JP6845724B2 - Underwater oil type emulsified cosmetic - Google Patents

Description

The present invention relates to an oil-in-water emulsified cosmetic containing a powder surface-coated with a specific surface coating treatment agent and hydrogenated phospholipids. More specifically, the present invention has high powder dispersibility and over time. It relates to an oil-in-water emulsified cosmetic that has excellent long-lasting makeup, uniform makeup film, and long-lasting makeup effect.

The oil-in-water emulsified cosmetic is a formulation used in makeup cosmetics such as foundations, foundations, and BB creams, and skin care cosmetics such as milky lotions, creams, and daytime beauty essences. , It is applied to various products because it exerts an appropriate emollient effect. In particular, in make-up cosmetics, it is a very important dosage form in order to realize a feeling of use such as freshness and lightness of spread when applied, and a feeling of moistness and dryness over time.

In recent years, not only make-up cosmetics but also skin care cosmetics may use powder for sensory adjustment, toning, UV protection function, etc., and various studies have been conducted on the use of powder. There is. In particular, in solid oil-in-water cosmetics, when powder is contained, powder agglomeration during heating and filling may become a problem, and it can be said that improving the dispersibility of the powder is an important issue.

Phospholipids are natural emulsifiers with a high moisturizing effect and are used as general-purpose emulsifiers in oil-in-water emulsified cosmetics. However, since phospholipids have a weak emulsifying power, the inclusion of powder or the like may cause a problem in stability. Therefore, studies have been conducted on powders that tend to aggregate in the emulsifier mold by subjecting them to surface treatment to suppress aggregation and improve dispersibility. For example, an oil in water with improved stability over time by combining silicon oil, water and anionic surfactant and / or phospholipid with fine particle powder surface-treated with an organosilicon compound having a weight of 10 to 30% by mass. There is a type cosmetic (see Patent Document 1).

However, oil-in-water emulsified cosmetics are easy to get used to sweat and sebum secreted from the skin, and the makeup film moves and floats easily, and the powder is localized in fine wrinkles and pores due to the movement of facial expressions (so-called twist).・ It is a problem that makeup breakage such as (pores fall off) is observed, and studies are being conducted to improve makeup retention when powder is contained. In particular, surface treatments of various powders have been developed in order to improve the longevity of makeup in oil-in-water emulsified cosmetics. For example, in order to improve the adhesion to the skin (adhesion, uniformity) and to improve the long-lasting makeup, a technique using composite particles formed by adhering a silicone elastomer using a silicone resin as a medium (see Patent Document 2) and amino acids. A technique using a powder treated with a modified organopolysiloxane (see Patent Document 3) and the like have been proposed. Further, as a cosmetic powder having excellent adhesion to the skin, a powder surface-treated with a silicone gel (see Patent Document 4) and the like have been proposed.

Japanese Unexamined Patent Publication No. 2003-286147 Japanese Unexamined Patent Publication No. 2011-1332. Japanese Unexamined Patent Publication No. 2012-102320 WO2014 / 102862

However, according to the technique of Patent Document 2, although the oil-in-water emulsified cosmetics can retain their makeup due to their adhesion to the skin and their uniformity, the described oil-in-water emulsified cosmetics are made of water-soluble polymers. It was emulsified or the interface was firmly solidified with higher alcohol to ensure emulsification stability, and it was very difficult to ensure stability when emulsified with phospholipids. Further, when the powder is surface-treated by the technique of Patent Document 3, the adhesion to the skin is also excellent, but the dispersion in the oil agent is good, so that the powder is contained in the composition emulsified with phospholipid. It can be difficult to ensure stability. Further, although the technique of Patent Document 4 has been studied for application to oil-in-water creams, sufficient studies have not been made on oil-in-water emulsified cosmetics emulsified with phospholipids. Therefore, there has been a demand for the development of oil-in-water emulsified cosmetics having high powder dispersibility, stable preparation even when phospholipids are used as emulsifiers, and excellent adhesion to the skin and long-lasting makeup effect. ..

In view of the above situation, as a result of diligent research, the present inventors have found that, among various surface coating powders, specific double-terminal reactive diorganopolysiloxane and specific ones when hydrogenated phospholipids are used as emulsifiers. By combining powders surface-coated with the amino group-containing silane compound of the above to form an oil-in-water emulsified cosmetic, the powder dispersibility is particularly high, and the powder is stretched without impairing the stability of the oil-in-water emulsified cosmetic. It was found that it is excellent in usability such as lightness and long-lasting effect of makeup over time. Further, by further containing a water-soluble thickener, the emulsion stability is more excellent even when a component such as an ultraviolet absorber (particularly an ultraviolet absorber solid at room temperature) that greatly affects the emulsion stability is contained. Among them, it has been found that an excellent effect can be obtained by containing agar or (PEG-240 / decyltetradeceth-20 / HDI) copolymer. Further, in the case of a solid oil-in-water emulsified cosmetic having a strong tendency to aggregate powder, particularly in the case of a solid-water oil-type emulsified cosmetic obtained by filling a container after heating and melting and cooling. , The present invention has been completed by finding that an effect particularly excellent in powder dispersibility, which is a problem in the present invention, can be obtained.

That is, the present invention describes the following components (A) and (B);
(A) Powder (a) surface-coated with the following surface coating treatment agents (a) and (b) Both-terminal reactive diorganopolysiloxane R ¹ R ² ₂ SiO-represented by the following general formula (1) (R ² ₂ SiO) _L- SiR ¹ R ² ₂ (1)
(In the formula, each R ¹ represents a hydroxyl group, each R ² independently represents a hydrocarbon group having 1 to 20 carbon atoms, and L represents an integer of 3 to 10,000) and.
(B) Amino group-containing silane compound represented by the following general formula (2)
R ³ R ⁴ _m SiX _(3-m) (2)
(In the formula, R ³ represents a hydrocarbon group having at least one amino group and having 1 to 20 carbon atoms, R ⁴ represents an alkyl group having 1 to 4 carbon atoms, and X represents an alkoxy group having 1 to 4 carbon atoms. Represents, m is 0 or 1)
(B) The present invention relates to an oil-in-water emulsified cosmetic containing hydrogenated phospholipids.

