JP7010607B2 - Solid powder cosmetics - Google Patents

Description

The present invention relates to a solid powder cosmetic, and more particularly to a solid powder cosmetic having an excellent finish and usability, a function of more transmitting light in a long wavelength region (red light selective transmission function) while maintaining a hiding power. ..

Titanium dioxide has a high refractive index and is excellent in whiteness, hiding power, and coloring power, and is therefore widely used as a white pigment for paints, plastics, and the like. In addition, titanium dioxide can be used as a substance that shields ultraviolet rays, as an ultraviolet absorber or as an ultraviolet shielding agent, in cosmetics, catalysts, etc. by controlling its particle size or photoactivity. Therefore, in recent years, research and development for these uses has been actively carried out.

If titanium dioxide powder having an apparent specific average particle size formed from small spherical particles of titanium dioxide having a specific average primary particle size in the shape of a marimo formed from a large number of titanium dioxides is used for cosmetics, it is conventional. It is known that it becomes a functional material that can impart good slipperiness and excellent light resistance that titanium dioxide does not have. (Patent Document 1).
Further, 1 to 15% by mass of rutile-type titanium oxide aggregate particles having an average particle size of 0.2 to 0.4 μm and an average friction coefficient (MIU value) of 0.4 to 0.6, and a semi-solid oil content of 1 to 40. It is known that lip cosmetics containing% by mass are glossy, suppress the conspicuous wrinkles of the lips, and have excellent makeup retention (Patent Document 2).
In addition, by blending a color material used as a cosmetic with a low absorption rate of light on the long wavelength side (wavelength 630 to 700 nm) even in the visible light region, the light transmission inside the skin becomes closer to that of bare skin. , It is known that a natural finish can be realized (Patent Document 3).

As described above, as titanium oxide having increased light transmission on the long wavelength side of light, the rod-shaped particles are oriented and aggregated in a bundle shape, and the oriented and aggregated particles have an apparent average major axis length of 80 to 300 nm and are oriented and aggregated. The apparent average minor axis length of the particles is 30 to 150 nm, the apparent average major axis length / apparent average minor axis length is 1.1 to 4, and the specific surface area is 120 to 180 m ² / g. Strip-shaped or straw-bundle-shaped rutile-type titanium oxide, which is a type of titanium oxide, has been developed and is known to have high transparency and ultraviolet shielding ability (Patent Document 4).
However, this titanium dioxide is an agglomerate of rod-shaped particles, and since there are many vacant spaces in the secondary agglomerates, the apparent refractive index is lowered, and it has a hiding power to be actually blended in cosmetics. It was inadequate. Also, because the main purpose is to protect against UV rays, the apparent particle size of the secondary aggregate is also less than 100 nm, which is clearly smaller than the particle size that maximizes the scattering effect of titanium oxide based on Mie's theory. Therefore, this also causes a small hiding power.

On the other hand, it has been reported that treating the surface of the powder with an organopolysiloxane derivative improves the feeling of use when applied to the skin.
However, even if conventional titanium dioxide is blended with this organopolysiloxane derivative-treated powder, it has a high hiding power such as skin spots, but when it is blended in a large amount to enhance the hiding power, the finish becomes unnatural. , The unevenness on the skin may be more noticeable than the bare skin.

Under these circumstances, it is desired to develop a solid powder cosmetic containing titanium dioxide, which has excellent impact resistance and usability, and which gives a natural finish when applied to the skin.

Japanese Unexamined Patent Publication No. 2000-191325 Japanese Unexamined Patent Publication No. 2010-24189 Japanese Unexamined Patent Publication No. 2006-265134 Japanese Unexamined Patent Publication No. 2010-173863 Japanese Unexamined Patent Publication No. 2012-239039

Therefore, the present invention has been made in view of the above-mentioned prior art, and the problem to be solved is that light in a long wavelength region is more transmitted while maintaining hiding power while being excellent in impact resistance and usability. The present invention is to provide a solid powder cosmetic having an excellent function (red light selective transmission function).

As a result of diligent research conducted by the present inventors to solve the above-mentioned problems, titanium dioxide having a specific particle size, a specific crystallite size, and a specific specific surface area by firing a specific titanium dioxide is used as a cosmetic. It was found that it has an excellent red light selective transmission function while having sufficient hiding power required for the material. The titanium dioxide mixed with a specific surface-treated talc and spherical powder has excellent usability and impact resistance, and has a natural finish and no whitening when applied to the skin. Do you get it.

（一般式（１）中、Ｘは炭素数１～１８のアルキル基、Ｒ，Ｒ’はアルキル基である。）

前記記載の固形粉末化粧料において、（Ｂ）成分が、下記一般式（２）で表されるカルボキシル基を有するシリコーンポリマー又は下記一般式（３）カルボキシル基を有するアクリルポリマーであることを特徴とする固形粉末化粧料。

