized in an aqueous phase, and came to complete this invention.

That is, the water-in-oil solid emulsified cosmetic of the present invention includes a powder dispersed in an inner aqueous phase, a powder dispersant that stably disperses the powder in an aqueous phase, a wax that solidifies an outer oil phase, and / or And a gelling agent.
In the water-in-oil solid emulsified cosmetic, the powder dispersant is selected from a nonionic surfactant, a fatty acid soap, trisodium phosphate, sodium pyrophosphate, and sodium hexametaphosphate. Is preferred.
Furthermore, in the water-in-oil solid emulsified cosmetic, it is preferable that the oil phase contains silicone oil.

Moreover, the manufacturing method of the water-in-oil type solid emulsified cosmetic of the present invention includes the following steps (A) and (B).
(A) a step of mixing an aqueous phase component, a powder and a powder dispersant;
(B) A step of emulsifying a water phase component and an oil phase component to which a wax and / or a gelling agent is added after the step (A).

  According to the present invention, it is possible to obtain a water-in-oil solid emulsified cosmetic that is lightly stretched when applied to the skin and gives a fresh feel. In addition, the cosmetic is excellent in oil absorption and is very useful in terms of having a long lasting makeup.

The water-in-oil solid emulsified cosmetic according to the present invention is based on a structure in which a continuous layer of a water-in-oil emulsion composition is solidified by a wax and / or a gelling agent, and an aqueous phase emulsified and dispersed in the continuous layer. It has a structure in which powder components are dispersed. In conventional water-in-oil emulsified cosmetics, by blending the powder component that has been blended in the oil phase into the water phase, aggregation of the wax and / or gelling agent in the continuous layer is suppressed, and the spread is light. Thus, an emulsified cosmetic with less stickiness can be obtained.
Hereinafter, each component is demonstrated along the manufacturing method of the water-in-oil type solid emulsified cosmetics concerning this invention.

The water-in-oil type solid emulsified cosmetic of the present invention comprises a step of mixing a water phase component, a powder and a powder dispersant, and an oil phase containing a water phase component and a wax and / or a gelling agent after the step. It can manufacture through the process of emulsifying a component.
Specifically, a powder component is added to a mixed solution of an aqueous phase component and a dispersant, and this is finely pulverized with a wet disperser having a high crushing force such as a bead mill to obtain a powder dispersion.
Subsequently, the dispersion is mixed with a mixture of a wax and / or gelling agent, an oil phase component, and an emulsifier, which are appropriately dissolved by heating, with a homomixer to obtain an emulsion. Furthermore, the water-in-oil type solid emulsified cosmetic of the present invention can be obtained by appropriately filling the emulsion into a container and cooling and solidifying it.
At this time, if there are powder particles having a particle size larger than the emulsified particles to be produced, a part of the powder may come out of the aqueous phase by the homomixer treatment and be adsorbed on the wax or gelling agent to be aggregated. Therefore, the average particle size of the powder needs to be smaller than the emulsified particle size. For example, when using a bead mill, the particle size of the crushed powder can be made sufficiently small by increasing the number of passes of the dispersion to the mill, and a crushed powder sufficiently smaller than the emulsified particle size can be obtained.

  The water-in-oil solid emulsified cosmetic of the present invention thus obtained is uniformly dispersed in the aqueous phase in a state where the secondary aggregates of the powder component are sufficiently crushed. For this reason, aggregates thought to be formed by adsorbing powder components on the network structure of the wax or gelling agent developed in the outer oil phase are reduced, and the emulsified cosmetic is lightly spread at the time of application and applied. It becomes a good dispersion state on the later skin.

In the above, the aqueous phase component is a component constituting the aqueous phase of the water-in-oil solid emulsified cosmetic of the present invention, and in addition to aqueous solvents such as water, cosmetics and pharmaceuticals within a range that does not impair the stability of the emulsion. For example, a water phase component that can be usually used can be blended.
As such an aqueous phase component, for example, 1,3-butylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, hexylene glycol, glycerin, diglycerin, xylitol, maltitol, maltose, D- Mannit etc. are mentioned.

  Examples of water-soluble polymers include plant polymers such as gum arabic, carrageenan, pectin, agar, quince seed (malmello), starch, and alge colloid (brown algae extract), microbial polymers such as dextran and pullulan, collagen, and casein. Animal polymers such as gelatin, starch polymers such as carboxymethyl starch and methylhydroxypropyl starch, alginic acid polymers such as sodium alginate, vinyl polymers such as carboxyvinyl polymer (such as CARBOPOL), polyoxyethylene Polymers, polyoxyethylene polyoxypropylene copolymer polymers, acrylic polymers such as sodium polyacrylate and polyacrylamide, inorganic water-soluble polymers such as bentonite, aluminum magnesium silicate, and laponite That.

  Examples of UV absorbers include benzoic acid UV absorbers such as paraaminobenzoic acid, anthranilic acid UV absorbers such as methyl anthramylate, salicylic acid UV absorbers such as octyl salicylate and phenyl salicylate, isopropyl paramethoxycinnamate, Cinnamic acid UV absorbers such as octyl paramethoxycinnamate and glyceryl di-2-methoxycinnamate mono-2-ethylhexanoate, 2,4-dihydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2- Benzophenone ultraviolet absorbers such as hydroxy-4-methoxybenzophenone-5-sulfonic acid, urocanic acid, 2- (2′-hydroxy-5′-methylphenyl) benzotriazole, 4-tert-butyl-4′-methoxybenzoyl There is methane.

