JP2001106858A - (Meth) acrylate resin particles and cosmetics containing the same - Google Patents

Abstract

(57) [Summary] [Problem] To obtain a cosmetic having both excellent feeling (soft feeling, sit-down feeling) and excellent effect (cleansing, massage). SOLUTION: The average particle diameter is 30 to 800 μm,
100 parts by weight of crosslinked (meth) acrylate resin particles having a compressive strength of 0.01 to 0.6 kgf / mm ² and an inorganic powder having an average particle diameter of 1/200000 to 1/200 of the resin particles The cosmetic contains 0.5 to 50% by weight of (meth) acrylate resin particles comprising 0.01 to 30 parts by weight, wherein the inorganic powder adheres to the surface of the resin particles. Solves the above problem.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to (meth) acrylate resin particles and cosmetics containing the same. More specifically, the present invention, when used in cosmetics, imparts an extremely excellent touch (soft feeling, sit-down feeling) and effect (cleansing, massage) (meta).
The present invention relates to an acrylic ester-based resin particle and a cosmetic containing the same.

[0002]

2. Description of the Related Art There have been many attempts to improve the cleansing effect and the massage effect by blending synthetic resin particles or inorganic particles in cosmetics such as facial cleansers. For example, nylon particles, polymethyl methacrylate particles, polyethylene particles,
It is known that synthetic resin particles such as fluorine resin particles or inorganic particles such as silica particles are blended in cosmetics.

However, conventionally used synthetic resin particles such as nylon particles and polymethyl methacrylate particles and inorganic particles such as silica particles have a high compressive strength and are highly irritating to the skin. Had some difficulties to use. In addition, soft particles such as fluorine resin particles and polyethylene particles can give a soft feeling to cosmetics as compared with nylon particles, polymethyl methacrylate particles, and silica particles, but in terms of cleansing effects and massage effects. It was not enough. Accordingly, an object of the present invention is to develop resin particles that are satisfactory in imparting a sufficient cleansing effect and massage effect to cosmetics and imparting a soft feeling and a crisp feeling.

[0004]

Means for Solving the Problems The inventors of the present invention have made intensive studies toward the above-mentioned problems, and as a result, have found that the surface of crosslinked (meth) acrylate resin particles having a specific average particle size and compressive strength is The present inventors have found that, when a cosmetic to which an inorganic powder having a specific average particle size is attached is contained in a cosmetic, not only an excellent cleansing effect and a massage effect, but also a soft feeling and a crisp feeling can be imparted. I came to. According to the present invention, the average particle diameter is 30.
８００800 μm, compression strength of 0.01 to 0.6 kgf / m
crosslinking is m ² (meth) acrylate resin particles (hereinafter, referred to as "resin particles") and 100 parts by weight, the inorganic powder having an average particle diameter of 1 / 200,000 to 1/200 of the resin particles (Meth) acrylate-based resin particles (hereinafter referred to as "compounding agent") comprising 0.01 to 30 parts by weight, wherein the inorganic powder adheres to the surface of the resin particles.
For short). Furthermore, according to the present invention, there is provided a cosmetic comprising the above compounding agent in an amount of 0.5 to 50% by weight.

[0005]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The resin particles used in the compounding agent of the present invention have a compressive strength of 0.01 to 0.6 kgf / mm ² . If the compressive strength is less than 0.01 kgf / mm ² , the resulting cosmetic does not feel the feel of the resin particles, so that the cosmetic cannot impart a soft feeling and a firm feeling, a cleansing effect and a massage effect, which is not preferable. On the other hand, the compressive strength is 0.6 kgf / m
Beyond m ^2, in the cosmetics obtained by using such a resin particles, although the feel of the resin particles is felt, the feeling becomes similar to a conventional synthetic resin particles, it is assumed that feel uncomfortable in use, In addition, it is not preferable because a sufficient soft feeling and a crisp feeling cannot be imparted to the cosmetic.

[0006] The compressive strength mentioned here is a value measured using a micro compression tester HCTM200 manufactured by Shimadzu Corporation. That is, when one resin particle is subjected to a compression test at a constant load speed up to a load of 1 gf, the value is calculated by the following equation from the load and the particle size when the particle size is deformed by 10%. Compressive strength (kgf / mm ² ) = 2.8 × Load (kgf)
/ {Π × particle diameter (mm) × particle diameter (mm)} The resin particles of the present invention are obtained by subjecting a (meth) acrylate-based monomer to aqueous suspension polymerization, emulsion polymerization, Although it can be obtained by polymerization by seed polymerization or dispersion polymerization, it is particularly preferable to produce by aqueous suspension polymerization. In addition, (meth) acrylic acid in the present invention means both acrylic acid and methacrylic acid.

The (meth) acrylic acid ester-based monomer is preferably an oil-soluble monomer, and the substituent forming an ester bond with (meth) acrylic acid has 1 to 1 carbon atoms.
Two (meth) acrylate monomers are preferred.
Specifically, methyl acrylate, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, 2-ethylhexyl acrylate, acrylates such as lauryl acrylate, methyl methacrylate, ethyl methacrylate, propyl methacrylate, N-butyl methacrylate,
Examples include methacrylates such as isobutyl methacrylate, 2-ethylhexyl methacrylate, and lauryl methacrylate, and these may be used alone or in combination of two or more. Among the above monomers, acrylates having 1 to 8 carbon atoms in the substituent forming an ester bond are particularly preferred. The (meth) acrylate monomer is preferably used in a proportion of 50 to 99.5% by weight based on all the monomers.