（式中Ｒ1及びＲ2は、メチル基若しくは下記の［化３］で表される基を示し、該基を１分子中に１～１００含有し、ｙは１～５０，０００の整数を表す。）

本発明にかかる固形粉末化粧料は、Ｘ線回折法で測定される平均結晶子径が１５～３０ｎｍ、比表面積が１０～３０ｍ^２／ｇであって、450nmの反射率の値が、650nmの反射率の値の1.3倍以上であり、色差（ΔＥ）が２２以下であるルチル型二酸化チタン粉体を1～30質量％と、
球状粉末5～30質量％と、
下記（A）成分と（B）成分からなるエラストマーまたは金属石鹸表面処理された粉末 を5～40質量％と、を含むことを特徴とする。
（Ａ）アミノ基を有するシリコーンポリマーと、
（Ｂ）カルボキシル基を有するシリコーンポリマー又はカルボキシル基を有するアクリルポリマーと、
からなるエラストマーであって、アミノ基とカルボキシル基のモル比が、Ｙ／Ｘ＝０．１～１．２ （Ｙは、（B）成分に含まれるカルボキシル基のモル量、Ｘは、（A）成分に含まれるアミノ基のモル量）の範囲にある。
なお、色差（ΔＥ）は、二酸化チタン粉体を５％の濃度になるようにニトロセルロースラッカーに分散混合し、得られた分散物を白黒の隠蔽率試験紙ＪＩＳ－Ｋ５４００上に０．１０１μｍの膜厚で塗布・乾燥して試験サンプルを得た。得られた試験サンプルを分光測色機にて、白と黒紙上の塗膜表面をそれぞれ測色した。Ｈｕｎｔｅｒ Ｌａｂ色空間における、色差（ΔＥ）を算出した。
本発明にかかる固形粉末化粧料は、下記の（ａ）～（ｃ）を満たす粒子表面に針状突起を有するルチル型二酸化チタンを焼成して得られるルチル型二酸化チタン粉体であって、見かけ上の平均粒子径が１００nm以上、５００ｎｍ未満、Ｘ線回折法で測定される平均結晶子径が１５～３０ｎｍ、比表面積が１０～３０ｍ２／ｇである二酸化チタン粉体を1～30質量％と、
球状粉末5～30質量％と、
下記（A）成分と（B）成分からなるエラストマーまたは金属石鹸表面処理された粉末を5～40質量％と、を含むことを特徴とする。
と、を含むことを特徴とする固形粉末化粧料。
（ａ）見かけ上の平均粒子径が１００ｎｍ以上、５００ｎｍ未満
（ｂ）Ｘ線回折法で測定される平均結晶子径が１～２５ｎｍ
（ｃ）比表面積が４０～２００ｍ２／ｇ
（Ａ）アミノ基を有するシリコーンポリマーと、
（Ｂ）カルボキシル基を有するシリコーンポリマー又はカルボキシル基を有するアクリルポリマーと、
からなるエラストマーであって、アミノ基とカルボキシル基のモル比が、Ｙ／Ｘ＝０．１～１．２ （Ｙは、（B）成分に含まれるカルボキシル基のモル量、Ｘは、（A）成分に含まれるアミノ基のモル量）の範囲にある
本発明にかかる固形粉末化粧料は、下記の（ａ）～（ｃ）を満たす粒子表面に針状突起を有するルチル型二酸化チタンを焼成して得られるルチル型二酸化チタン粉体であって、焼成後のルチル型二酸化チタン粉体の比表面積が、焼成前に対して８～50%であることを特徴とする二酸化チタン粉体を1～30質量％と、
球状粉末5～30質量％と、
下記（A）成分と（B）成分からなるエラストマーまたは金属石鹸表面処理された粉末 を5～40質量％と、を含むことを特徴とする。
と、を含むことを特徴とする固形粉末化粧料。
（ａ）見かけ上の平均粒子径が１００ｎｍ以上、５００ｎｍ未満
（ｂ）Ｘ線回折法で測定される平均結晶子径が１～２５ｎｍ
（ｃ）比表面積が４０～２００ｍ２／ｇ
（Ａ）アミノ基を有するシリコーンポリマーと、
（Ｂ）カルボキシル基を有するシリコーンポリマー又はカルボキシル基を有するアクリルポリマーと、
からなるエラストマーであって、アミノ基とカルボキシル基のモル比が、Ｙ／Ｘ＝０．１～１．２ （Ｙは、（B）成分に含まれるカルボキシル基のモル量、Ｘは、（A）成分に含まれるアミノ基のモル量）の範囲にある
前記固形粉末化粧料において、二酸化チタンの焼成温度が、500℃～800℃であることが好適である。
前記固形粉末化粧料において、二酸化チタンの焼成温度が、550℃～750℃であることが好適である。 That is, the titanium dioxide powder according to the present invention has an apparent average particle diameter of 100 nm or more and less than 500 nm, an average crystallite diameter measured by the X-ray diffractometry of 15 to 30 nm, and a specific surface area of 10 to 30 m2 / g. The particles have a shape in which the needle-shaped protrusions protruding radially are condensed, and the ratio of the minor axis to the major axis (major axis / minor axis) is 1.0 or more and less than 2.5. The characteristic titanium dioxide powder is 1 to 30% by mass,
Spherical powder 5 to 30% by mass,
It is characterized by containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) In the solid powder cosmetics in the range of the molar amount of amino groups contained in the component), it is preferable that the component (A) is a side chain type amino-modified silicone represented by the following general formula (1). ..

(In the general formula (1), X is an alkyl group having 1 to 18 carbon atoms, and R and R'are alkyl groups.)