Further, the present invention relates to the above-mentioned oil-in-water emulsified cosmetic containing the component (C) water-soluble thickener.

Further, the present invention relates to the above-mentioned oil-in-water emulsified cosmetic in which the component (C) is agar or a (PEG-240 / decyltetradeceth-20 / HDI) copolymer.

The oil-in-water emulsified cosmetic according to the above, wherein the content mass ratio of the powder and the surface coating treatment agents (a) and (b) in the component (A) is 99.9: 0.1 to 90:10. It is about.

The present invention relates to the above-mentioned oil-in-water emulsified cosmetic having a mass ratio of the component (A) to the surface coating treatment agents (a) and (b) of 100: 0.1 to 100: 35.

The above-mentioned oil-in-water oil, which is a powder whose surface is coated with a polymer having a fine three-dimensional crosslinked structure of silicone, in which the component (A) is condensed with the surface coating treatment agents (a) and (b). It is related to type emulsified cosmetics.

Further, the present invention relates to the above-mentioned oil-in-water emulsified cosmetic in which the oil-in-water emulsified cosmetic is solid.

Further, the present invention relates to the above-mentioned oil-in-water emulsified cosmetic obtained by heating and melting, filling a container, and cooling.

The oil-in-water emulsified cosmetic of the present invention has high powder dispersibility, is stable even when a phospholipid is used as an emulsifier, and has excellent cosmetic film uniformity and makeup-sustaining effect.

Hereinafter, the present invention will be described in detail. The numerical range represented by using "~" in the present specification means a range including the numerical values before and after "~" as the lower limit value and the upper limit value. In addition, the numerical value expressed in% is a value based on mass unless otherwise specified.

The surface-coated powder of the component (A) used in the present invention is obtained by coating the powder with the following surface coating treatment agent (a) and the following surface coating treatment agent (b). Is.
(A) Double-ended reactive diorganopolysiloxane represented by the following general formula (1) R ¹ R ² ₂ ^{SiO- (R 2} ₂ SiO) _L- ^{SiR 1} R ² ₂ (1)
(In the formula, each R ¹ represents a hydroxyl group, each R ² independently represents a hydrocarbon group having 1 to 20 carbon atoms, and L represents an integer of 3 to 10,000).
(B) Amino group-containing silane compound represented by the following general formula (2)
R ³ R ⁴ _m SiX _(3-m) (2)
(In the formula, R ³ represents a hydrocarbon having at least one amino group and having 1 to 20 carbon atoms, R ⁴ represents an alkyl group having 1 to 4 carbon atoms, and X represents an alkoxy group having 1 to 4 carbon atoms. Represented, m is 0 or 1)

The surface coating treatment agent (a) used in the present invention is a bi-terminal reactive diorganopolysiloxane, and is a bi-terminal hydroxysilyl group-modified silicone represented by the following general formula (1).
R ¹ R ² ₂ SiO- (R ² ₂ SiO) _L- ^{SiR 1} R ² ₂ (1)
(In the formula, each R ¹ represents a hydroxyl group, each R ² independently represents a hydrocarbon group having 1 to 20 carbon atoms, and L represents an integer of 3 to 10,000).

The form of the above (a) is not particularly limited, but in the present invention, it is preferable to use it in the form of a water suspension or a water emulsion from the viewpoint of improving the feel of the component (A). As the method for preparing the water emulsion of (a), a generally known method may be used, and a method of emulsion polymerization using a low molecular weight cyclic siloxane as a starting material or a method of emulsifying an oily double-ended reactive diorganopolysiloxane. Etc. are exemplified.

The surface coating treatment agent (b) used in the present invention is an amino group-containing silane compound and is represented by the following general formula (2).
R ³ R ⁴ _m SiX _(3-m) (2)
(In the formula, R ³ represents a hydrocarbon group having at least one amino group and having 1 to 20 carbon atoms, R ⁴ represents an alkyl group having 1 to 4 carbon atoms, and X represents an alkoxy group having 1 to 4 carbon atoms. Represents, m is 0 or 1)

Preferred examples of the above (b) are not particularly limited, and examples thereof include N- (2-aminoethyl) -3-aminopropyltriethoxysilane, 3-aminopropyltriethoxysilane, and 3-aminopropyltrimethoxysilane. it can.

Further, as a preferable mode of the component (A) used in the present invention, a polymerization having a fine three-dimensional crosslinked structure of silicone in which the above-mentioned surface coating treatment agents (a) and (b) are condensed and reacted. A powder whose surface is coated with a substance (hereinafter referred to as "silicone microcrosslinked product"). The silicone microcrosslinked product may be a compound having no rubber elasticity, and the mass ratio of (a) and (b) is approximately surface coating treatment agent (a): surface coating treatment agent (b) = 100. : 0.1 to 100: 35 is preferable.

Further, the silicone microcrosslinked product is preferably a polymer having rubber elasticity, that is, rubber hardness. A polymer having no rubber hardness is one in which the measured value of the durometer type AO measurement method (soft rubber hardness measurement) defined in ISO7619-1 is less than 10, more preferably less than 5, and even more preferably 0. Is.

Further, the rheological properties of the silicone microcrosslinked product are not particularly limited, but the complex elastic modulus in dynamic viscoelasticity measurement (25 ° C., strain rate 17%, shear frequency 4 Hz) is 3,000 to 100,000 Pa, and the loss coefficient. The tan δ (loss elastic modulus G ”/ storage elastic modulus G ′) is preferably 1.0 to 2.5, more preferably the complex elastic modulus is 10,000 to 100,000 Pa, and the loss coefficient tan δ is. The range is 1.0 to 2.0, which is more preferable because it is more excellent in usability, adhesion to the skin, and uniformity of the cosmetic film.

The rheological properties of the silicone microcrosslinked product can be measured as follows.
Dynamic viscoelasticity measuring device: Rheosol-G3000 (manufactured by UBM)
Measuring jig: Parallel plate with a diameter of 20 mm Measuring frequency: 4 Hz
Measurement temperature: 25 ± 1.0 ° C
Measurement distortion setting: Set the distortion rate to 17% and perform measurement in the automatic measurement mode.
Measurement sample thickness (gap): 1.0 mm
Here, the shear frequency is set to 4 Hz because it is in the range of the physical operating speed that is common for humans and is close to the speed when the cosmetic is applied to the skin.