Examples of the sequestering agent include sodium edetate, sodium metaphosphate, phosphoric acid and the like.
Examples of the antioxidant include ascorbic acid, α-tocopherol, dibutylhydroxytoluene, butylhydroxyanisole and the like.
Drugs include vitamin A oil, retinol, retinol palmitate, inosit, pyridoxine hydrochloride, benzyl nicotinate, nicotinamide, nicotinic acid DL-α-tocopherol, ascorbic acid magnesium phosphate, ascorbic acid 2-glucoside, vitamin D2 ( Ergocassipherol), dl-α-tocopherol 2-L ascorbic acid phosphate diester potassium salt, dl-α-tocopherol, dl-α-tocopherol acetate, pantothenic acid, biotin and other vitamins, allantoin, azulene and other anti-inflammation Agents, whitening agents such as arbutin, astringents such as zinc oxide and tannic acid, sulfur, lysozyme chloride, pyridoxine hydrochloride, γ-oryzanol and the like.
In addition to the above drugs being used in a free state, those capable of salt formation can be used in the form of an acid or base salt, and those having a carboxylic acid group can be used in the form of its ester.
The compounding quantity of the water phase component with respect to the cosmetics of this invention is 1-70 weight%, Preferably it is 3-60 weight%, More preferably, it is 5-50%. If the amount of the aqueous phase component is less than 1% by weight, a sufficient amount of powder may not be dispersed.

In the present invention, the powder refers to a powder that can be usually used in cosmetics and pharmaceuticals, and is preferably hydrophilic so that it can be stably dispersed in an aqueous system.
Such powders include, for example, inorganic powders (eg, talc, kaolin, sericite, muscovite, synthetic mica, phlogopite, red mica, biotite, lithia mica, vermiculite, magnesium carbonate, calcium carbonate, diatomaceous earth, silica Magnesium silicate, calcium silicate, aluminum silicate, barium silicate, strontium silicate, metal tungstate, silica, hydroxyapatite, zeolite, boron nitride, ceramic powder, etc.); inorganic white pigment (for example, zinc oxide, etc.); Inorganic red pigments (eg, iron titanate); inorganic purple pigments (eg, mango violet, cobalt violet, etc.); inorganic green pigments (eg, chromium oxide, chromium hydroxide, cobalt titanate, etc.); inorganic blue Pigments (eg ultramarine, bitumen, etc.); pearl pigments (eg Titanium oxide coated mica, titanium oxide coated bismuth oxychloride, titanium oxide coated talc, colored titanium oxide coated mica, bismuth oxychloride, fish scale foil, etc.); Bengala, yellow iron oxide, black iron oxide, carbon black; metal powder pigment (for example, , Aluminum powder, copper powder, etc.); organic pigments such as zirconium, barium or aluminum lake (for example, red 201, red 202, red 204, red 205, red 220, red 226, red 228, Organic pigments such as red 405, orange 203, orange 204, yellow 205, yellow 401, and blue 404, red 3, red 104, red 106, red 227, red 230, red 401, red 505, orange 205, yellow 4 and yellow 5 , Yellow No. 202, Yellow No. 203, Green No. 3 and Blue No. 1, etc.); natural colors (e.g., chlorophyll, beta-carotene, etc.) and the like, may be used alone or in combination.

  In consideration of the dispersion of the powder component in the aqueous phase, the powder component may be hydrophilized such as a hydrophobic treatment with silicone, fluorine, Teflon (registered trademark), fatty acid, fatty acid soap, lauroyl lysine, or the like. It is preferable that the process which reduces property is not performed. That is, in the present invention, it is possible to omit the hydrophobization treatment that has been conventionally required for dispersing the powder in the oil phase. Thereby, not only the touch at the time of application | coating of cosmetics becomes a fresh thing, but it also becomes possible to improve makeup | smoothness by the oil absorption property hold | maintained at powder.

  In this invention, 0.1-35 mass% is preferable with respect to cosmetics, as for the compounding quantity of the said powder component, More preferably, it is 5-30 mass%, More preferably, it is 10-25 mass%. If the blending amount of the powder component is less than 0.1% by mass, the cosmetic effect of the powder will not be sufficiently exerted, and if it exceeds 35% by mass, the powder will not disperse in the aqueous phase and will aggregate or from the aqueous phase It may jump out into the oil phase and cause a decrease in the feeling of use.

  In the present invention, the powder dispersant refers to a substance that is adsorbed on the surface of the powder component and can uniformly disperse the powder component without agglomerating in the aqueous phase component. Examples of the powder dispersant that can be applied to the present invention include aqueous dispersants commonly used in cosmetics and pharmaceuticals, such as nonionic surfactants, fatty acid soaps, condensed phosphate compounds, polycarboxylic acid compounds (polycarboxylic acid compounds). Ammonium), amino acid compounds, polyacrylic acid compounds, amines (amino alcohols, etc.) and the like. In the present invention, it is particularly preferable to use a nonionic surfactant, a fatty acid soap, or a condensed phosphate compound.