A monomer copolymerizable with a (meth) acrylate monomer, for example, a monomer having a vinyl group such as styrene, p-methylstyrene, α-methylstyrene, vinyl acetate, You may add suitably as long as the effect of this invention is not impaired. Examples of the crosslinking agent include a crosslinking monomer having a plurality of vinyl groups. For example, ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, decaethylene glycol di (Meta)
Acrylate, pentadecaethylene glycol di (meth) acrylate, pentacontaector ethylene glycol di (meth) acrylate, 1,3-butylene glycol di (meth) acrylate, 1,4 butanediol di (meth) acrylate, 1,6 hexane Diol di (meth) acrylate, (meth) acrylate, glycerin di (meth) acrylate, allyl methacrylate, trimethylolpropane tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, diethylene glycol di (meth) acrylate phthalate, caprolactone Modified dipentaerythritol hexa (meth) acrylate, caprolactone-modified hydroxypivalic acid ester neopentyl glycol diacrylate, polyester acrylate Such as urethane acrylate (meth) acrylic acid ester monomer, divinylbenzene,
Examples thereof include divinylnaphthalene and aromatic divinyl monomers which are derivatives thereof, and these may be used alone or in combination of two or more.

Among these crosslinking agents, ethylene glycol di (meth) acrylate, diethylene glycol di (meth) acrylate, triethylene glycol di (meth) acrylate, 1,3-butylene glycol di (meth) acrylate, 1,4 butanediol (Meth) acrylate-based crosslinkable monomers such as di (meth) acrylate and 1,6 hexanediol di (meth) acrylate, and caprolactone-modified dipentaerythritol hexaacrylate, caprolactone-modified hydroxypivalic acid ester neopentyl glycol diacrylate ,
Polyester acrylate has low skin irritation,
Particularly preferred. The crosslinking agent is preferably used in a proportion of 0.5 to 50% by weight based on all monomers. The composition and the mixing ratio of the (meth) acrylic acid ester monomer and the crosslinkable monomer are such that the obtained resin particles have a compressive strength of 0.01 to 0.1.
6 kgf / mm ² , preferably 0.1 to 0.4 kgf /
It is appropriately determined according to the types of both monomers so as to obtain mm ² .

[0010] In the aqueous suspension polymerization, a polymerization initiator, a dispersant, a surfactant and the like are used as necessary. Examples of the polymerization initiator include, for example, benzoyl peroxide, lauroyl peroxide, octanoyl peroxide, orthochlorobenzoyl peroxide, methyl ethyl ketone peroxide, diisopropyl peroxydicarbonate, cumene hydroperoxide, t-butyl hydroperoxide, and the like. Peroxide, 2,2′-azobisisobutyronitrile,
Oil-soluble azo compounds such as 2,2′-azobis (2,4-dimethylvaleronitrile) are exemplified. Examples of the dispersant include poorly water-soluble inorganic salts such as calcium phosphate and magnesium pyrophosphate, and water-soluble polymers such as polyvinyl alcohol, methyl cellulose, and polyvinylpyrrolidone.

Examples of the surfactant include anionic surfactants such as sodium oleate, sodium lauryl sulfate, sodium dodecylbenzenesulfonate, alkyl naphthalene sulfonate, alkyl phosphate ester salt, polyoxyethylene alkyl ether, polyoxyethylene Nonionic surfactants such as ethylene alkyl phenyl ether, polyoxyethylene fatty acid ester, sorbitan fatty acid ester, polyoxysorbitan fatty acid ester, polyoxyethylene alkylamine, and glycerin fatty acid ester; amphoteric surfactants such as lauryl dimethylamine oxide; Is mentioned.

The above-mentioned polymerization initiators, dispersants and surfactants may be used alone or in combination of two or more. The addition ratio of the polymerization initiator is preferably 0.01 to 1% by weight based on all the monomers, and the addition ratio of the dispersant is preferably 0.05 to 10% by weight based on all the monomers.
When using a surfactant, 0.005 to water
It is preferable to add about 0.2% by weight. The polymerization reaction is
After mixing the monomer phase and the aqueous phase, the temperature is raised while stirring. The reaction temperature is 40 to 90 ° C, and the reaction time is usually
It is about 1 to 10 hours. During the polymerization reaction, by controlling the mixing and stirring conditions of the monomer and water,
The average particle size of the resin particles can be appropriately adjusted.

In the present invention, the average particle diameter is from 30 μm to 8 μm.
Resin particles that are 00 μm are used. When the thickness is 30 μm or less, it is not preferable because the feeling (soft feeling, sittling) and effect (cleansing, massage) of the cosmetic cannot be sufficiently obtained. On the other hand, if the average particle size exceeds 800 μm, the feel (soft feeling, sit-down feeling) and the effect (cleansing, massage) of the cosmetic are unpreferably reduced. After the polymerization is completed, the dispersant is decomposed with an acid or the like, if necessary, and the resin is filtered, washed, dried, and crushed (crushing a lump formed by partially coagulating during drying into particles), and then classified. Particles are obtained. The compounding agent of the present invention is obtained by adhering an inorganic powder having a specific average particle diameter to the surface of the resin particles obtained as described above. Inorganic powders prevent coalescence of particles during resin particle production,
It is used for imparting a good feel to cosmetics, especially a feeling of sit-down.