In the component (A) used in the present invention, the powder that can be surface-coated is not particularly limited as long as it is a powder used in ordinary cosmetics, and is an inorganic powder, an organic powder, or a metal soap powder. , Glittering powder, dye powder, composite powder, etc., and their particle shape (spherical, needle-like, plate-like, amorphous, etc.), particle size (foam-like, fine particles, pigment grade, etc.), particle structure Any of them can be used regardless of (porous, non-porous, etc.).

Specific examples of the inorganic powder include titanium oxide, zirconium oxide, zinc oxide, cerium oxide, magnesium oxide, barium sulfate, calcium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate, talc, mica, kaolin, sericite, and white cloud. Mother, synthetic mica, gold mica, red mica, black mica, lithia mica, silicic acid, silicic acid anhydride, aluminum silicate, magnesium silicate, aluminum magnesium silicate, calcium silicate, barium silicate, strontium silicate, tungsten Acid metal salts, hydroxyapatite, vermiculite, hygilite, bentonite, montmorillonite, hectrite, zeolite, ceramic powder, dicalcium phosphate, alumina, aluminum hydroxide, boron nitride, silica, etc. may be mentioned. Two or more types can be used in combination.

Organic powders include polyamide powder, polyester powder, polyethylene powder, polypropylene powder, polystyrene powder, polyurethane powder, benzoguanamine powder, polymethylbenzoguanamine powder, tetrafluoroethylene powder, polymethylmethacrylate powder, cellulose powder, silk powder, nylon powder. (12 nylon, 6 nylon), styrene / acrylic acid copolymer powder, divinylbenzene / styrene copolymer powder, vinyl resin powder, urea resin powder, phenol resin powder, fluororesin powder, silicon resin powder, acrylic resin powder, Examples thereof include melamine resin powder, epoxy resin powder, polycarbonate resin powder, microcrystalline fiber powder, rice starch, lauroyl lysine and the like, and one or a combination of two or more can be used as required.

Among these, but not particularly limited, barium sulfate, calcium carbonate, talc, mica, sericite, white mica, synthetic mica, gold mica, titanium oxide, zinc oxide, iron oxide, iron hydroxide, dark blue, ultramarine blue, polystyrene powder. , Polyurethane powder, Polymethylmethacrylate powder, Cellulose powder, Silk powder, Nylon powder (12 nylon, 6 nylon), Styrene / acrylic acid copolymer powder, Silicone powder, Polyethylene terephthalate powder, Titanium oxide coated mica, Titanium oxide / Oxidation It is particularly preferable to select tin-coated synthetic mica, titanium oxide-coated glass powder, or the like because a surface-coated powder having a higher cosmetic effect can be obtained. The average particle size of these powders is not particularly limited, but those of about 3 to 200 μm are preferable from the viewpoint of cosmetic effect. The average powder particle size can be measured by the particle size distribution measuring device LA-960 (HORIBA, Ltd.).

In the component (A) used in the present invention, the method of surface-coating these powders with the above-mentioned surface coating treatment agents (a) and (b) is not particularly limited, but for example, a surface coating treatment agent. A dry coating method in which and powder are directly mixed (heated) and coated, a surface coating treatment agent is dissolved or dispersed in a solvent such as ethanol, isopropyl alcohol, or n-hexane, and the powder is added to this solution or dispersion. Examples thereof include a wet coating method in which the solvent is added, mixed, and then the solvent is removed by drying or the like, heated, and pulverized, a mechanochemical method, and the like.

In addition, the component (A) can be obtained based on the method described in International Publication No. 2014/102863. For example, it is also possible to simply mix the powder and the above-mentioned silicone microcrosslinked product with a mixer or the like and coat them. Further, more preferably, a method of fixing the silicone microcrosslinked product to the particle surface by precipitating the silicone microcrosslinked product on the surface of the powder particles in the presence of the powder by the in-situ method and then heating the material. Can be used. By this method, the uniformity of coating on the surface of the powder particles is enhanced, and it is possible to obtain a powder having better dispersibility and excellent adhesion to the skin.

The component (A) thus obtained has a powder surface coated with the surface coating treatment agents (a) and (b), and the coating amount thereof is not particularly limited, but the powder and the powder. The content mass ratio with the surface coating treatment agent is preferably (powder that can be surface coated) :( surface coating treatment agents (a) and (b)) = 99.99: 0.01 to 70:30, 99. 9: 0.1 to 90:10 is particularly preferable. Within this range, the powder has good dispersibility, and a smoother, lighter feel and a moist feeling can be obtained, and a surface coating powder having excellent uniformity of the cosmetic film and long-lasting makeup can be obtained.

The content of the component (A) in the present invention is not particularly limited, but is preferably 1 to 20%, more preferably 3 to 15%, based on the total amount of the cosmetic. Within this range, the oil-in-water emulsified cosmetic of the present invention is preferable because it has good stability and is excellent in smooth spread and spread, uniformity, and long-lasting makeup.

By using the hydrogenated phospholipid of the component (B) used in the present invention as an emulsifier, the effect of excellent freshness at the time of application, lightness of spread, uniformity of the cosmetic film, and long-lasting makeup over time. Play. The component (B) hydrogenated phospholipid used in the present invention includes hydrogenated substances such as phosphatidylcholine, phosphatidylethanolamine, phosphatidylserine, phosphatidylglycerol, phosphatidylinositol, and sphingolinlipid, and similar substances thereof or similar substances thereof. Examples of the composition contained include hydrogenated soybean lecithin, egg yolk lecithin, and corn lecithin. Of these phospholipids, hydrogenated soybean lecithin is preferable. Commercially available products include Resinol S-10, Resinol S-10E (all manufactured by Nikko Chemicals), HSL-70 (manufactured by YMC), Basis LS-60HR (manufactured by Nisshin Oillio Group), and Egg Yolk Lecithin PL-100P. (Made by Kewpie Corp.) and the like. Cholesterol and / or phytosterol can also be used as a premixed phospholipid, and commercially available products such as PRESOME C-2 (manufactured by Nippon Fine Chemical Co., Ltd.) and PHYTOCOMPO-PP (Nippon Fine Chemical Co., Ltd.) can be used. Made) and the like.