In the above-mentioned solid powder cosmetics, the component (B) is characterized by being a silicone polymer having a carboxyl group represented by the following general formula (2) or an acrylic polymer having the following general formula (3) carboxyl group. Solid powder cosmetics.

(In the formula, R1 and R2 represent a methyl group or a group represented by the following [Chemical formula 3], and 1 to 100 of the group is contained in one molecule, and y represents an integer of 1 to 50,000. )

The solid powder cosmetic according to the present invention has an average crystallite diameter of 15 to 30 nm and a specific surface area of 10 to 30 m ² / g measured by an X-ray diffraction method, and has a reflectance value of 450 nm of 650 nm. Rutyl-type titanium dioxide powder having a reflectance of 1.3 times or more and a color difference (ΔE) of 22 or less is 1 to 30% by mass.
Spherical powder 5 to 30% by mass,
It is characterized by containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) The amount of molar amount of amino group contained in the component).
The color difference (ΔE) was 0.101 μm on the black-and-white concealment test paper JIS-K5400 by dispersing and mixing titanium dioxide powder in a nitrocellulose lacquer so as to have a concentration of 5%. A test sample was obtained by applying and drying with a film thickness. The obtained test sample was colorimetrically measured on the surface of the coating film on white and black paper using a spectrophotometer. The color difference (ΔE) in the Hunter Lab color space was calculated.
The solid powder cosmetic according to the present invention is a rutyl-type titanium dioxide powder obtained by firing rutyl-type titanium dioxide having needle-like protrusions on the surface of particles satisfying the following (a) to (c), and is apparent. Titanium dioxide powder having an average particle size of 100 nm or more and less than 500 nm, an average crystallite diameter of 15 to 30 nm measured by X-ray diffractometry, and a specific surface area of 10 to 30 m2 / g is 1 to 30% by mass. ,
Spherical powder 5 to 30% by mass,
It is characterized by containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
And, a solid powder cosmetic characterized by containing.
(A) Apparent average particle diameter is 100 nm or more and less than 500 nm (b) Average crystallite diameter measured by X-ray diffraction method is 1 to 25 nm.
(C) Specific surface area is 40-200 m2 / g
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) The solid powder cosmetic according to the present invention in the range of the molar amount of amino groups contained in the component) fires rutyl-type titanium dioxide having needle-like protrusions on the surface of particles satisfying the following (a) to (c). 1 of the rutile-type titanium dioxide powder obtained in the above process, wherein the specific surface area of the rutile-type titanium dioxide powder after firing is 8 to 50% of that before firing. ~ 30% by mass,
Spherical powder 5 to 30% by mass,
It is characterized by containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
And, a solid powder cosmetic characterized by containing.
(A) Apparent average particle diameter is 100 nm or more and less than 500 nm (b) Average crystallite diameter measured by X-ray diffraction method is 1 to 25 nm.
(C) Specific surface area is 40-200 m2 / g
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) The firing temperature of titanium dioxide in the solid powder cosmetics in the range of the molar amount of amino groups contained in the component) is preferably 500 ° C to 800 ° C.
In the solid powder cosmetics, it is preferable that the firing temperature of titanium dioxide is 550 ° C to 750 ° C.

According to the present invention, there is provided a solid powder cosmetic having excellent impact stability, excellent finish and usability, and excellent function of transmitting light in a long wavelength region (red light selective transmission function) while maintaining hiding power. can do.

How to calculate the apparent average particle size It is a figure which shows the spectral reflectance of rutile type pigment grade titanium oxide (* 1), titanium oxide B (unfired) and titanium oxide B fired at 700, 900 degreeC. It is a figure which shows the change of the shape of the titanium dioxide B fired at each firing temperature by TEM observation. It is a figure which shows the change of the hiding power of titanium oxide B by the change of the firing temperature in a rotary kiln. It is a figure which shows the change of the red permeability by the change of the firing temperature of titanium oxide B by the change of the firing temperature in a rotary kiln.

The titanium dioxide powder according to the present invention is obtained by firing titanium dioxide having needle-like protrusions on the surface of particles in which rod-shaped or needle-shaped particles are radially oriented and aggregated at 500 to 800 ° C, more preferably 550 to 750 ° C. Titanium dioxide powder having an average crystallite diameter of 15 to 30 nm measured by X-ray diffractometry, an apparent average particle size of titanium dioxide of 100 nm or more and less than 500 nm, more preferably 200 to 400 nm, and a specific surface area. Is 10 to 30 m ² / g.

[Titanium dioxide used for the mother nucleus]
The crystal type of titanium dioxide used for the mother nucleus is classified into anatase type and rutile type due to the difference in crystal structure. Here, the crystal type of titanium dioxide used in the present invention needs to be a rutile type having a low photocatalytic activity and a high refractive index, and therefore has a high hiding power.

As the rutile-type titanium dioxide used for the mother nucleus, titanium dioxide having a red light transmitting function is used. Considering that the apparent average particle size of titanium dioxide used for the mother nucleus generally causes a shrinkage phenomenon after firing, the hiding power due to the scattering of titanium dioxide obtained in the present invention and the excellent red transmission function are realized. From this point of view, it is preferably 100 nm or more and less than 500 nm, and more preferably 200 to 400 nm.