Examples of the nonionic surfactant include POE-sorbitan fatty acid esters (for example, POE-sorbitan monooleate, POE-sorbitan monostearate, POE-sorbitan monooleate, POE-sorbitan tetraoleate, etc.); POE Sorbit fatty acid esters (eg, POE-sorbite monolaurate, POE-sorbite monooleate, POE-sorbite pentaoleate, POE-sorbite monostearate, etc.); POE-glycerol fatty acid esters (eg, POE-glycerol monoester) POE-monooleate such as stearate, POE-glycerin monoisostearate, POE-glycerin triisostearate, etc.); POE-fatty acid esters (eg, POE-distearate, POE-monodiolate, ethylene glycol distearate, etc.); Pluronic Type (eg Pluronic POE • POP-alkyl ethers (eg POE • POP-cetyl ether, POE • POP-2-decyltetradecyl ether, POE • POP-monobutyl ether, POE • POP-hydrogenated lanolin, POE • POP-glycerin) Ethers, etc.); tetra-POE / tetra-POP-ethylenediamine condensates (eg, Tetronic, etc.); POE-castor oil hardened castor oil derivatives (eg, POE-castor oil, POE-hardened castor oil, POE-hardened castor oil mono) Isostearate, POE-hardened castor oil triisostearate, POE-hardened castor oil monopyroglutamic acid monoisostearic acid diester, POE-hardened castor oil maleic acid, etc .; POE-beeswallow lanolin derivatives (eg POE-sorbite beeswax) Alkanolamides (for example, coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide) POE-propylene glycol fatty acid ester; POE-alkylamine; POE-fatty acid amide; alkylethoxydimethylamine oxide; trioleyl phosphoric acid and the like.
POE-sorbitan fatty acid esters (eg POE-sorbitan monooleate, POE-sorbitan monostearate, POE-sorbitan monooleate, POE-sorbitan tetraoleate, etc.); POE sorbitan fatty acid esters (eg POE-sorbitol) Monolaurate, POE-sorbite monooleate, POE-sorbite pentaoleate, POE-sorbite monostearate, etc .; POE-glycerin fatty acid esters (eg, POE-glycerin monostearate, POE-glycerin monoisostearate) POE-monooleate such as POE-glycerin triisostearate); POE-fatty acid esters (eg POE-distearate, POE-monodiolate, ethylene glycol distearate); POE-alkyl ethers (eg POE-lauryl) Ether, POE-oleyl ether, POE- Tearyl ether, POE-behenyl ether, POE-2-octyldodecyl ether, POE-cholestanol ether, etc.); Pluronic type (eg, Pluronic etc.); POE / POP-alkyl ethers (eg, POE / POP-cetyl ether) POE / POP-2-decyltetradecyl ether, POE / POP-monobutyl ether, POE / POP-hydrogenated lanolin, POE / POP-glycerin ether, etc.); tetra-POE / tetraPOP-ethylenediamine condensates (eg, POE-castor oil hardened castor oil derivatives (for example, POE-castor oil, POE-hardened castor oil, POE-hardened castor oil monoisostearate, POE-hardened castor oil triisostearate, POE-hardened castor Oil monopyroglutamic acid monoisostearic acid diester, POE-hardened castor oil maleic acid, etc.); POE-beeswax lanolin derivatives (eg POE-sodium Rubanol beeswax etc.); alkanolamides (eg coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide etc.); POE-propylene glycol fatty acid ester; POE-alkylamine; POE-fatty acid amide; Oxide; trioleyl phosphate and the like.

Examples of the fatty acid soap include sodium laurate, sodium myristate, sodium palmitate, sodium stearate, potassium laurate, potassium myristate, potassium palmitate, potassium stearate and the like. Alternatively, caustic potash or caustic soda may be blended first and a fatty acid such as lauric acid, myristylic acid, palmitic acid, and / or stearic acid may be added thereto to act as a fatty acid soap during the preparation of the aqueous phase.
Examples of the condensed phosphoric acid compound include trisodium phosphate, sodium pyrophosphate, sodium hexametaphosphate, and the like.
The blending amount of the dispersant may be appropriately adjusted depending on the kind and amount of the powder to be applied, or the amount of the aqueous phase component, and is usually preferably about 0.02 to 5% by mass relative to the cosmetic.

In the present invention, the wax and / or gelling agent is a component that is present in the outer oil phase and solidifies the system by adjusting the viscosity of the emulsified cosmetic.
The waxes include cocoa butter, coconut oil, horse oil, hydrogenated coconut oil, palm oil, beef tallow, sheep fat, hardened castor oil and other solid oils, paraffin wax (linear hydrocarbons), and microcrystalline wax (branched saturated hydrocarbons). , Hydrocarbons such as ceresin wax, mole, montan wax, Fischer-Trops wax, beeswax, lanolin, carnauba wax, candelilla wax, rice bran wax (rice wax), gay wax, jojoba oil, nukarou, montan wax, kapok wax, bayberry wax, Shellac wax, sugarcane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, hard lanolin, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid poly Waxes such as tylene glycol and POE hydrogenated lanolin alcohol ether, higher fatty acids such as myristic acid, palmitic acid, stearic acid and behenic acid, higher alcohols such as cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol and cetostearyl alcohol Can be used, and one kind or a combination of two or more kinds can be used. Among these, a combination of a linear saturated hydrocarbon wax and a branched saturated hydrocarbon wax, or candelilla wax and rice bran wax can be preferably used. The linear saturated hydrocarbon wax and the branched saturated hydrocarbon wax are preferably blended in combination with candelilla wax, and the blending ratio (mass ratio) is more preferably the linear saturated hydrocarbon wax and the branched saturated wax. Saturated hydrocarbon wax: candelilla wax = 9: 1 to 1: 1.