The content of the hydrogenated phospholipid of the component (B) in the present invention is not particularly limited, but is preferably 0.3 to 3.0%, more preferably 0.1 to 2.0%, based on the total amount of the cosmetic. This range is preferable because it is superior in the uniformity of the makeup film and the longevity of the makeup over time.

Further, the present invention further enhances the moist feeling over time, the lack of dryness, the makeup lasting effect, and the stabilizing effect of the oil-in-water emulsified cosmetic by containing the water-soluble thickener as the component (C). Play. The component (C) water-soluble thickener used in the present invention is one that forms a thickening or aqueous gel when dispersed or dissolved in water. When forming the gel, heating and cooling may be performed or neutralization may be performed, if necessary. Further, when it is dispersed or dissolved in water, it may be dispersed or dissolved using an aqueous solvent that dissolves in water such as ethanol. Examples of the water-soluble thickener include water-soluble natural polymers, water-soluble synthetic polymers, clay minerals, and silicic anhydride.

The water-soluble thickener of the component (C) used in the present invention is not particularly limited as long as it is usually used for cosmetics, and for example, a carboxyvinyl polymer, an alkyl-modified carboxyvinyl polymer, a hydroxypropylmethyl cellulose, and a hydroxy. Synthetic / semi-synthetic systems such as ethyl cellulose, carboxymethyl cellulose, (acryloyldimethyltaurine ammonium / VP) copolymer, sodium polyacrylate, polystyrene sulfonate, etc., cellulose gum, gellan gum, pectin, carrageenan, xanthan gum, sclerothium gum, karaya gum, agar, etc. Natural polysaccharides, (acryloyldimethyltaurine ammonium / carboxyethyl acrylate) crosspolymers, acrylates / alkyl acrylates (C10-30) crosspolymers, (PEG-240 / decyltetradeceth-20 / HDI) copolymers, etc. Examples thereof include a water-soluble thickener having a hydrophobic group. These water-soluble thickeners may be used alone or in combination of two or more. Among these water-soluble thickeners, agar (PEG-240 / decyltetradeceth-20 / HDI) copolymer is particularly preferable because it improves the stabilizing effect of the oil-in-water emulsified cosmetic. As specific commercial products, for example, commercial products such as Ina Agar UP-37 (manufactured by Ina Food Industry Co., Ltd.) and ADEKA NOL GT-700 (manufactured by ADEKA) can also be used.

The content of the component (C) water-soluble thickener in the present invention is not particularly limited, but is preferably 0.05 to 3%, more preferably 0.1 to 2%, based on the total amount of the cosmetic. Within this range, the oil-in-water emulsified cosmetic of the present invention is preferable because it has good stability and is superior in moist feeling, smooth spreading and spreading, adhesion feeling, and long-lasting makeup.

In the present invention, a solid UV absorber can be further contained at 25 ° C. The solid UV absorber used in the present invention is usually a component used to obtain a UV protection effect, but the inclusion of the solid UV absorber in an oil-in-water emulsified cosmetic reduces stability. It may become sticky or sticky. In particular, it may precipitate over time, causing problems such as a decrease in the ultraviolet protection effect, which poses a major problem in cosmetics that require an ultraviolet protection effect. However, by combining the ingredients of the present invention, it is possible to solve such a problem and obtain an oil-in-water emulsified cosmetic having an ultraviolet protection effect without impairing stability, which is preferable. The ultraviolet absorber solid at 25 ° C. used in the present invention is not particularly limited as long as it is usually used for cosmetics, but specifically, 2- (4-diethylamino-2-hydroxybenzoyl) benzoic acid. Acid hexyl ester, 2,4-bis {[4- (2-ethylhexyloxy) -2-hydroxy] phenyl} -6- (4-methoxyphenyl) -1,3,5-triazine), 4-tert- Examples thereof include butyl-4'-methoxy-dibenzoylmethane, 2,4,6-tris [4- (2-ethylhexyloxycarbonyl) anilino] -1,3,5-triazine, and if necessary, one type or Two or more types can be used in combination.

The content of the solid ultraviolet absorber in the oil-in-water emulsified cosmetic of the present invention is not particularly limited, but is preferably 0.1 to 3%, preferably 0.3 to 1.5%, based on the total amount of the cosmetic. Is more preferable. Within this range, it is preferable because it has an appropriate ultraviolet protection function and is excellent in stability of the oil-in-water emulsified cosmetic.

The oil-in-water emulsified cosmetic of the present invention may be liquid, milky, gelled, solid or the like, and may have any property. Among them, if the oil-in-water emulsified cosmetic is solid, it needs to be dispersed and maintained in a highly fluid state without being dissolved at a high temperature when filling the bulk, so powder dispersibility is a problem. However, by combining the components of the present invention, the problem of aggregation can be solved. Therefore, among various properties, solids are preferable because they are excellent in powder dispersibility and have an excellent effect in stability of oil-in-water emulsified cosmetics.

The method of solidifying is not particularly limited, but a method of heating before emulsification, emulsifying while dispersing including powder, and cooling while dispersing to thicken and solidify, or an emulsion is prepared in advance. A method of mixing and adding with a heated water-soluble thickening gelling agent and solidifying by cooling, a method in which an emulsion and a thickening gelling agent are prepared in advance are mixed, and after heating and melting, a container is used. Examples thereof include a method of filling and cooling the mixture. Among them, after heating and melting the oil-in-water emulsified cosmetic, powder aggregation and disintegration of emulsified droplets are likely to occur in the process of filling the container. Therefore, in particular, the container is filled and cooled after being heated and melted. In the oil-in-water emulsified cosmetics obtained as described above, the powder dispersibility and stabilizing effect can be more exhibited, which is preferable.