Examples of the shape of rutile-type titanium dioxide used for the mother nucleus include cocoon-shaped, straw-bundle-shaped, strip-shaped, spherical, needle-shaped, rod-shaped and the like. In the present invention, it is preferable that the rod-shaped or needle-shaped particles have needle-shaped protrusions on the surface of the particles that are radially oriented and aggregated.

The specific surface area of titanium dioxide used for the mother nucleus is preferably 40 to 200 m ² / g from the viewpoint of efficient improvement of the apparent refractive index by firing.

The rutile-type titanium dioxide used for the mother nucleus preferably has an average crystallite diameter of 1 to 25 nm measured by an X-ray diffraction method.

The titanium dioxide used for the mother nucleus may be a commercially available product. For example, the ST700 series manufactured by Titan Kogyo Co., Ltd. can be mentioned. Among them, ST710 and the like can be mentioned.

[Titanium dioxide powder used in the present invention]
The titanium dioxide powder of the present invention can be obtained by calcining the titanium dioxide used for the mother nucleus.
The firing temperature is determined by the firing device, in which needle-shaped protrusions that radiate out from the surface of the particles that existed before firing are in the particles that have condensed by firing, and between the needle-shaped particles that have condensed by firing. It is desirable that the temperature conditions are such that the existing vacancy is reduced and the needle-shaped particles are sintered and the average crystallite diameter measured by the X-ray diffractometry does not increase excessively. This makes it possible to achieve both a sufficient hiding power and a red light selective transmission function.

The titanium dioxide powder used in the present invention is characterized in that the needle-like protrusions radially protruding from the surface of the particles existing before firing are in the form of particles condensed by firing. The particles are characterized in that the ratio of the minor axis to the major axis (major axis / minor axis) is 1.0 or more and less than 2.5. More preferably, it is 1.0 to 2.0.

The appropriate firing temperature varies depending on the firing apparatus, but when firing in a general firing furnace such as a muffle furnace or a rotary kiln, it is desirable to fire in the range of 500 to 800 ° C, more preferably 550 to 750 ° C. Below 500 ° C, the hiding power is not sufficient because the vacancy existing before firing is not sufficiently reduced, and above 800 ° C, sintering proceeds excessively and the red light selective transmission function is lost.

The titanium dioxide of the present invention needs to have an average crystallite diameter of 15 to 30 nm as measured by an X-ray diffraction method.
If the crystallite diameter is less than 15 nm, it is not preferable because sufficient hiding power cannot be obtained. On the other hand, if it exceeds 30 nm, sintering proceeds and a sufficient red light selective transmission function is lost, which is not preferable.

Further, the titanium dioxide powder of the present invention has an apparent average particle size of 100 nm or more, less than 500 nm, more preferably 200 to 400 nm from the viewpoint of effectively realizing the hiding power by scattering and the excellent red transmission function. It is necessary to be.

The specific surface area of the titanium dioxide powder used in the present invention is an index showing the decrease in the porosity of the obtained titanium oxide particles and the progress of sintering, and the specific surface area of the titanium dioxide powder as the mother nucleus after firing is the specific surface area. It is preferably in the range of 8 to 50% as compared with that before firing (100%). More preferably, it is 8 to 30%.

Further, the specific surface area of the titanium dioxide powder of the present invention needs to be 10 to 30 m ² / g. If it is less than 10 m ² / g, sintering proceeds and sufficient red light selective transmission function is lost, which is not preferable. Further, if it exceeds 30 m ² / g, there are excessive voids, which is not preferable in that sufficient hiding power cannot be achieved.

The titanium dioxide powder of the present invention can also be surface-treated after firing. By performing the surface treatment, it is possible to obtain titanium dioxide having excellent usability while improving the viscosity, the dispersibility in oil, and the long-lasting makeup associated with water repellency.

Examples of the inorganic substance that can be used as the surface treatment agent include hydrous oxides or oxides of metals such as aluminum, silicon, zinc, titanium, zirconium, iron, cerium and tin. The metal salt used for this is not particularly limited.

Organic substances that can be used as surface treatment agents include, for example, stearic acid, oleic acid, and isostear in order to add lipophilicity after surface treatment with metal oxides such as aluminum hydroxide and aluminum oxide and metal hydroxides. Acids, fatty acids such as myristic acid, palmitic acid, behenic acid, methylhydrogenpolysiloxane, dimethicone, alkyl (C8-C18, etc.) trialkoxysilane, amino-modified silicone, carboxyl-modified silicone and other silicone compounds, perfluoroalkylalkylphosphate Examples thereof include fluorine compounds such as salts, amino acid derivatives such as dextrin myristate, dextrin palmitate, lauroyl lysine, and lauroyl glutamate.

These surface treatment agents are preferably 1 to 10% by mass with respect to the titanium dioxide powder because of their high hiding power.

The titanium dioxide powder used in the present invention can be widely blended in cosmetics, pigments, inks, paints and the like.

The blending amount of titanium dioxide used in the present invention is 1 to 30% by mass, more preferably 5 to 15% by mass, based on the total weight of the powdered cosmetic. If it is less than 1% by mass, the effect of the titanium dioxide compounding of the present invention may not be obtained, and if it exceeds 30% by mass, the finish may be unnatural.