The inorganic powder may be either hydrophobic or hydrophilic and includes, for example, silica, alumina, titania, zirconia, ceria, iron oxide, zinc oxide, alumina oxide and the like. Among these inorganic powders, those obtained by subjecting the surface of a hydrophilic inorganic powder to a hydrophobizing treatment are particularly preferable since the resulting compounding agent can be easily mixed with cosmetics. By using the resin particles to which the inorganic powder is adhered, that is, the compounding agent of the present invention, unexpectedly, it is possible to give the cosmetic a sharp feel.

As a method of the hydrophobic treatment, there is a method in which a hydrophilic inorganic powder is surface-treated with a surface treating agent having a hydrophilic group and a hydrophobic group under wet or dry conditions. Examples of the surface treatment agent include coupling agents such as a silane coupling agent, a titanate coupling agent, and an aluminate coupling agent; silicone oils and resins such as dimethylpolysiloxane and methylhydrogenpolysiloxane; and hydrophobic groups and hydrophilic groups. Examples include a surfactant having a group, an acrylic resin, an amino acid, and lecithin.

The resin particles used in the present invention can easily adhere an inorganic powder to the surface of the resin particles. For this reason, in the obtained cosmetics, there is no deterioration in the touch which is observed when inorganic powder is added to and mixed with resin particles having a high compressive strength, and the unique touch (soft feeling, sit-down feeling) possessed by the resin particles. Very good effects (cleansing, massage) can be exerted while utilizing the effect. The average particle diameter of the inorganic powder is preferably 1/200000 to 1/2200 of the average particle diameter of the resin particles. When the average particle size is out of the above range, a compounding agent obtained by using such an inorganic powder can obtain a cosmetic having a good touch (soft feeling, firm feeling) and an effect (cleansing, massage). It is not preferable because it cannot be done.

The inorganic powder can be added in any of a polymerization step, a filtration step, a drying step, a crushing step, and a classification step of the resin particles, or in a plurality of steps, but is added in the drying step or the crushing step. Is preferred. It is preferable to add 0.01 to 30 parts by weight of the inorganic powder to 100 parts by weight of the resin particles. If the addition amount is less than 0.01 part by weight, the feel (soft feeling, sit-down feeling) and the effect (cleansing, massage) of the cosmetic are undesirably reduced. In addition, even if the amount is more than 30 parts by weight, the feel (soft feeling, sit-down feeling) and effect (cleansing,
Massage) is not improved.

The compounding agent of the present invention may be one treated with a surface treating agent such as an oil agent, a silicone compound or a fluorine compound. Oils may be those used in cosmetics, for example, liquid paraffin, squalane, petrolatum, hydrocarbon oils such as paraffin wax, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, behenic acid , Undecylenic acid, oxystearic acid, linoleic acid, lanolin fatty acids, higher fatty acids such as synthetic fatty acids, glyceryl trioctanoate, propylene glycol dicaprate, cetyl 2-ethylhexanoate, ester oils such as isocetyl stearate, beeswax, spermaceti, Waxes such as lanolin, carnauba wax, candelilla wax, linseed oil, cottonseed oil, castor oil, egg yolk oil, oils such as palm oil, metal soaps such as zinc stearate, zinc laurate, cetyl alcohol stearyl alcohol, oleyl alcohol, etc. Fine alcohol And the like.

The method of treating the compounding agent with the oily agent is not particularly limited. For example, a dry method in which the oiling agent is added to the compounding agent and the mixture is stirred with a mixer or the like to coat the compounding agent with the oily agent, or the oily agent is ethanol or propanol , Ethyl acetate, hexane, etc., dissolved by heating, the compounding agent is added thereto, and the mixture is stirred. Then, the solvent is removed under reduced pressure or heat, and the compounding agent is coated with an oil agent by a wet method or the like. be able to. The silicone compound may be any compound used in cosmetics, such as dimethylpolysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, acryl-silicone-based graft polymer, and organic silicone resin partially crosslinked organopolysiloxane. Examples include siloxane polymers. The method of treating the compounding agent with the silicone compound is not particularly limited, and for example, the above-mentioned dry method and wet method can be used. If necessary, a baking treatment may be performed. In the case of a reactive silicone compound, a reaction catalyst or the like may be appropriately added.

The fluorine compound may be any compound as long as it is compounded in cosmetics, and examples thereof include esters having perfluoroalkyl groups, perfluoroalkylsilanes, perfluoropolyethers, and polymers having perfluoro groups. Can be The method of treating the compounding agent with the fluorine compound is not particularly limited, either, and the above-mentioned dry method and wet method can be used.
These surface treatment agents may be used alone or in combination of two or more. Further, the addition ratio of the surface treatment agent varies depending on the particle diameter of the compounding agent and the like, but is preferably 0.001 to 50% by weight based on the compounding agent.
01 to 5% by weight is particularly preferred. If the blending ratio of the surface treating agent is less than 0.001% by weight, sufficient water repellency and oil repellency cannot be obtained, and if it exceeds 50% by weight, the effect corresponding to the increase in the added amount cannot be improved. On the contrary, it is not preferable because aggregation of the compounding agent easily occurs.