Examples of gelling agents include organic modified clay minerals, 12-hydroxystearic acid, hydrogenated castor oil, starch fatty acid esters, dimethylpolysiloxane polymers, and the like, and one or a combination of two or more types is used. can do.
Further, as the wax or gelling agent, the same function as the component, that is, a film agent capable of solidifying the system in the oil phase of the emulsion (for example, silicone resin (BY11-018, DC593), silicone rubber (9045 Silicone Elastomer Blend (above Toray Dow Corning), fluorine-modified silicone resin (XS66-B8226) (GE Toshiba Silicone, etc.) may be applied.

The above wax and gelling agent can be used alone or in combination of one or more, or both from one or more, but the blending amount with respect to the total mass of the cosmetic is combined. The content is preferably 0.1 to 15% by mass, more preferably 0.5 to 10% by mass, and still more preferably 1 to 7% by mass. If the blending amount of the wax and / or gelling agent is less than 0.1% by mass, the oil phase may not be sufficiently solidified, and if it exceeds 15% by mass, the cosmetic may be too hard and the feeling of use may be reduced. is there.
In the present invention, since the powder component is dispersed in the water phase, the amount of the powder component present in the oil phase is extremely small compared to the conventional water-in-oil solid emulsified cosmetic containing the powder component in the oil phase. . Thereby, since the wax trap produced at the time of preparation of the solid emulsion is reduced, a solid emulsion cosmetic having the same hardness as the conventional one can be obtained with a smaller amount of wax and / or gelling agent. Further, since the water phase ratio is increased by reducing the amount of the wax and / or gelling agent, the freshness of the cosmetic is improved.

The oil phase component in the present invention is a component constituting the oil phase of the emulsified cosmetic, and preferably contains a liquid oil. In the present invention, the term “liquid oil” refers to oil that is normally used in cosmetics and pharmaceuticals and is liquid at room temperature (25 ° C.).
Examples of such liquid oils include avocado oil, camellia oil, macadamia nut oil, mink oil, olive oil, castor oil, jojoba oil, triglycerin, trioctanoic acid glycerin and other liquid oils, liquid paraffin, squalane, paraffin, ceresin, Hydrocarbons such as squalene, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, 12-hydroxystearic acid, isostearic acid, linoleic acid, linolenic acid and other higher fatty acids, lauryl alcohol, cetyl alcohol, stearyl Higher alcohols such as alcohol, behenyl alcohol, oleyl alcohol, monostearyl glycerol ether, monopalmityl glycerol ether, cholesterol, phytosterol, isostearyl alcohol , Isononyl isononanoate, isopropyl myristate, cetyl octanoate, octyldodecyl myristate, butyl stearate, decyl oleate, ethylene glycol dioctanoate, diisostearyl malate, trimethylolpropane trioctanoate, trimethylolpropane triisostearate, Ester oils such as pentaerythritol tetraoctanoate, glyceryl trioctanoate, glyceryl triisostearate, ethyl acetate, butyl acetate, amyl acetate, linear silicone oils such as dimethylpolysiloxane, methylphenylpolysiloxane, methylhydrogenpolysiloxane, Cyclic silicones such as decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, and octamethylcyclotetrasiloxane Etc., and may be used alone or in combination. In the present invention, it is particularly preferable to use silicone oil.

In addition to the liquid oil as described above, oily components such as natural animal and vegetable oils and synthetic oils, fat-soluble vitamins, lecithins, and fragrances can be blended in the oil phase component.
In general, the blending amount of the oil phase component in the water-in-oil solid emulsified cosmetic of the present invention is preferably 20 to 70% by mass, and the liquid oil content is preferably 50 to 97% by mass with respect to the oil phase component.

  Moreover, in this invention, the emulsifier which can generally be mix | blended with a water-in-oil type emulsion composition can be mix | blended as an emulsifier of an above-mentioned water phase component and an oil phase component. As such an emulsifier, an emulsifier having an HLB of 7 or less is preferably used. For example, sorbitan fatty acid esters such as sorbitan monolaurate, sorbitan monooleate, sorbitan monoisostearate, sorbitan tristearate; glycerol monostearate, glycerol Glycerol fatty acid esters such as monooleate, glycerol isostearate, diglycerol diisostearate, decaglyceryl pentaisostearate; polyoxyethylene such as POE (5), POE (7.5), POE (10) hydrogenated castor oil Hardened castor oil; dipolyhydroxystearate esters: polyglyceryl-2 dipolyhydroxystearate (manufactured by Cognis: PGPH), PEG30 dipolyhydroxystearate (manufactured by Unikema) High molecular weight lipophilic active agents such as Alacel P135); cetyl dimethicone copolyol [eg, “ABIL EM90” (manufactured by Goldschmidt)], polyether-modified silicone [eg, “KF6017” (manufactured by Shin-Etsu Chemical Co., Ltd.)], Polyether-based silicones such as cross-linked polyether-modified silicones [eg, “KSG series” (manufactured by Shin-Etsu Chemical Co., Ltd.)]; polyglycerin-based silicones such as polyglycerin-modified silicones and alkyl co-modified polyglycerin-modified silicones; etc. Is mentioned. In the present invention, one or two or more emulsifiers having an HLB of 7 or less can be used. In particular, it is preferable to use a polyether-based or polyglycerin-based silicone emulsifier.