[Spherical powder]
The material of the spherical powder to be blended with the cosmetic of the present invention is not particularly limited as long as it is a material of the spherical powder that can be blended with ordinary cosmetics. For example, elastic spherical powder (eg, refill, urepearl, plastic powder), polyethylene, polypropylene, polystyrene, polymethyl methacrylate, polyamide resin (nylon), urethane, silicone resin, silicone rubber, silicone resin coated rubber, polytetrafluoride. Examples thereof include ethylene, silicon dioxide (silica), a copolymer resin of styrene and acrylic acid, a benzoguanamine resin, and cellulose.

Further, the spherical powder may be surface-treated. Examples of the surface treatment include silicone compound treatment, fluorine-modified silicone compound treatment, fluorine compound treatment, higher fatty acid treatment, higher alcohol treatment, fatty acid ester treatment, metal soap treatment, amino acid treatment, and alkyl phosphate treatment.

Commercially available spherical powders include KSP100 (manufactured by Shin-Etsu Chemical Co., Ltd.), KSP-300 (manufactured by Shin-Etsu Chemical Co., Ltd.), Nylon SP-500 (manufactured by Toray Industries, Inc.), and D-400 (Toray Pigment Co., Ltd.). Made)
And so on.

Further, the particle size (average particle size) of the spherical powder is preferably in the range of 1 to 30 μm from the viewpoint of usability, and particularly preferably in the range of 3 to 20 μm. The cosmetic of the present invention may contain one or more spherical powders.

The blending amount of the spherical powder in the cosmetic of the present invention is 5 to 30% by mass, preferably 10 to 20% by mass with respect to the cosmetic. If the blending amount exceeds 30% by mass, the moldability tends to be extremely deteriorated, and if it is less than 5% by mass, it becomes difficult to impart sufficient extensibility to the product.

It is used after being treated with talc, eras otomer or metal soap used in the present invention. The blending amount of the elas otomer-treated or metal soap-treated talc is preferably 5 to 40% by mass, more preferably 15 to 35% by mass in the cosmetic. If it is more than 40% by mass, it may be difficult to remove the cosmetics. If it is less than 5% by mass, a cosmetic having sufficient impact resistance may not be obtained.

[Elastomer-treated talc]
The elastomer for treating the talc used in the present invention with an elastomer can be obtained by the following method.

The elastomer according to the present invention is produced by mixing a silicone polymer having an amino group and a silicone polymer having a carboxyl group and heating the mixture.

(A) Silicone polymer having an amino group (A) The silicone polymer having an amino group used in the present invention is a side chain type amino-modified silicone represented by the following general formula (1).

（一般式（１）中、Ｘは炭素数１～１８のアルキル基、Ｒ，Ｒ’はアルキル基である。）

(In the general formula (1), X is an alkyl group having 1 to 18 carbon atoms, and R and R'are alkyl groups.)

In the general formula (1), m is preferably 20 to 2000 because the hardness of the obtained elastomer is preferable. If it is less than 20, it is not preferable in that an elastomer may not be formed. Further, if it exceeds 2000, it may cause difficulty in handling and manufacturing, which is not preferable.

In the general formula (1), n is preferably 1 to 100 because the hardness of the obtained elastomer is preferable. If it is less than 1, it may not be preferable in that it may not form an elastomer. Further, if it exceeds 100, it may not be preferable in that the elastomer may be too hard.

In the general formula (1), an alkyl chain is preferably used for R, and a propyl group is preferable because of mass productivity.
In the general formula (1), an alkyl chain is preferably used for R', and an ethyl group is preferable because of mass productivity.

(A) The amino group equivalent of the silicone polymer having an amino group is preferably 500 g / mol to 20000 g / mol because the hardness of the obtained elastomer is preferable. If the amino group equivalent is less than 500, the elastomer may be too hard, which is not preferable. Further, if the amino group equivalent exceeds 20000, an elastomer may not be formed, which is not preferable.

(A) Commercially available products of silicone polymers having an amino group include, for example, KF-8004, KF-8005S, KF-867S (manufactured by Shin-Etsu Chemical Co., Ltd.), XF42-B1989 (manufactured by MOMENTIVE), ADM1650, ADM1370 (Asahi Kasei). Wacker Silicone Co., Ltd.), SF8452C, SS3551 (Toray Dow Corning Co., Ltd.) and the like.

The amino group equivalent represents a numerical value representing the weight of the substance per mol of the amino group with respect to the substance containing the amino group.

(B) Silicone polymer having a carboxyl group or acrylic polymer having a carboxyl group As the (B) silicone polymer having a carboxyl group used in the present invention, the carboxyl group equivalent represented by the following general formula (2) is 1000 g / mol. It is a side-chain type carboxyl-modified silicone having a weight of about 40,000 g / mol.
The (B) acrylic polymer having a carboxyl group used in the present invention is a side chain type carboxyl-modified acrylic polymer having a carboxyl group equivalent of 200 g / mol to 1000 g / mol represented by the following general formula (3).

The above-mentioned carboxyl group equivalent represents a numerical value representing the weight of the substance per mol of the carboxyl group with respect to the substance containing the carboxyl group.

The general formula (2) is composed of the following chemical formula 2 and chemical formula 3.