The compounding agent of the present invention may contain a coloring pigment. The coloring pigment is preferably one that is sparingly soluble in the water phase and oil phase used for the polymerization reaction of the resin particles. Examples of the coloring pigment include titanium oxide, zinc oxide, zirconium oxide, magnesium oxide, iron oxide, iron hydroxide, chromium oxide, chromium hydroxide, ultramarine, navy blue, manganese violet, ultramarine purple, titanium black, carbon black, and aluminum. Powder, titanium mica, bismuth oxychloride, iron oxide treated mica titanium, navy blue treated mica titanium, carmine treated mica titanium, silica, calcium carbonate, magnesium carbonate, barium sulfate, barium silicate, calcium silicate, magnesium silicate, calcium phosphate, Inorganic pigments such as hydroxyapatite, zeolite, alumina, talc, mica, bentonite, kaolin, and sericite; aluminum lakes such as tartrazine, sunset yellow FCF, brilliant blue FCF; zirconium lakes; Rake, to Lyndon pink CN, Lithol Rubine BCA, Lake Red CBA, phthalocyanine blue, and organic pigments of permanent orange, and the like. These color pigments may be used alone or in combination of two or more.

When a coloring pigment is added to the compounding agent, its ratio is preferably about 1 to 70% by weight based on the total weight of the compounding agent. If the content is less than 1% by weight, the effect of adding the coloring pigment is poor, which is not preferable. On the other hand, when the content ratio is 70
If it exceeds 10% by weight, at the stage of producing a dispersion before polymerization,
Since the amount of the coloring pigment is too large relative to the monomer, the viscosity of the dispersion becomes high and the production of resin particles becomes difficult, which is not preferable. The method for dispersing the color pigment is not particularly limited, but the surface of the color pigment may be prepared by using a carboxylic acid, a sulfonic acid, a sulfate, a phosphate, a phosphonate, or a salt thereof, or a coupling agent such as silane, titanate, or aluminate. Is subjected to a hydrophobic treatment and then added to a polymerization system. The addition ratio of the coupling agent to the color pigment is preferably 0.1 to 30% by weight.

The apparatus for dispersing the color pigment is not particularly limited as long as it can impart sufficient dispersion energy to the dispersion system, and examples thereof include a ball mill, a sand mill, an ultrasonic disperser, and a homogenizer. In the cosmetic of the present invention, the compounding agent as described above contains 0.5 to 50% by weight.
It is contained. The method for incorporating the compounding agent into the cosmetic is not particularly limited, and a known method can be used. As cosmetics, soaps, body shampoos, facial cleansers,
Examples include a scrub face wash, a massage cream, a pre-shave lotion, and the like, but are not particularly limited as long as the effects of the present invention are recognized.

If the compounding ratio is less than 0.5% by weight, the effect of adding the compounding agent is not clearly recognized, which is not preferable. On the other hand, if the blending ratio exceeds 50% by weight, the effect corresponding to the increase in the added amount is not improved, which is not preferable. In addition, components generally used in cosmetics can be blended according to the purpose within a range that does not impair the effects of the present invention. As such components, for example, water, lower alcohols, fats and waxes, hydrocarbons, higher fatty acids, higher alcohols, sterols, fatty acid esters, metal soaps, humectants, surfactants, polymer compounds, coloring material raw materials, Fragrances, preservatives / bactericides, antioxidants, UV absorbers,
Special compounding components are included.

Examples of fats and oils and waxes include avocado oil, almond oil, olive oil, cocoa butter, tallow,
Sesame oil, wheat germ oil, safflower oil, shea butter, turtle oil, camellia oil, persic oil, castor oil, grape oil, macadamia nut oil, mink oil, egg yolk oil, mokuro, coconut oil, rosehip oil, hydrogenated oil, silicone oil , Orange luffy oil, carnauba wax, candelilla wax, whale wax,
Jojoba oil, montan wax, beeswax, lanolin and the like. Examples of hydrocarbons include liquid paraffin,
Vaseline, paraffin, ceresin, microcrystalline wax, squalane and the like.

Examples of the higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, behenic acid, undecylenic acid, oxystearic acid, linoleic acid, lanolin fatty acid, and synthetic fatty acids. As higher alcohols, for example, lauryl alcohol, cetyl alcohol, cetostearyl alcohol, stearyl alcohol, oleyl alcohol, behenyl alcohol, lanolin alcohol, hydrogenated lanolin alcohol, hexyldecanol, octyldecanol, isostearyl alcohol, jojoba alcohol, decyl And tetradecanol. Sterols include, for example, resterol, dihydrocholesterol, phytocholesterol and the like.

Examples of the fatty acid ester include ethyl linoleate, isopropyl myristate, isopropyl lanolin fatty acid, hexyl laurate, myristyl myristate, cetyl myristate, octyl dodecyl myristate, decyl oleate, octyl dodecyl oleate, and dimethyloctane. Hexyldecyl acid, cetyl octanoate, cetyl isooctanoate, decyl palmitate,
Glycerin trimyristate, glycerin tri (capryl / caprate), propylene glycol dioleate, glycerin triisostearate, glycerin triisooctanoate, cetyl lactate, myristyl lactate, diisostearyl malate and cholesteryl isostearate,
And cyclic alcohol fatty acid esters such as cholesteryl 12-hydroxystearate.