  In addition, the water-in-oil solid emulsified cosmetic of the present invention can be blended with components that can be blended with cosmetics and pharmaceuticals other than the above-described components, as long as the effect thereof is not impaired. It can be widely applied to basic cosmetics such as creams and packs, makeup cosmetics such as foundations, eye shadows, eye liners, mascaras and blushers, and hair cosmetics such as hair conditioners and hair dyes.

The term “solid” or “solid” used in the present invention means that the composition or component does not exhibit fluidity at a temperature of 50 ° C. or lower, and does not exhibit significant deformation even under normal storage conditions. Indicates that there is.
EXAMPLES Hereinafter, although an Example is given and this invention is further explained in full detail, this invention is not limited at all by this. Unless otherwise specified, the blending amount is expressed in mass% with respect to the system in which the component is blended.

About the sample obtained by the prescription and manufacturing method shown to the following test example 1 and the comparative example 1, the shear stress (Pa) with respect to the shear rate (s < ^-1 >) in 25 degreeC was measured.
For the rheology measurement, a stress control type rheometer (PHYSICA MCR 300, manufactured by Paar Physica) was used, and a cone having a diameter of 25 mm and a cone angle of 2 ° C. was used for the measurement. The results are shown in FIG.

Test Example 1 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 26.5
(2) Dimethylpolysiloxane 14
(3) Liquid paraffin 3
(4) Microcrystalline wax 5
(5) Glycerol monostearate 2
(6) Powder rake 15
(7) Ion exchange water 25
(8) Glycerin 7
(9) 1,3-butylene glycol 2
(10) Trisodium phosphate 0.3
(11) Preservative 0.1
(12) Fragrance 0.1

(Production method)
(7) to (11) are heated to 80 ° C. and dissolved. Add (6) to this and disperse. Next, the mixture of (1) to (5) and (12) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

Comparative Example 1 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 26.8
(2) Dimethylpolysiloxane 14
(3) Liquid paraffin 3
(4) Microcrystalline wax 5
(5) Glycerol monostearate 2
(6) Silicone-treated powder 15
(7) Ion exchange water 25
(8) Glycerin 7
(9) 1,3-butylene glycol 2
(10) Preservative 0.1
(11) Fragrance 0.1

(Production method)
After heating (1) to (5) and (11) to 80 ° C., (6) is added and dispersed. Next, the mixture of (7) to (10) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
Silicone-treated powder was prepared according to the methods described in JP-A-63-113081 and JP-A-63-113082, 3.65 parts talc, 5 parts titanium oxide, 0.25 parts iron oxide red, 1 part iron oxide yellow, iron oxide After mixing 0.1 part of black, tetramethyltetrahydrogencyclosiloxane was reacted and then tetradecene was added.

As shown in FIG. 1, both samples had thixotropic properties in which the viscosity decreased when stirring was continued, but Test Example 1 in which the powder component was blended in the aqueous phase was compared with Comparative Example 1 in which the powder component was blended in the oil phase. In comparison, the shear stress was constantly low. From this, it can be seen that Test Example 1 shows the same change in apparent viscosity as Comparative Example 1, while the fluidity of Test Example 1 is higher. That is, Test Example 1 is considered to be very easy to extend when the sample is applied to the skin. On the other hand, Comparative Example 2 is considered to be inferior in lightness to the former because the stress is applied to the skin when extended.
This difference in shear stress between Test Example 1 and Comparative Example 1 was presumed to be due to the difference in the powder treatment and powder dispersion phase of both samples.
Therefore, in the water-in-oil type solid emulsified cosmetic according to the present invention, the powder component is dispersed in the aqueous phase by the dispersant, and this is emulsified and dispersed in the oil phase, thereby extending the spread at the time of applying the outer cosmetic. It was suggested to be light.

Next, in accordance with the above rheological measurement results, the lightness and freshness of each sample were evaluated in actual use of the cosmetics.
Evaluation Method The samples of Test Example 1 and Comparative Example 1 obtained by the above method were applied to the cheeks of 20 professional panels, and the usability was evaluated according to the following criteria. The results are shown in Table 1 below.
Evaluation (1): Lightness of spread ○: More than 15 out of 20 responded that the spread was light.
Δ: 8 to 14 out of 20 responded that the spread was light.
×: 7 or less of 20 responded that the spread was light.

Evaluation (2): Freshness during application ○: More than 15 out of 20 responded that they felt freshness during application.
Δ: 8 to 14 out of 20 responded that they feel fresh during application.
X: 7 or less of 20 people answered that they feel fresh during application.