（式中Ｒ1及びＲ2は、メチル基若しくは下記の［化３］で表される基を示し、該基を１分子中に１～１００含有し、ｙは１～５０，０００の整数を表す。）

(In the formula, R1 and R2 represent a methyl group or a group represented by the following [Chemical formula 3], and 1 to 100 of the group is contained in one molecule, and y represents an integer of 1 to 50,000. )

The general formula (3) is composed of the following chemical formula 4.

（一般式（３）中、m/(m+n) = 0～0.5である。）

(In the general formula (3), m / (m + n) = 0 to 0.5.)

Examples of commercially available products of the silicone polymer having a carboxyl group represented by the general formula (2) include Sensorcil PCA (manufactured by Croda International).

The acrylic polymer having a carboxyl group represented by the general formula (3) can be synthesized by a known method.
Specific examples include 12-methacrylamide dodecanoic acid (MAD) / 2-acrylamide-2-methylpropanesulfonic acid (AMPS) copolymer (90/10), 12-methacrylamide dodecanoic acid (MAD) 18.50 g (65). .37 mmol), 2-acrylamide-2-methylpropanesulfonic acid (AMPS: manufactured by Sigma-Aldrich Japan) 1.50 g (7.24 mmol), sodium hydroxide 0.29 g (7.25 mmol), azobisisobuty 0.30 g (1.83 mmol) of ronitrile (manufactured by Nakaraitesk) was dissolved in 60.0 g of methanol. Azobisisobutyronitrile was recrystallized from methanol according to a conventional method. Argon was bubbled for 60 minutes to degas, the container was covered with septum, and the mixture was heated at 60 ° C. for 20 hours for polymerization. After completion of the polymerization reaction, the reaction solution was dropped into a large excess of diethyl ether, and the precipitate was collected by suction filtration. After drying under reduced pressure, 15.2 g of a random MAD / AMPS copolymer (90/10) was obtained (yield: 75.1%). The weight average molecular weight was 50,000.

The carboxyl group equivalent of the component (B) is preferably 200 to 40,000 because the hardness of the obtained elastomer is preferable. If it is less than 200, the elastomer may be too hard, which is not preferable. Further, if it exceeds 40,000, it may not form an elastomer, which is not preferable.

The molar ratio of the amino group in the (A) silicone polymer having an amino group to the carboxyl group of (B) the silicone polymer having a carboxyl group or the acrylic polymer having a carboxyl group is Y / X = 0.1 to 1.2. (Y is the molar amount of the carboxyl group contained in the component (B), and X is the molar amount of the amino group contained in the component (A)). More preferably, it is 0.1 to 0.8. If it is less than 0.1, it may not form an elastomer, which is not preferable. Further, if it is larger than 1.2, it may not form an elastomer, which is not preferable.

The amount of the elastomer coated on the talc is 0.5 to 20% by mass, more preferably 1 to 15% by mass with respect to the talc. If it is blended in an amount of more than 20% by mass, talc may be fused and the moldability of the powdered cosmetic may be deteriorated, which is not preferable. Further, if the blending amount is less than 0.5% by mass, the effect of improving the feel may not be obtained, which is not preferable.

[Manufacturing method of elastomer-treated talc]
The elastomer-treated talc according to the present invention can be obtained by a step of mixing the talc with (A) a silicone polymer having an amino group and a step of mixing (B) a silicone polymer having a carboxyl group and heating the talc.

Elastomer-treated talc can be obtained by a known method for producing a coated powder. To give a specific example, talc and (A) a silicone polymer having an amino group are added to a henshal mixer and mixed at a low speed for 10 minutes. Then, (B) a silicone polymer having a carboxyl group is added thereto, mixed at a low speed for 10 minutes, and heated to obtain an elastomer-coated inorganic powder according to the present invention.
Further, the elastomer-coated inorganic powder according to the present invention can be obtained even if the order of addition of the component (A) and the component (B) is reversed.

[Metal soap treatment talc]
As the metal soap-treated talc used in the present invention, various metal soap-treated talc can be used. Examples of the metal soap treatment include decyltrisiloxane carboxylic acid metal treatment such as zinc decyltrisiloxane carboxylate, calcium stearate treatment, magnesium stearate treatment and the like.

For example, decyltrisiloxane carboxylic acid metal-treated talc is a talc surface-treated with a metal salt of a carboxydecyltrisiloxane derivative. As the metal salt of the carboxydecyltrisiloxane derivative, all or part of the terminal carboxyl group of the derivative forms a metal salt. Examples of such divalent or trivalent metal atoms include Zn, Mg, Ca, Ba, Mn, Fe, Co, Al, Ni, Cu, V, Mo, Nb, Ti and the like. Of these divalent or trivalent metal atoms, Zn or Mg can be particularly preferably used.

The carboxydecyltrisiloxane used in the present invention is a kind of carboxylic acid-modified silicone and is represented by the following general formula (4).

Its chemical name is 3- (10-carboxydecyl) -1,1,1,3,5,5,5-heptamethyltrisiloxane, which is a known carboxy-modified silicone. In the present invention, commercially available products such as "DOWN CORNING TORAY OP-1800MF CARBOXY FLUID (Toray Dow Corning) are preferably used.

The amount of the metal soap treatment coated on the talc is 0.5 to 20% by mass, more preferably 1 to 15% by mass with respect to the talc. If it is blended in an amount of more than 20% by mass, talc may be fused and the moldability of the powdered cosmetic may be deteriorated, which is not preferable. Further, if the blending amount is less than 0.5% by mass, the effect of improving the feel may not be obtained, which is not preferable.