Examples of the metal soap include zinc laurate, zinc myristate, magnesium myristate, zinc palmitate, zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, zinc undecylenate and the like. Examples of the humectant include glycerin, propylene glycol, 1,3-butylene glycol, polyethylene glycol, sodium dl-pyrrolidonecarboxylate, sodium lactate, sorbitol, sodium hyaluronate, polyglycerin, xylitol, maltitol and the like. Examples of the surfactant include anionic surfactants such as higher fatty acid soaps, higher alcohol sulfates, N-acyl glutamates, phosphates, and alkyl sulfates, amine salts, and quaternary ammonium salts. Cationic surfactant, betaine type, amino acid type,
Non-ionic surfactants such as imidazoline type, lecithin and other amphoteric surfactants, fatty acid monoglyceride, propylene glycol fatty acid ester, sorbitan fatty acid ester, sucrose fatty acid ester, polyglycerin fatty acid ester, alkyl alkanolamide, ethylene oxide condensate, etc. No.

Examples of the high molecular compound include natural high molecular compounds such as gum arabic, tragacanth gum, guar gum, locust bean gum, karaya gum, iris moth, quince seed, gelatin, shellac, rosin, casein, sodium carboxymethyl cellulose, and hydroxyethyl cellulose. , Methyl cellulose, ethyl cellulose, sodium alginate, ester gum, nitrocellulose, hydroxypropyl cellulose, semi-synthetic polymer compounds such as crystalline cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, sodium polyacrylate, carboxyvinyl polymer, polyvinyl methyl ether, polyamide resin, Silicone oil, nylon particles,
Polymethyl methacrylate particles, cross-linked polystyrene particles,
Synthetic polymer compounds such as synthetic resin particles such as silicon particles, urethane particles, and polyethylene particles.

Examples of the coloring material raw materials include iron oxide, ultramarine, konjo, chromium oxide, chromium hydroxide, carbon black, manganese violet, titanium oxide, zinc oxide, talc, kaolin, mica, calcium carbonate, magnesium carbonate, and mica. Inorganic pigments such as aluminum silicate, barium silicate, calcium silicate, magnesium silicate, silica, zeolite, barium sulfate, calcined calcium sulfate (baked gypsum), calcium phosphate, hydroxyapatite, ceramic powder, azo-based, nitro-based, Examples include tar dyes such as nitroso, xanthene, quinoline, anthraquinoline, indigo, triphenylmethane, phthalocyanine, and pyrene.

The powdery raw materials such as the above-mentioned polymer compounds and coloring material raw materials may be subjected to a surface treatment in advance. Known techniques can be used as the surface treatment method, for example, oil treatment with hydrocarbon oil, ester oil, lanolin, etc., silicone treatment with dimethylpolysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, etc., perfluoroalkyl Fluorine compound treatment with ester containing group, perfluoroalkylsilane, perfluoropolyether and polymer having perfluoroalkyl group, etc., with 3-methacryloxypropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, etc. Treatment with silane coupling agent, treatment with titanium coupling agent with isopropyl triisostearoyl titanate, isopropyl tris (dioctyl pyrophosphate) titanate, treatment with metal soap, acylglutamine Amino processing by an equal, lecithin treatment with hydrogenated egg yolk lecithin, Koragen processing, polyethylene processing, moisture retention treatment, an inorganic compound treatment, and methods such as mechanochemical treatment.

Examples of the fragrance include natural fragrances such as lavender oil, peppermint oil and lime oil, and synthetic fragrances such as ethylphenyl acetate, geraniol, p-tert-butylcyclohexyl acetate and the like. Examples of the antiseptic / bactericide include methylparapene, ethylparapene, propylparapene, benzalkonium, benzethonium and the like. Examples of the antioxidant include dibutylhydroxytoluene, butylhydroxyanisole, propyl gallate, and tocopherol.

Examples of the ultraviolet absorber include inorganic absorbers such as fine titanium oxide, fine zinc oxide, fine cerium oxide, fine iron oxide, fine zirconium oxide, and the like.
Organic absorbents such as benzoic acid, p-aminobenzoic acid, anthranilic acid, salicylic acid, cinnamic acid, benzophenone, and dibenzoylmethane may be used. As special compounding ingredients, for example, hormones such as estradiol, estrone, ethinyl estradiol, cortisone, hydrocortisone, prednisone, vitamins such as vitamin A, vitamin B, vitamin C, vitamin E, citric acid, tartaric acid, lactic acid, aluminum chloride , Skin astringents such as aluminum potassium potassium, allantoinchlorohydroxyaluminum, zinc paraphenolsulfonate, zinc sulfate, cantaristic tincture, capsicum tincture, ginger tincture, assembly extract, garlic extract, hinokitiol, carpronium chloride, glyceride pentadecanoate , Vitamin E, estrogens, photosensitizers and the like, and whitening agents such as magnesium phosphate-L-ascorbate and kojic acid.

[0034]

EXAMPLES The present invention will be described below with reference to examples, but the present invention is not limited to such examples.