In the present invention, in addition to the above components (A) to (C), a solid ultraviolet absorber that exhibits the effect of the present invention more prominently can be contained, and as a component usually contained in cosmetics, an oily component, Surfactants other than component (B), water-soluble polymers other than component (C), moisturizing components, UV absorbers other than solids, antioxidants, metal chelating agents, preservatives, powders other than component (A) , Dyes, fragrances, various chemicals and the like can be arbitrarily contained as long as the effects of the present invention are not impaired.

The method for producing the oil-in-water emulsified cosmetic of the present invention is not particularly limited, but the component (A) is, if necessary, dispersed in an aqueous component containing the component (C) and then heated. B) and, if necessary, a method of adding and dispersing an oily component obtained by heating and dissolving a solid ultraviolet absorber, emulsifying and then cooling to obtain an oil-in-water emulsified cosmetic, component (B), and if necessary. If necessary, an oily component containing a solid ultraviolet absorber is added to an aqueous component containing the component (C) after being dispersed and then emulsified, and then cooled to obtain an emulsion. After that, a method of obtaining an oil-in-water emulsified cosmetic by adding and then dispersing the component (A) can be mentioned. The filling method is not particularly limited, and examples thereof include a method in which a solid oil-in-water emulsified cosmetic is obtained by heating and melting, filling the container, and then cooling and solidifying. The filling container is a dish-shaped container. , Compact container, stick-shaped container, etc., the container can be selected according to the desired shape.

The dosage form of the oil-in-water emulsified cosmetic of the present invention is not particularly limited as long as it is an oil-in-water type, and may be a water-in-water type, liposomes, vesicles, or the like.

The oil-in-water emulsified cosmetic of the present invention is not particularly limited, but is not limited to makeup cosmetics such as foundation, foundation, BB cream, eye shadow, eyebrow, and concealer, and skin care cosmetics such as milky lotion, cream, and daytime beauty essence. Suitable for use. The cosmetics in which the effects of the present invention are remarkably exhibited are makeup cosmetics such as foundations, foundations and BB creams containing powder and solid ultraviolet absorbers, and skin care cosmetics such as daytime beauty essences.

Examples are shown below, but the present invention is not limited to these examples.

<Manufacturing method of component (A)>
1. 1. Preparation of Silicone Microcrosslinked Sample In a polyethylene beaker with a capacity of 2 liters, 450 g of octamethylcyclotetrasiloxane, 500 g of ion-exchanged water, and 6.75 g of sodium lauroylmethyltaurine were charged, premixed by stirring with a homomixer at 2000 rpm, and then 4 g of citric acid was added. The mixture was added, heated to 70 ° C., and emulsion-polymerized by a homomixer at 5000 rpm for 24 hours. A high molecular weight water emulsion (a) was obtained by emulsifying and dispersing once at 50 MPa with a tabletop pressure homogenizer (manufactured by APV Gorin). Then, 10% sodium carbonate was added to adjust the pH to 7, and the water emulsion of (a) was obtained. The molecular weight of the solid content obtained by volatilizing and removing water by drying this water emulsion at 105 ° C. for 3 hours was found to be 10000 when the molecular weight in terms of PS was determined by GPC. The solid content was 46.5%.

In a PP 300 ml container, 88.5 g of ion-exchanged water was added to 21.5 g of the above emulsion, and the mixture was stirred at room temperature at 6000 rpm for 10 minutes using a homomixer. While stirring this with a stirrer, 4 g of a 25 wt% IPA solution of (b) aminopropyltriethoxysilane (KBE-903: manufactured by Shin-Etsu Chemical Co., Ltd.) is added. Then, the pH was adjusted to 10.5 with a 1N-NaOH aqueous solution, and the mixture was stirred for 15 minutes, transferred to an aluminum dish, and dried at 105 ° C. for 24 hours to obtain a silicone microcrosslinked product. The obtained silicone microcrosslinked product was measured by a durometer AO with NA (below the measurement limit), a complex elastic modulus of 17500 Pa, and a tan δ of 1.353.

(Measurement by Durometer AO)
In a styrene square case (vertical 36 x horizontal 36 x height 14 mm), a silicone microcrosslinked product is placed so as to slightly protrude from the surface, and the surface is flattened to be a test surface. The pressure plate of the durometer is placed at a position of 20 mm on the test surface, and while the pressure plate is kept parallel to the surface of the test surface, the pressure plate is pressed against the test piece and the scale of the needle is read. This operation was performed 5 times and the average value was taken as the measured value. If the needle did not move due to the measurement, it was set to NA (Not Applicable).

粘弾性測定装置：Ｒｈｅｏｓｏｌ−Ｇ３０００（ＵＢＭ社製）
測定治具：直径２０ｍｍのパラレルプレート
測定周波数：４Ｈｚ
測定温度：２５±１．０℃
測定歪の設定：歪み率１７％に設定し、自動測定モードにて測定を行う。
測定試料厚み（ギャップ）：１．０ｍｍ (Dynamic viscoelasticity measurement)
G'(storage elastic modulus) and G'(loss elastic modulus) were determined under the conditions shown below, and the complex elastic modulus and tan δ were determined.

Viscoelasticity measuring device: Rheosol-G3000 (manufactured by UBM)
Measuring jig: Parallel plate with a diameter of 20 mm Measuring frequency: 4 Hz
Measurement temperature: 25 ± 1.0 ° C
Measurement distortion setting: Set the distortion rate to 17% and perform measurement in the automatic measurement mode.
Measurement sample thickness (gap): 1.0 mm

2. Production of surface-coated powder (A) Production Example 1: (Surface coating agent (a) / Surface coating agent (b) = 100/10) 5% Surface-coated mica In a PE container with a capacity of 20 liters, 7 L of water and 1 kg of Y-2300 (manufactured by Yamaguchi Mica) were charged and dispersed at 2000 rpm for 5 minutes with a disper mixer (Prime Mix Co., Ltd .; AM-40). 103 g of the above water emulsion was added and stirred at 2500 rpm for 5 minutes. Next, 96 g of a 5% by mass aqueous solution of aminopropyltriethoxysilane (KBE-903; manufactured by Shin-Etsu Chemical Co., Ltd.) was added as a cross-linking agent. After adjusting the pH to 10.3 with a 1N-NaOH aqueous solution, the mixture was stirred and reacted at 3000 rpm for 30 minutes. After filtering with a centrifugal dehydrator and washing with 7 L of water, the dehydrated cake was dried in a dryer at 120 ° C. for 16 hours. At this time, when a temperature sensor was inserted into the cake and the temperature was recorded, it was heated at 115 ° C. or higher for 7 hours. The dried cake was ground with a parvelizer to give 5% surface coated mica.