[Manufacturing method of talc treated with decyltrisiloxane zinc carboxylate]
The zinc decyltrisiloxane carboxylate-treated talc can be obtained by a known method for producing a coated powder. To give a specific example, it is carried out by the following two types of methods, a dry method and a wet method. However, it is not limited to these.

Dry method After converting the organosiloxane derivative of the above chemical formula 5 into a sodium salt in a 1% sodium hydroxide aqueous solution, salt exchange is performed by further adding a 1% zinc chloride aqueous solution, and the Zn salt of the organosiloxane derivative is added. To prepare. Then, 15 g of talc and 5 g of the Zn salt of the organosiloxane derivative are pulverized and mixed.

Wet method 100 g of talc, 30.5 g of a 1% aqueous sodium hydroxide solution, 3 g of an organosiloxane derivative of the above compound 1, and 156 ml of a 1% aqueous solution of zinc chloride are sequentially added to disperse the mixture. The reaction up to this point is performed at 70 ° C. Then, the powder surface-treated by filtration is isolated, washed with water, dried (105 ° C., 12 hours), and pulverized using a pulverizer.

Surface treatment by a wet method is more preferably adopted. In the wet method, the mixing temperature is preferably 60 to 80 ° C. The mixing time varies depending on the amount to be processed and the type of powder, but is usually 1 to 1.
Preferably 3 hours

Here, the elastomer treatment and the metal soap treatment can be performed on powders other than talc.
For example, inorganic powders include boron nitride, sericite, natural mica, calcined mica, synthetic mica, synthetic sericite, alumina, mica, kaolin, bentonite, smectite, calcium carbonate, magnesium carbonate, calcium phosphate, silicic acid anhydride, magnesium oxide. , Tin oxide, iron oxide, ittrium oxide, chromium oxide, titanium oxide, zinc oxide, cerium oxide, aluminum oxide, magnesium oxide, chromium hydroxide, dark blue, ultramarine, calcium phosphate, aluminum hydroxide, barium sulfate, magnesium sulfate, silicic acid , Aluminum magnesium silicate, Calcium silicate, Barium silicate, Magnesium silicate, Aluminum silicate, Strontium silicate, Silicon carbide, Magnesium fluoride, Metallic acid tungstate, Magnesium aluminate, Magnesium aluminometasilicate, Chlorhydroxy Aluminum, clay, zeolite, hydroxyapatite, ceramic powder, spinel, mullite, cordierite, aluminum nitride, titanium nitride, silicon nitride, lanthanum, samarium, tantalum, terbium, europium, neodium, Mn-Zn ferrite, Ni-Zn ferrite, Silicone carbide, cobalt titanate, barium titanate, iron titanate, lithium cobalt titanate, cobalt aluminate, tin oxide containing antimon, indium oxide containing tin, magnetite, aluminum powder, gold powder, silver powder, platinum powder, copper powder, precious metal As colloid, iron powder, zinc powder, cobalt blue, cobalt violet, cobalt green, low-order titanium oxide, fine particle titanium oxide, butterfly-like barium sulfate, petal-like zinc oxide, tetrapod-like zinc oxide, fine particle zinc oxide, and pearl pigment. Titanium oxide coated mica, titanium oxide coated mica, titanium oxide coated synthetic mica, titanium oxide coated silica, titanium oxide coated synthetic mica, titanium oxide coated talc, zinc oxide coated silica, titanium oxide coated colored mica, red iron oxide coated mica, red iron oxide, Examples thereof include black iron oxide-coated mica titanium, carmine-coated mica titanium, and conjo-coated mica titanium.
Of these, mica, sericite, kaolin, titanium oxide, iron oxide, zinc oxide and the like are preferably used.

Organic powders include polyester powder, polyethylene powder, polypropylene powder, polymethylmethacrylate powder, polystyrene powder, polyurethane powder, benzoguanamine powder, polymethylmethacrylate powder, polymethylbenzoguanamine powder, polytetrafluoroethylene powder, cellulose, silk powder. , Nylon powder, 12 nylon powder, 6 nylon powder, styrene / acrylic acid copolymer powder, divinylbenzene / styrene copolymer powder, vinyl resin powder, urea resin powder, phenol resin powder, fluororesin powder, acrylic resin powder, Examples thereof include melamine resin powder, epoxy resin powder, polycarbonate resin powder, microcrystalline fiber powder, starch powder, lauroyl lysine powder and the like.

Examples of the surface active agent metal salt powder include zinc stearate, aluminum stearate, calcium stearate, magnesium stearate, zinc myristate, magnesium myristate, zinc cetyl phosphate, calcium cetyl phosphate, sodium cetyl phosphate and the like.

[Other ingredients]
The solid powder cosmetic according to the present invention includes other components such as esters, anionic surfactants, cationic surfactants, amphoteric surfactants and nonionic surfactants, as long as the effects of the present invention are not impaired. Moisturizers, water-soluble polymers, thickeners, film agents, UV absorbers, metal ion blockers, lower alcohols, polyhydric alcohols, sugars, amino acids, organic amines, polymer emulsions, pH adjusters, skin nutrients, Vitamin, antioxidant, antioxidant aid, fragrance, water and the like can be appropriately blended as needed, and can be produced by a conventional method according to the desired dosage form.
Although specific compoundable ingredients are listed below, solid powder cosmetics can be prepared by blending the above essential compounding ingredients with any one or more of the following ingredients.