Example 1 Oil phase Ethyl acrylate 90 parts by weight 1,6 Hexanediol dimethacrylate 10 parts by weight 0.5 parts by weight benzoyl peroxide Aqueous phase Deionized water 400 parts by weight Polyvinyl alcohol (degree of saponification 85%) 1 part by weight Sodium lauryl sulfate 0.01 part by weight Titanium oxide 3 parts by weight Put the above oil phase and aqueous phase into a polymerization vessel equipped with a stirrer and a thermometer, and continue stirring at 60 ° C. for 6 hours to carry out suspension polymerization. Completed. After cooling, the suspension was filtered and washed, and titanium oxide (KA-10, manufactured by Titanium Industry Co., Ltd., average particle size: 0.3 μm) was added, dried, and crushed to have a compressive strength of 0.15 kgf / m.
m ² and an average particle diameter of 288 μm was obtained. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.8% by weight.

Example 2 A compounding agent was obtained in the same manner as in Example 1 except that the titanium oxide was changed to hydrophobic colloidal silica (manufactured by Nippon Aerosil Co., Ltd., average particle size: 7 nm). Scanning electron micrographs confirmed that colloidal silica had adhered to the particle surfaces.
The ash content (silica content) of this compounding agent was 2.5% by weight.

Example 3 A compounding agent was obtained in the same manner as in Example 1 except that the addition amount of titanium oxide was changed to 25 parts by weight. By scanning electron micrograph,
It was confirmed that titanium oxide was attached to the particle surface.
The ash content (titanium oxide content) of this compounding agent was 24.6% by weight.

Example 4 Example 1 was repeated except that the amount of titanium oxide was changed to 0.05 part by weight.
In the same manner as in the above, a compounding agent was obtained. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 0.046% by weight.

Example 5 Titanium oxide in Example 1 was replaced with silica (manufactured by Fuji Silysia Chemical Ltd., average particle size 1.4).
A composition was obtained in the same manner as in Example 1 except that μm) was used. Scanning electron micrographs confirmed that silica had adhered to the particle surfaces. The ash content (silica content) of this compounding agent was 2.6% by weight.

Example 6 Oil Phase Ethyl acrylate 60 parts by weight Butyl methacrylate 30 parts by weight Tetraethylene glycol dimethacrylate 10 parts by weight Lauroyl peroxide 0.5 part by weight Water phase Deionized water 400 parts by weight Calcium triphosphate 2 Parts by weight Sodium lauryl sulfate 0.02 parts by weight Titanium oxide 3 parts by weight Put the above oil phase and aqueous phase into a polymerization vessel equipped with a stirrer and thermometer, and continue stirring at 60 ° C for 6 hours to complete suspension polymerization. did. After cooling, the suspension was filtered and washed, and titanium oxide (manufactured by Teica Co., Ltd., JR-600A, average particle diameter: 0.3 μm) was added, followed by drying and pulverization to obtain a compressive strength of 0.51 kgf / m.
m ² and an average particle diameter of 295 μm was obtained. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.7% by weight.

Example 7 Oil Phase Ethyl acrylate 95 parts by weight 1,6 Hexanediol dimethacrylate 5 parts by weight 2,2′-azobis (2,4-dimethylvaleronitrile) 0.5 parts by weight Water phase deionization Water 400 parts by weight Metathesis magnesium pyrophosphate 1 part by weight Sodium lauryl sulfate 0.02 parts by weight Silicon-treated zinc oxide 3 parts by weight The above oil phase and aqueous phase are put into a polymerization vessel equipped with a stirrer and a thermometer, and heated at 60 ° C. For 6 hours to complete the suspension polymerization. After cooling, the suspension was filtered and washed, and silicon-treated zinc oxide (SI-FINEX50-LHC6 manufactured by Miyoshi Kasei Co., Ltd.) was used.
% Average particle diameter 50 nm), and dried and pulverized to obtain a spherical compounding agent having a compressive strength of 0.06 kgf / mm ² and an average particle diameter of 302 μm. Scanning electron micrographs confirmed that zinc oxide had adhered to the particle surfaces. The ash content (zinc oxide content) of this compounding agent was 2.9% by weight.

Example 8 Oil phase Ethyl acrylate 90 parts by weight 1,6 Hexanediol dimethacrylate 10 parts by weight 0.5 parts by weight benzoyl peroxide Aqueous phase Deionized water 400 parts by weight Polyvinyl alcohol (degree of saponification 85%) 6 parts by weight Sodium lauryl sulfate 0.02 parts by weight Titanium oxide 3 parts by weight Put the above oil phase and aqueous phase into a polymerization vessel equipped with a stirrer and a thermometer, and continue stirring at 60 ° C. for 6 hours to carry out suspension polymerization. Completed. After cooling, the suspension was filtered and washed, and titanium oxide (KA-10, manufactured by Titanium Industry Co., Ltd., average particle size: 0.3 μm) was added, followed by drying and pulverization to obtain a compression strength of 0.12 kgf / m.
m ² and a spherical compounding agent having an average particle diameter of 43 μm. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.9% by weight.

Example 9 Oil phase Ethyl acrylate 90 parts by weight 1,6 Hexanediol dimethacrylate 10 parts by weight Benzoyl peroxide 0.5 parts by weight Aqueous phase Deionized water 400 parts by weight Polyvinyl alcohol (degree of saponification 85%) 0.5 parts by weight Sodium lauryl sulfate 0.005 parts by weight Titanium oxide 3 parts by weight The above oil phase and aqueous phase are put into a polymerization vessel equipped with a stirrer and a thermometer, and are suspended by stirring at 60 ° C. for 6 hours. The polymerization was completed. After cooling, the suspension was filtered and washed, and titanium oxide (KA-10, manufactured by Titanium Industry Co., Ltd., average particle size: 0.3 μm) was added, dried and pulverized, and the compressive strength was 0.17 kgf / m.
m ² and an average particle diameter of 756 μm was obtained. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.8% by weight.