Production Example 2: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/10) Preparation of 0.1% surface coating mica water emulsion of Production Example 1 and 5% by mass aqueous solution of aminopropyltriethoxysilane 0.1% surface-coated mica was obtained according to Production Example 1 except that the amounts were changed to 2.0 g and 1.8 g, respectively.

Production Example 3: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/10) 10% surface coating mica Amount of the water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane Was replaced with 196 g and 182 g, respectively, to obtain 10% surface-coated mica according to Production Example 1.

Production Example 4: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/10) 0.05% surface-coated mica A water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane. A 0.05% surface-coated mica was obtained according to Production Example 1 except that the charged amounts were changed to 1.0 g and 0.9 g, respectively.

Production Example 5: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/1) 5% surface coating mica Amount of the water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane Was replaced with 108 g and 9.6 g, respectively, to obtain 5% surface-coated mica according to Production Example 1.

Production Example 6: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/35) 5% surface coating mica Amount of the water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane A 5% surface-coated mica was obtained according to Production Example 1 except that the amounts were changed to 80 g and 259 g, respectively.

Production Example 7: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/0.05) 5% surface-coated mica The water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane. A 5% surface-coated mica was obtained according to Production Example 1 except that the charged amounts were changed to 107 g and 0.5 g, respectively.

Production Example 8: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/50) 5% surface coating mica Amount of the water emulsion of Production Example 1 and a 5% by mass aqueous solution of aminopropyltriethoxysilane A 5% surface-coated mica was obtained according to Production Example 1 except that the amounts were changed to 72 g and 333 g, respectively.

Production Example 9: (Surface coating treatment agent (a) / Surface coating treatment agent (b) = 100/10) 5% surface coating talc The powder of Production Example 1 was replaced with talc JA-13R (manufactured by Asada Flour Milling Co., Ltd.). Except for the above, 5% surface-coated talc was obtained according to Production Example 1.

Examples 1 to 17 and Comparative Examples 1 to 4 Bases Bases having the compositions shown in Tables 1 to 3 were prepared according to the following production methods. Regarding the obtained substrate, a: powder dispersion stability, b: emulsification stability, c: smooth spreading and spreading, d: makeup film uniformity, e: makeup retention (for sweat and sebum) Durability) was evaluated. The results are also shown in Tables 1 to 3.

Note 1: Adecanol GT-700 (manufactured by ADEKA)
Note 2: Sepigel 305 (manufactured by SEPPIC)

(Manufacturing method): Examples 1 to 17, Comparative Examples 1 to 4
A. The components (14) to (29) are uniformly dispersed with a roll mill.
B. Ingredients (1) to (7) are heated to 75 ° C. and uniformly mixed.
C. The components (8) to (13) are heated to 75 ° C. and uniformly mixed.
D. Add A to B and mix.
E. D is added to C, mixed, and emulsified at 75 ° C.
F. E was cooled to room temperature to obtain a substrate.

<Evaluation method (a: Powder dispersion stability)>
Each sample is placed in a transparent glass container, sealed, and stored in a constant temperature bath at 50 ° C. for 1 month. Then, visually observe the aggregation level of the powder and judge using the following 4-step judgment criteria. did.
<Criteria>
(Evaluation result): (Judgment)
No unevenness of powder: ◎
There is slight unevenness in the powder, but there is no problem. Level: ○
Uneven powder is seen: △
Severe powder unevenness is seen: ×

<Evaluation method (b: emulsification stability)>
Each sample was placed in a transparent glass container and sealed, and after storing in a constant temperature bath at 50 ° C. for 1 month, the presence or absence of waste liquid was confirmed in the bulk, and a part thereof was taken out and expanded, and the texture was visually confirmed.
<Criteria>
(Evaluation result): (Judgment)
No change compared to the initial stage: ◎
The texture deteriorates slightly, but there is no significant change from the initial stage: ○
The texture is getting worse and a slight drainage is seen: △
Drainage is seen: ×

<Evaluation method (C: Smooth spread and spread, D: Uniformity of makeup film, E: Makeup retention (durability to sweat and sebum))>
We asked 20 cosmetics evaluation panel to use the bases of the above-mentioned Examples and Comparative Examples, and "C: Smooth spread and spread" at the time of application, "D: Uniformity of makeup film" as a finish effect of makeup, Regarding "e: makeup retention" for sweat and sebum over time, each person evaluates on a 5-point scale according to the following criteria, gives a score for each base, and calculates the average score of the scores of all panels, and the following criteria Judgment was made according to. Regarding "e: makeup retention" against sweat and sebum over time, the state 6 hours after the base application (daily life) was evaluated.
<Evaluation criteria>
(Evaluation result): (Score)
Very good: 5 points Good: 4 points Normal: 3 points Slightly defective: 2 points Bad: 1 point <Judgment criteria>
(Average score): (Judgment)
4.5 or higher: ◎
3.5 or more and less than 4.5: ○
1.5 or more and less than 3.5: △
Less than 1.5: ×

(result)
As is clear from the results in Tables 1 to 3, the substrates of Examples 1 to 17, which are the products of the present invention, have powder dispersion stability, emulsion stability, smooth spreading and spreading, and cosmetic film uniformity. It was an excellent base for all items of makeup retention (durability against sweat and sebum). On the other hand, Comparative Examples 1 and 2 containing other emulsifiers instead of the hydrogenated phospholipid of the component (B) did not give satisfactory results in smooth spread and spread, uniformity of makeup film, and longevity of makeup. In Comparative Example 3 in which a powder subjected to another surface treatment was used instead of the component (A), and Comparative Example 4 in which a powder not subjected to the surface treatment was used, the dispersion of the powder was not good, and the skin was treated. As a result, the adhesion of the makeup film was not uniform, resulting in lack of uniformity of the makeup film and longevity of the makeup.