(Table 1)
Test Example 1 Comparative Example 1
Evaluation (1): Lightness of spread ○ △
Evaluation (2): Freshness ○ △

  As shown in Table 1, Test Example 1 was superior to Comparative Example 1 in both lightness and freshness. In Comparative Example 1 in which the hydrophobized powder is dispersed in the oil phase, an emulsification system of W / O · P (P: powder, W: aqueous phase, O: oil phase) is formed. For this reason, the powder in the oil phase is adsorbed on the network structure of the solid oil (wax) that develops in the same oil phase and agglomerates this, and as a result, it is presumed that the feel of the spread was heavy and sticky at the time of application. The

On the other hand, in Test Example 1 having a P / W / O system in which an untreated powder component (not hydrophobized) is dispersed in an aqueous phase and then emulsified with an oil, a powder that causes agglomeration of wax However, since it was hardly present in the same phase as the wax, a uniform emulsion without aggregation was obtained. Therefore, it is considered that the sample of Test Example 1 could be uniformly applied to the skin with a light touch. Further, in Test Example 1, not only the stickiness and distortion due to the aggregation of the wax were observed, but also the hydrophilic powder derived from the aqueous phase was applied on the skin, so that the freshness was significantly improved during the application.
Therefore, in the present invention, a water-in-oil solid emulsified cosmetic that is excellent in lightness and freshness by spreading powder that has not been hydrophobized in the aqueous phase component in advance and then emulsifying with the oil phase component. It was recognized that the fee could be obtained.

Furthermore, a usability test was performed on the samples (solid emulsified foundation) of Test Example 2 and Comparative Example 2 below, and makeup was evaluated. The evaluation method will be described below.
Test Example 2 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 23.9
(2) Dimethylpolysiloxane 14
(3) Cetyl isooctanoate 5
(4) Microcrystalline wax 5
(5) Sorbitan monoisostearate 2
(6) Powder rake 10
(7) Ion exchange water 22
(8) Glycerin 15
(9) 1,3-butylene glycol 2
(10) Caustic potash 0.1
(11) Preservative 0.1
(12) Stearic acid 0.8
(13) Fragrance 0.1

(Production method)
(7) to (11) are heated to 80 ° C. and dissolved. (12) is added and dissolved therein, and then (6) is added and dispersed. Next, the mixture of (1) to (5) and (13) heated in advance to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

Comparative Example 2 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 24.8
(2) Dimethylpolysiloxane 14
(3) Cetyl isooctanoate 5
(4) Microcrystalline wax 5
(5) Sorbitan monoisostearate 2
(6) Silicone-treated powder 10
(7) Ion exchange water 22
(8) Glycerin 15
(9) 1,3-butylene glycol 2
(10) Preservative 0.1
(11) Fragrance 0.1

(Production method)
After heating (1) to (5) and (11) to 80 ° C., (6) is added and dispersed. Next, the mixture of (7) to (10) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
Silicone-treated powder was prepared according to the methods described in JP-A-63-113081 and JP-A-63-113082, 3.65 parts talc, 5 parts titanium oxide, 0.25 parts iron oxide red, 1 part iron oxide yellow, iron oxide After mixing 0.1 part of black, tetramethyltetrahydrogencyclosiloxane was reacted and then tetradecene was added.

Evaluation method Each sample obtained by the above method was applied to the cheeks of 20 professional panels, and the following evaluations (3) to (6) were performed on the state immediately after the application and 2 hours after the application. The results are shown in Table 1 below.

Evaluation (3): Conspicuous (immediately after application)
○: 15 or more of 20 responded that the texture is not noticeable.
Δ: 8 to 14 out of 20 responded that the texture was inconspicuous.
×: 7 or less of 20 responded that the texture was not noticeable.

Evaluation (4): Conspicuous pores (immediately after application)
○: 15 or more of 20 responded that pores were not noticeable.
Δ: 8 to 14 out of 20 responded that pores were not noticeable.
X: 7 or less of 20 responded that pores were not noticeable.

Evaluation (5): Conspicuous (2 hours after application)
○: 15 or more of 20 responded that the texture is not noticeable.
Δ: 8 to 14 out of 20 responded that the texture was inconspicuous.
×: 7 or less of 20 responded that the texture was not noticeable.

Evaluation (6): Conspicuous pores (2 hours after application)
○: 15 or more of 20 responded that pores were not noticeable.
Δ: 8 to 14 out of 20 responded that pores were not noticeable.
X: 7 or less of 20 responded that pores were not noticeable.

(Table 1)
Test Example 2 Comparative Example 2
Evaluation (3): Conspicuous (immediately after) ○ ○
Evaluation (4): Pore conspicuous (immediately after) ○ ○
Evaluation (5): Conspicuous (after 2 hours) ○ △
Evaluation (6): Conspicuous pores (after 2 hours) ○ ×

  As shown in Table 1, it was revealed that Test Example 2 was superior to Comparative Example 2 in that the hiding power of the texture and pores was maintained for a long time, and the makeup was excellent. In Test Example 2, the hydrophobized untreated powder dispersed in the aqueous phase exerts lightness on the skin to uniformly cover the texture and pores, and the oil-absorbing untreated It is thought that the state immediately after application could be maintained for a long time because the powder adsorbed sebum, which is a source of makeup loss.

On the other hand, in Comparative Example 2 in which the hydrophobized powder was blended in the oil phase, the texture and pores were covered immediately after application, but due to the low oil absorbability of the hydrophobized powder, sebum etc. The makeup loss over time was significant.
Therefore, in the water-in-oil type solid emulsified cosmetic according to the present invention, it was recognized that the makeup feeling is improved by dispersing the hydrophilic powder in the aqueous phase.