Comparative Example 1 A compounding agent was obtained in the same manner as in Example 1 except that titanium oxide was changed to silica (average particle diameter: 12 μm). Scanning electron micrographs confirmed that silica had adhered to the particle surfaces. The ash content (silica content) of this compounding agent was 2.3% by weight.

Comparative Example 2 A compounding agent was obtained in the same manner as in Example 1 except that the amount of titanium oxide was changed to 0.005 parts by weight. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent is 0.00
It was 48% by weight.

Comparative Example 3 Oil phase Ethyl acrylate 90 parts by weight 1,6 Hexanediol dimethacrylate 10 parts by weight 0.5 parts by weight benzoyl peroxide Aqueous phase Deionized water 400 parts by weight Polyvinyl alcohol (degree of saponification 85%) 0.5 parts by weight Sodium lauryl sulfate 0.001 parts by weight Titanium oxide 3 parts by weight The above oil phase and aqueous phase are put into a polymerization vessel equipped with a stirrer and a thermometer, and are stirred at 60 ° C. for 6 hours to suspend them. The polymerization was completed. After cooling, the suspension was filtered and washed, and titanium oxide (KA-10, manufactured by Titanium Industry Co., Ltd., average particle diameter: 0.3 μm) was added, followed by drying and pulverization to obtain a compression strength of 0.18 kgf / m.
m ² and a spherical compounding agent having an average particle size of 2015 μm. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.7% by weight.

Comparative Example 4 Oil phase Ethyl acrylate 90 parts by weight 1,6 Hexanediol dimethacrylate 10 parts by weight 0.5 parts by weight benzoyl peroxide Aqueous phase Deionized water 400 parts by weight Calcium triphosphate 10 parts by weight Lauryl sulfate Sodium 0.08 parts by weight Hydrophobic colloidal silica (average particle diameter 7 nm) 3 parts by weight The above oil phase is dispersed in the aqueous phase by a homomixer (Desktop TK homomixer manufactured by Tokushu Kika Kogyo Co., Ltd.) at 9000 rpm. After that, this dispersion was put into a polymerization vessel equipped with a stirrer and a thermometer, and stirring was continued at 60 ° C. for 6 hours to complete the suspension polymerization. After cooling, the suspension was filtered and washed, and hydrophobic colloidal silica was dividedly added before and after drying, dried, and pulverized to have a compressive strength of 0.13 kgf / mm ² and an average particle size of 0.13 kgf / mm ^2. A 5.3 μm spherical compounding agent was obtained. Scanning electron micrographs confirmed that colloidal silica had adhered to the particle surfaces. The ash content (silica content) of this compounding agent was 2.5% by weight.

Comparative Example 5 Oil phase Ethyl acrylate 30 parts by weight 30 parts by weight of butyl methacrylate 40 parts by weight of 1,6-hexanediol dimethacrylate 0.5 parts by weight of benzoyl peroxide Aqueous phase 400 parts by weight of deionized water polyvinyl Alcohol (degree of saponification: 85%) 1 part by weight Sodium lauryl sulfate 0.01 part by weight Titanium oxide 3 parts by weight The above oil phase and aqueous phase are put into a polymerization vessel equipped with a stirrer and a thermometer, and stirred at 60 ° C. for 6 hours. To complete the suspension polymerization. After cooling, the suspension was filtered and washed, and titanium oxide (manufactured by Teica, JR-600A, average particle diameter: 0.3 μm) was added, followed by drying and pulverization to obtain a compressive strength of 0.95 kgf / m.
m ² and a spherical compounding agent having an average particle diameter of 314 μm. Scanning electron micrographs confirmed that titanium oxide had adhered to the particle surfaces. The ash content (titanium oxide content) of this compounding agent was 2.6% by weight.

[Example 10] (Production of face wash cream) Oil phase Stearic acid 8.0 parts by weight Palmitic acid 5.0 parts by weight Myristic acid 10.0 parts by weight Lauric acid diethanolamide 4.0 parts by weight Lanolin 2.0 Parts by weight cetyl alcohol 3.0 parts by weight aqueous phase sodium lauryl sulfate 8.0 parts by weight glycerin 15.0 parts by weight methyl paraben 0.2 parts by weight potassium hydroxide 5.0 parts by weight purified water 34.6 parts by weight Example 1) 5.0 parts by weight Perfume 0.2 parts by weight The above oil phase and aqueous phase were each heated and dissolved at 70 ° C.
The oil phase was gradually added to the aqueous phase while stirring, and the mixture was sufficiently emulsified by a homomixer until uniform, and then stirred for a while. Thereafter, the mixture was cooled to 50 ° C., and after adding a compounding agent and a fragrance, the mixture was uniformly mixed and further cooled to obtain a face wash cream.

Example 11 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Example 2.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 12 Example 1 was repeated except that the compounding agent in Example 10 was replaced with the one obtained in Example 3.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 13 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Example 4.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 14 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Example 5.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 15 Example 1 was repeated except that the compounding agent in Example 10 was replaced with the one obtained in Example 6.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 16 Example 1 was repeated except that the compounding agent in Example 10 was replaced with the one obtained in Example 7.
In the same manner as in Example No. 0, a face wash cream was obtained.