Example 18 Foundation A foundation was produced by the following formulation and production method.
(Prescription) (%)
(1) Lecithin-treated titanium oxide 8.0
(2) Bengala 0.2
(3) Yellow iron oxide 0.8
(4) Black iron oxide 0.1
(5) 5% surface-coated talc of Production Example 9 2.0
(6) 1,3-butylene glycol 4.0
(7) Sorbitan sesquioleate 0.2
(8) Triceteares-4 phosphate 0.4
(9) Glyceryl tri2-ethylhexanoate 0.6
(10) Ethylhexyl methoxycinnamate 3.0
(11) 2- (4-Diethylamino-2-hydroxybenzoyl)
Benzoic acid hexyl ester 0.3
(12) Hydrogenated phospholipid 2.5
(13) Setostearyl alcohol 1.5
(14) Methyl paraoxybenzoate 0.1
(15) Agar 2.0
(16) Carrageenan 0.02
(17) 1,3-butylene glycol 10.0
(18) Glycosyl trehalose 0.05
(19) Residual amount of purified water

(Production method)
A. Ingredients (14) to (19) are uniformly mixed and dissolved at 90 ° C.
B. The components (1) to (8) are uniformly dispersed in a roll mill and added to A with stirring.
C. Ingredients (9) to (13) are uniformly mixed and dissolved at 75 ° C.
D. C is added to B with a homodisper (type 2.5; manufactured by PRIMIX) while stirring, and emulsified at 75 ° C.
E. Cool D to room temperature with stirring to defoam.
F. After heating and dissolving E at 75 ° C., it was filled in a tube container with a coating body and cooled to room temperature to obtain a foundation.

The foundation obtained as described above has good powder dispersion stability, excellent emulsion stability, excellent spread smoothness at the time of application, excellent finish uniformity, and extremely good makeup retention over time. It was something like that.

Example 19 Daytime beauty essence A daytime beauty essence was produced by the following formulation and manufacturing method.
(Prescription) (%)
(1) 5% surface-coated mica of Production Example 6 0.5
(2) (PEG-240 / decyltetradeceth-20)
/ HDI) Copolymer (Note 1) 0.5
(3) Alkyl-modified carboxyvinyl polymer 0.4
(4) 1,3-butylene glycol 5.0
(5) Residual amount of purified water (6) Potassium hydroxide 0.05
(7) Hydrogenated phospholipid 0.5
(8) PEG-30 phytosterol 0.1
(9) 4-tert-Butyl-4'-methoxy-dibenzoylmethane 0.2
(10) Ethylhexyl methoxycinnamate 5.0
(11) Polysilicone-15 1.0
(12) Methylphenylpolysiloxane 1.0
(13) Propylene Glycol Dicaprate 2.0
(14) Setostearyl alcohol 1.0
(15) Glyceryl monostearate 0.4
(16) Ethanol 2.0
(17) Methyl paraoxybenzoate 0.2

(Production method)
A. Ingredients (1) to (6) are uniformly mixed and dissolved at 75 ° C.
B. Ingredients (7) to (15) are uniformly mixed and dissolved at 75 ° C.
C. B is added to A with a homodisper (2.5 type; manufactured by PRIMIX) while stirring, and emulsified at 75 ° C.
D. After cooling C to room temperature with stirring, components (16) to (17) are added and mixed uniformly.
E. D was defoamed to obtain a daytime beauty essence.

The obtained daytime beauty essence has good powder dispersion stability and emulsion stability, has smooth spread and spread during application, and has excellent finish uniformity and long-term makeup retention. It was a medium-sized beauty essence.

Example 20 Day cream A day cream was produced by the following formulation and production method.
(Prescription) (%)
(1) Agar 0.5
(2) (PEG-240 / decyltetradeceth-20)
/ HDI) Copolymer (Note 1) 1.0
(3) 1,3-butylene glycol 5.0
(4) Glycerin 2.0
(5) Residual amount of purified water (6) Hydrogenated phospholipid 1.5
(7) Behenyl alcohol 1.5
(8) Ethylhexyl methoxycinnamate 5.0
(9) 2- (4-Diethylamino-2-hydroxybenzoyl)
Benzoic acid hexyl ester 1.0
(10) Squalan 2.0
(11) Di2-ethylhexyl succinate 1.0
(12) Dimethylpolysiloxane (Note 3) 0.2
(13) Ethanol 5.0
(14) Methyl paraoxybenzoate 0.2
(15) Boron nitride (average particle size 6.5 μm) 0.5
(16) 10% surface-coated mica of Production Example 3 3.0
(17) Nylon powder (spherical, average particle size 10 μm) 0.5
(18) Purified water 3.0
Note 3: KF-96-10CS (manufactured by Shin-Etsu Chemical Co., Ltd.)

(Production method)
A. Ingredients (1) to (5) are uniformly mixed and dissolved at 75 ° C.
B. Ingredients (6) to (12) are uniformly mixed and dissolved at 75 ° C.
C. B is added to A with a homodisper (type 2.5; manufactured by PRIMIX) with stirring, and emulsified at 75 ° C.
D. After cooling C to room temperature while stirring, the components (13) to (18) dispersed in advance are added and uniformly mixed.
E. D was defoamed to obtain a day cream.

The obtained day cream is a day cream that has good powder dispersion stability and emulsification stability, has smooth spread and spread during application, and has excellent finish uniformity and long-term makeup retention. It was.