About the solid emulsification foundation obtained by the prescription and manufacturing method of the following test example 3 and comparative example 3, the shear stress (Pa) with respect to the shear rate (s- ¹ ) in 25 degreeC was measured.
For the rheology measurement, a stress control type rheometer (PHYSICA MCR 300, manufactured by Paar Physica) was used, and a cone having a diameter of 25 mm and a cone angle of 2 ° C. was used for the measurement. The results are shown in FIG.

Test Example 3 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 23.8
(2) Dimethylpolysiloxane 10
(3) Isononyl isononanoate 1
(4) Ceresin 5
(5) PEG-9 polydimethylsiloxyethyl dimethicone 2
(6) Powder rake 20
(7) Ion exchange water 25
(8) Glycerin 10
(9) 1,3-butylene glycol 2
(10) Caustic potash 0.1
(11) Preservative 0.1
(12) Palmitic acid 0.8
(13) Sodium hexametaphosphate 0.1
(14) Fragrance 0.1

(Production method)
(7) to (11) are heated to 80 ° C. and dissolved. (12) is added and dissolved therein, and then (6) is added and dispersed. Next, the mixture of (1) to (5) and (14) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

Comparative Example 3 Solid emulsion foundation (formulation) (mass%)
(1) Decamethylcyclopentasiloxane 24.8
(2) Dimethylpolysiloxane 10
(3) Isononyl isononanoate 1
(4) Ceresin 5
(5) PEG-9 polydimethylsiloxyethyl dimethicone 2
(6) Powder rake 20
(7) Ion exchange water 25
(8) Glycerin 10
(9) 1,3-butylene glycol 2
(10) Preservative 0.1
(11) Fragrance 0.1

(Production method)
(1) to (5) and (11) are heated to 80 ° C. and dissolved. Add (6) to this and disperse. Next, the mixture of (7) to (10) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

As shown in FIG. 3, at a low shear rate, the test example 3 in which the powder rake was dispersed in the aqueous phase showed a greater shear stress than the comparative example 3 in which the powder was dispersed in the oil phase. It was low. However, the shear stress of Comparative Example 3 in shear rate 2～5S ^-1 is rapidly lowered, shear stress of both samples at a shear rate of 10s ^-1 is almost the same.
From the above results, it is possible to reduce the initial shear stress when the untreated powder is dispersed in the water phase, rather than dispersing the untreated powder in the oil phase. It was revealed.

Furthermore, the foundations of Test Example 3 and Comparative Example 3 were applied to the cheeks of 20 specialist panels, and the following evaluation (7) was performed on the lightness of spreading during application. The results are shown in Table 2 below.
Evaluation (7): Lightness at the time of application ○: More than 15 out of 20 responded that the spread was light.
Δ: 8 to 14 out of 20 responded that the spread was light.
×: 7 or less of 20 responded that the spread was light.
(Table 2)
Test Example 3 Comparative Example 3
Evaluation (7): Lightness at the time of application ○ △

As shown in Table 2, the water-in-oil solid emulsified cosmetic of Test Example 3 obtained by dispersing the hydrophobized untreated powder in the aqueous phase dispersed the untreated powder together with emulsified water droplets in the oil phase. The spread at the time of application was lighter than the water-in-oil solid emulsified cosmetic of Comparative Example 3 obtained above. That is, this evaluation test result supports the above-mentioned rheology test result.
Therefore, the water-in-oil emulsified cosmetic according to the present invention is excellent in terms of lightness at the time of application.

An attempt was made to produce a water-in-oil solid emulsified cosmetic according to the formulation shown in Table 3 below. Each sample was evaluated for the presence or absence of powder agglomeration (O: no agglomeration of powder was observed, x: agglomeration of powder was observed and color fringing occurred) and hardness. About hardness, hardness ((gamma)) was measured on the following measurement conditions using the hardness meter (RHEO METER: FUDOH company make). The results are shown in Table 2.
(Measurement condition)
Load weight: 200g
Needle diameter: 5.6φ
Needle penetration speed: 2 cm / min
Needle penetration distance: 1mm
Measurement temperature: 37 ° C

(Table 3)
(Prescription) Test Example 4 Test Example 5 Test Example 6 Test Example 7 Comparative Example 4
(1) Ion exchange water 25 25 25 25 25
(2) Sodium hexametaphosphate---0.2-
(3) 1.3-butylene glycol
5 5 5 5 5
(4) Caustic potash 0.05 0.05 0.05--
(5) Methylparaben 0.1 0.1 0.1 0.1 0.1
(6) Pigment grade titanium oxide 8 8 8 8 8
(7) Fine particle titanium oxide 4 4 4 4 4
(8) Yellow iron oxide 2 2 2 2 2
(9) Red iron oxide 0.3 0.3 0.3 0.3 0.3
(10) Black iron oxide 0.1 0.1 0.1 0.1 0.1
(11) Stearic acid 0.4 0.8 1.2 − −
(12) Cyclic silicone pentamer
43.05 42.65 42.25 43.3 43.5
(13) Dimethyl silicone 2 2 2 2 2
(14) Microcrystalline wax
6 6 6 6 6
(15) PEG-11 methyl ether dimethicone
4 4 4 4 4
Presence or absence of powder aggregation ○ ○ ○ ○ ×
Hardness (RT) 132 130 50 132 123

(Production method)
(1) to (5) are heated to 80 ° C. and dissolved. The mixture of (6) to (10) is added and mixed in this, and (2) or (11) is added and dispersed. Next, the mixture of (12) to (15) previously heated to 80 ° C. is added and emulsified and dispersed. Then, it filled in the inside plate with the fluid state, and cooled to room temperature, and the target cosmetics were obtained.