Example 17 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Example 8.
In the same manner as in Example No. 0, a face wash cream was obtained.

Comparative Example 6 A face wash cream was obtained in the same manner as in Example 10, except that the compounding agent in Example 10 was changed to fluororesin particles (average particle diameter: 306 μm).

Comparative Example 7 A face wash cream was obtained in the same manner as in Example 10, except that the compounding agent in Example 10 was changed to polyethylene particles (average particle diameter: 312 μm).

Comparative Example 8 A face wash cream was obtained in the same manner as in Example 10, except that the compounding agent in Example 10 was changed to PMMA particles (average particle size: 292 μm).

Comparative Example 9 Example 10 was repeated except that the compounding agent in Example 10 was replaced by PMMA particles (average particle diameter: 292 μm) whose surface was coated with titanium oxide (average particle diameter: 0.3 μm). Similarly, a facial cleansing cream was obtained.

Comparative Example 10 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Comparative Example 1.
In the same manner as in Example No. 0, a face wash cream was obtained.

Comparative Example 11 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Comparative Example 2.
In the same manner as in Example No. 0, a face wash cream was obtained.

Comparative Example 12 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Comparative Example 3.
In the same manner as in Example No. 0, a face wash cream was obtained.

Comparative Example 13 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Comparative Example 4.
In the same manner as in Example No. 0, a face wash cream was obtained.

Comparative Example 14 Example 1 was repeated except that the compounding agent in Example 10 was changed to that obtained in Comparative Example 5.
In the same manner as in Example No. 0, a face wash cream was obtained.

[Example 18] (Production of lotion) Oil phase Stearic acid 2.0 parts by weight Cetyl alcohol 1.2 parts by weight Vaseline 5.0 parts by weight Liquid paraffin 11.0 parts by weight Polyoxyethylene oleyl ether (20E. O.) 3.0 parts by weight Polyoxyethylene sorbitan monolaurate (5EO) 3.0 parts by weight Aqueous phase propylene glycol 4.0 parts by weight Triethanolamine 1.0 parts by weight Methyl paraben 0.2 parts by weight Purification Water 64.4 parts by weight Compounding agent (Example 9) 5.0 parts by weight Fragrance Appropriate amount The above oil phase and aqueous phase were each heated and dissolved at 70 ° C.
The oil phase was gradually added to the aqueous phase while stirring, and emulsified by a homogenizer until the mixture became sufficiently uniform. Then 50
After cooling to 0 ° C. and adding a compounding agent and a fragrance, the mixture was uniformly mixed and further cooled to obtain a lotion.

A sensory test was conducted by 10 panelists on the cosmetics (facial cleansing cream, lotion) thus produced. In this test, a cleansing effect, a massage effect, a soft feeling, and a feeling of fit were selected as evaluation items, and each item was evaluated on a 5-point scale according to the following criteria. 1 ... bad 2 ... somewhat bad 3 ... normal 4 ... somewhat good 5 ... good The results of this sensory test are shown in Table 1. In addition, the numerical value in a table | surface is an average value of evaluation of 10 persons. The judgment was made according to the following criteria by summing up the average value of each item for each of the feel and the effect.・ ・ ・: Total of 8 or more △: Total of 5 to 7.9 ×: Total of 4.9 or less However, even if the total is 8 or more, the average value of one item is 3.0 to 3.5. If there is any item, it is marked as △, and even if the total is 8 or 5 or more, even if one item has an average value of 2.9 or less, it is marked as x.

[0068]

[Table 1]

From Table 1, it can be seen that the cosmetic containing the (meth) acrylic ester resin particles of the present invention has excellent softness and sittability, and also has excellent cleansing and massage effects, which is unprecedented. It was found that it had the characteristics described above.

[0070]

According to the present invention, (meth) acrylic acid obtained by adhering an inorganic powder having a specific average particle size to the surface of crosslinked (meth) acrylate resin particles having a specific compressive strength and an average particle size. Cosmetics containing ester-based resin particles (compounding agents) have both excellent feel (soft feeling, sit-down feeling) and excellent effects (cleansing, massage), and have characteristics not found in the past.

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4C083 AB032 AB172 AB212 AB242 AB501 AC012 AC022 AC072 AC122 AC182 AC242 AC442 AC482 AC542 AC642 AC782 AD091 AD092 AD512 BB23 BB25 CC01 CC04 CC05 CC23 DD31 EE06 EE10 EE12 EE50 4J002 DE10601 DJ016 FB086 FB096 FB166 GC00

Claims (3)

[Claims] 1. 100 parts by weight of crosslinked (meth) acrylate resin particles having an average particle size of 30 to 800 μm and a compressive strength of 0.01 to 0.6 kgf / mm ² , and 1/200000 of the resin particles. (Meth) acrylic acid ester comprising 0.01 to 30 parts by weight of an inorganic powder having an average particle diameter of from 1/200, wherein the inorganic powder adheres to the surface of the resin particles. Resin particles. 2. The (meth) acrylate resin particles according to claim 1, wherein the inorganic powder has been subjected to a hydrophobic treatment. 3. The method according to claim 1, wherein the (meth) acrylate-based resin particles according to claim 1 are contained in an amount of from 0.5 to 5%.
A cosmetic comprising 0% by weight.