Example 21 Oil-in-water solid teak A solid oil-in-water cheek was produced by the following formulation and production method.
(Prescription) (%)
(1) Red No. 226 0.1
(2) Bengala 0.3
(3) Yellow No. 4 Aluminum Rake 0.02
(4) 2% perfluorooctyltriethoxysilane treatment Mica titanium 1.5
(5) 5% surface-coated talc of Production Example 9 2.0
(6) 1,3-butylene glycol 4.0
(7) Sorbitan sesquiisostearate 0.2
(8) Triceteares-4 phosphate 0.4
(9) Glyceryl tri2-ethylhexanoate 1.8
(10) Ethylhexyl methoxycinnamate 2.0
(11) 2- (4-Diethylamino-2-hydroxybenzoyl)
Benzoic acid hexyl ester 0.2
(12) Sucrose polystearate 2.5
(13) Hydrogenated phospholipid 0.5
(14) Setostearyl alcohol 1.5
(15) Purified water 20.0
(16) Methyl paraoxybenzoate 0.1
(17) Agar 2.0
(18) Locust bean gum 0.05
(19) 1,3-butylene glycol 10.0
(20) Orange flower water 5.0
(21) Residual amount of purified water

(Production method)
A. Ingredients (9) to (14) are uniformly mixed and dissolved at 75 ° C.
B. The component (15) heated to 75 ° C. is added with stirring with a homodisper (2.5 type; manufactured by PRIMIX Corporation), and emulsified at 75 ° C.
C. B is cooled to room temperature with stirring and defoamed.
D. The components (16) to (21) are heated to 90 ° C. and uniformly mixed and dissolved.
E. The components (1) to (8) are uniformly dispersed in a roll mill and added to D cooled to 70 ° C. with stirring.
F. E is cooled to 40 ° C. with stirring with a homodisper (2.5 type; manufactured by PRIMIX), and then C is added.
G. Cool F to room temperature with stirring to defoam.
H. After warming and dissolving G at 75 ° C., it was filled in a resin dish of an airtight container and cooled to room temperature to obtain a solid oil-in-water teak.

The solid oil-in-water blush obtained as described above has good powder dispersion stability, excellent emulsion stability, smooth spread during application, excellent finish uniformity, and makeup over time. It had a very good hold.

Example 22 Oil-in-water stick-shaped eye color An oil-in-water stick-shaped eye color was produced by the following formulation and manufacturing method.
(Prescription) (%)
(1) Red No. 226 0.1
(2) Bengala 0.3
(3) Yellow No. 4 Aluminum Rake 0.05
(4) 2% Dimethicone-treated Bengala-coated mica titanium 1.5
(5) 5% surface-coated mica of Production Example 8 2.0
(6) 1,3-butylene glycol 4.0
(7) Sorbitan isostearate 0.2
(8) Triceteares-4 phosphate 0.4
(9) Mineral oil 1.8
(10) Hydrogenated polyisobutene 2.0
(11) Celesin wax (melting point: 73 ° C) 0.2
(12) Sodium behenate 2.5
(13) Hydrogenated phospholipid 0.5
(14) Setostearyl alcohol 1.5
(15) Purified water 20.0
(16) Methyl paraoxybenzoate 0.1
(17) Agar 5.0
(18) Locust bean gum 0.1
(19) 1,3-butylene glycol 10.0
(20) Lavender water 2.0
(21) Residual amount of purified water

(Production method)
A. Ingredients (9) to (14) are uniformly mixed and dissolved at 75 ° C.
B. The component (15) heated to 75 ° C. is added with stirring with a homodisper (2.5 type; manufactured by PRIMIX Corporation), and emulsified at 75 ° C.
C. B is cooled to room temperature with stirring and defoamed.
D. The components (16) to (21) are heated to 90 ° C. and uniformly mixed and dissolved.
E. The components (1) to (8) are uniformly dispersed in a roll mill and added to D cooled to 70 ° C. with stirring.
F. E is cooled to 40 ° C. with stirring with a homodisper (2.5 type; manufactured by PRIMIX), and then C is added.
G. Cool F to room temperature with stirring to defoam.
H. G was heated and dissolved at 75 ° C., filled in an airtight stick container, and cooled to room temperature to obtain an oil-in-water stick-shaped eye color.

The oil-in-water stick-shaped eye color obtained as described above has good powder dispersion stability, excellent emulsion stability, smooth spread during application, excellent finish uniformity, and over time. The makeup lasting was also extremely good.

Claims (10)

The following components (A) and (B);
(A) Powder (a) surface-coated with the following surface coating treatment agents (a) and (b) Both-terminal reactive diorganopolysiloxane R ¹ R ² ₂ SiO-represented by the following general formula (1) (R ² ₂ SiO) _L- SiR ¹ R ² ₂ (1)
(In the formula, each R ¹ represents a hydroxyl group, each R ² independently represents a hydrocarbon group having 1 to 20 carbon atoms, and L represents an integer of 3 to 10,000) and.
(B) Amino group-containing silane compound represented by the following general formula (2)
R ³ R ⁴ _m SiX _(3-m) (2)
(In the formula, R ³ represents a hydrocarbon group having at least one amino group and having 1 to 20 carbon atoms, R ⁴ represents an alkyl group having 1 to 4 carbon atoms, and X represents an alkoxy group having 1 to 4 carbon atoms. Represents, m is 0 or 1)
(B) An oil-in-water emulsified cosmetic containing hydrogenated phospholipids. The oil-in-water emulsified cosmetic according to claim 1, further comprising the component (C) a water-soluble thickener. The oil-in-water emulsified cosmetic according to claim 2 , wherein the component (C) is agar or a (PEG-240 / decyltetradeceth-20 / HDI) copolymer. Any of claims 1 to 3 in which the content mass ratio of the powder and the surface coating treatment agents (a) and (b) in the component (A) is 99.9: 0.1 to 90:10. The oil-in-water emulsified cosmetic according to item 1. The oil-in-water mold according to any one of claims 1 to 4, wherein the mass ratio of the component (A) to the surface coating treatment agents (a) and (b) is 100: 0.1 to 100: 35. Emulsified cosmetics. Claims 1 to 5 which are powders in which the component (A) is surface-coated with a polymer having a fine three-dimensional crosslinked structure of silicone, which is a condensation reaction of the surface coating treatment agents (a) and (b). The oil-in-water emulsified cosmetic according to any one of the above. The oil-in-water emulsified cosmetic according to any one of claims 1 to 6, wherein the oil-in-water emulsified cosmetic is solid. The oil-in-water emulsified cosmetic according to claim 7, which is obtained by heating and melting, filling a container, and cooling. The oil-in-water emulsified cosmetic according to any one of claims 1 to 8, wherein the content of the component (A) is 1 to 20%. The oil-in-water emulsified cosmetic according to any one of claims 1 to 9, wherein the content of the component (B) is 0.3 to 3.0%.