All of the water-in-oil type solid emulsified cosmetics of Test Examples 4 to 7 in which a powder dispersant was blended were suitably solidified, and were excellent in ease of use such as lightness and freshness. Moreover, it became clear that the hardness of cosmetics changes with the compounding quantity of the stearic acid which forms a dispersing agent (potassium stearate) by saponification by caustic potash.
On the other hand, in Comparative Example 4 in which the dispersant was not blended, the powder aggregated in the cosmetic material, resulting in color fringing.
From this, by adding a powder dispersant in the aqueous phase, not only the aggregation of the powder is eliminated, but the hardness of the cosmetic can be controlled by the type or blending amount of the powder dispersant. It was suggested.

Although the example of formulation of the water-in-oil type solid emulsified cosmetics concerning this invention is shown below, this invention is not limited to these. In addition, unless otherwise indicated, all the numerical values in the prescription examples indicate mass%.
Formulation Example 1 Emulsified blusher (prescription) (mass%)
(1) Dimethylpolysiloxane 5
(2) Decamethylcyclopentasiloxane 8.4
(3) Cetyl isooctanoate 15
(4) Polyoxyalkylene-modified organopolysiloxane 3
(5) 12-hydroxystearic acid 6
(6) Isostearic acid diglyceride 20
(7) Distearyldimethylammonium chloride 0.2
(8) Powder rake 15
(Mixed talc 6 parts, kaolin 2 parts, iron oxide red 0.3 parts, titanium oxide 1.7 parts)
(9) Ion exchange water 25
(10) Propylene glycol 2
(11) Sodium pyrophosphate 0.2
(12) Preservative 0.1
(13) Fragrance 0.1

(Manufacturing method)
(9) to (12) are heated to 80 ° C. and dissolved. Add (8) to this and disperse. Next, the mixture of (1) to (7) and (13) previously heated to 80 ° C. is added and emulsified and dispersed. Then, it filled in the inside plate with the fluid state, and cooled to room temperature, and the target cosmetics were obtained.

Formulation Example 2 Solid Emulsion Foundation (Prescription) (mass%)
(1) Decamethylcyclopentasiloxane 24.3
(2) Dimethylpolysiloxane 10
(3) Octyl methoxycinnamate 5
(4) Microcrystalline wax 5
(5) Sorbitan monoisostearate 3
(6) Powder rake 15
(7) Ion exchange water 21
(8) Glycerin 10
(9) 1,3-butylene glycol 6
(10) Polyoxyethylene hydrogenated castor oil (40) 0.5
(11) Preservative 0.1
(12) Fragrance 0.1

(Production method)
(7) to (11) are heated to 80 ° C. and dissolved. Add (6) to this and disperse. Next, the mixture of (1) to (5) and (12) heated to 80 ° C. in advance is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

Formulation Example 3 Solid Emulsion Foundation (Prescription) (mass%)
(1) Decamethylcyclopentasiloxane 30.1
(2) Dimethylpolysiloxane 15
(3) Octyl methoxycinnamate 5
(4) Microcrystalline wax 4
(5) Paraffin wax 2
(6) Sorbitan monoisostearate 2
(7) Powder rake 10
(8) Ion exchange water 15
(9) Glycerin 10
(10) 1,3-butylene glycol 6
(11) Polyisoethylene glycerol monoisostearate 0.7
(12) Preservative 0.1
(13) Fragrance 0.1

(Production method)
(8) to (12) are heated to 80 ° C. and dissolved. Add (7) to this and disperse. Next, the mixture of (1) to (6) and (13) previously heated to 80 ° C. is added and emulsified and dispersed. Thereafter, the medium dish was filled in a fluid state and cooled to room temperature to obtain the desired cosmetic.
The powder lake is a mixture of 3.65 parts of talc, 5 parts of titanium oxide, 0.25 part of iron oxide red, 1 part of iron oxide yellow, and 0.1 part of iron oxide black.

  All of the water-in-oil type solid emulsified cosmetics according to the above Formulation Examples 1 to 3 were light in spreading at the time of application, had a fresh feel, and were excellent in makeup.

2 is a graph showing the shear stress of the water-in-oil solid emulsion composition in Example 1. FIG. 3 is a graph showing shear stress of a water-in-oil solid emulsion composition in Example 3. FIG.

Claims (4)

Powder dispersed in the inner aqueous phase;
A powder dispersant for stably dispersing the powder in an aqueous phase;
Waxes and / or gelling agents that solidify the outer oil phase;
A water-in-oil solid emulsified cosmetic comprising:   The water-in-oil according to claim 1, wherein the powder dispersant is selected from a nonionic surfactant, fatty acid soap, trisodium phosphate, sodium pyrophosphate, and sodium hexametaphosphate. Type solid emulsified cosmetics.   The water-in-oil solid emulsion cosmetic according to claim 1 or 2, wherein the oil phase contains silicone oil. The method for producing a water-in-oil solid emulsified cosmetic according to any one of claims 1 to 3, comprising the following steps (A) and (B).
(A) a step of mixing an aqueous phase component, a powder and a powder dispersant;
(B) A step of emulsifying a water phase component and an oil phase component to which a wax and / or a gelling agent is added after the step (A).

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