Examples of the anionic surfactant include fatty acid sequent (eg, sodium laurate, sodium palmitate, etc.); higher alkyl sulfate ester salts (eg, sodium lauryl sulfate, potassium lauryl sulfate, etc.); alkyl ether sulfate ester salts (eg, eg, sodium lauryl sulfate). POE-sodium lauryl sulfate triethanolamine, POE-sodium lauryl sulfate, etc.); N-acylsarcosic acid (eg, sodium lauroyl sarcosin, etc.); higher fatty acid amide sulfonate (eg, N-myristoyl-N-methyltaurine sodium, palm). Oil fatty acid methyl taurid sodium, lauryl methyl taurid sodium, etc.); Phosphate ester salts (POE-oleyl ether phosphate sodium, POE-stearyl ether phosphoric acid, etc.); Sodium, monolauroyl monoethanolamide polyoxyethylene sulfosuccinate sodium, lauryl polypropylene glycol sodium sulfosuccinate, etc.); Acids, etc.); Higher fatty acid ester sulfate ester salts (eg, hardened coconut oil fatty acid, sodium glycyl sulfate, etc.); N-acylglutamate (eg, N-sodium lauroyl glutamate, disodium N-stearoyl glutamate, N-myristoyl-L). -Sulfated oil (eg, funnel oil, etc.); POE-alkyl ether carboxylic acid; POE-alkylallyl ether carboxylate; α-olefin sulfonate; higher fatty acid ester sulfonate; secondary Alcohol sulfate ester salt; higher fatty acid alkyrolamide sulfate ester salt; sodium lauroyl monoethanolamide succinate; N-palmitoyl aspartate ditriethanolamine; sodium caseinate and the like.

Examples of the cationic surfactant include alkyltrimethylammonium salts (eg, stearyltrimethylammonium chloride, lauryltrimethylammonium chloride, etc.); alkylpyridinium salts (eg, cetylpyridinium chloride, etc.); disstearyldimethylammonium chloride dialkyldimethylammonium salts; Polychloride (N, N'-dimethyl-3,5-methylenepiperidinium); alkyl quaternary ammonium salt; alkyldimethylbenzylammonium salt; alkylisoquinolinium salt; dialkylmoriphonium salt; POE-alkylamine; Examples thereof include an alkylamine salt; a polyamine fatty acid derivative; an ammonium alcohol fatty acid derivative; a benzalconium chloride; and a benzethonium chloride.

Examples of the amphoteric surfactant include imidazoline-based amphoteric surfactants (eg, 2-undecyl-N, N, N- (hydroxyethylcarboxymethyl) -2-imidazolin sodium, 2-cocoyl-2-imidazolinium hydroki. Side-1-carboxyethyroxy 2-sodium salt, etc.); Betaine-based surfactants (eg, 2-heptadecyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, lauryldimethylaminoacetic acid betaine, alkylbetaine, amide betaine) , Sulfobetaine, etc.) and the like.

Examples of the lipophilic nonionic surfactant include sorbitan fatty acid esters (eg, sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan sesquioleate, etc. Solbitan trioleate, penta-2-ethylhexylate diglycerol sorbitan, tetra-2-ethylhexylate diglycerol sorbitan, etc.; Glycerin acid, α, α'-glycerin pyroglutamate oleate, glycerin monostearate, malic acid, etc.); propylene glycol fatty acid esters (eg, propylene glycol monostearate, etc.); cured castor oil derivative; glycerin alkyl ether, etc. Be done.

Examples of the hydrophilic non-ionic surfactant include POE-sorbitan fatty acid esters (eg, POE-sorbitan monooleate, POE-sorbitan monostearate, POE-sorbitan monooleate, POE-sorbitan tetraoleate, etc.). POE-Sorbit fatty acid esters (eg, POE-Sorbit monolaurate, POE-Sorbit monooleate, POE-Sorbit pentaoleate, POE-Sorbit monostearate, etc.); POE-glycerin fatty acid esters (eg, POE) -POE-monooleates such as glycerin monostearate, POE-glycerin monoisostearate, POE-glycerin triisostearate, etc.); POE-fatty acid esters (eg, POE-distearate, POE-monodiolate, ethylene glycol distearate, etc.) ); POE-alkyl ethers (eg, POE-lauryl ether, POE-oleyl ether, POE-stearyl ether, POE-behenyl ether, POE-2-octyldodecyl ether, POE-cholestanol ether, etc.); For example, Pluronic etc.); POE / POP-alkyl ethers (eg, POE / POP-cetyl ether, POE / POP-2-decyltetradecyl ether, POE / POP-monobutyl ether, POE / POP-hydrous lanolin, POE -POP-glycerin ether, etc.); Tetra POE-Tetra POP-ethylene diamine condensates (eg, Tetronic, etc.); POE-Himasi oil hardened bean oil derivative (eg, POE-Himasi oil, POE-hardened bean oil, POE- Hardened castor oil monoisostearate, POE-hardened castor oil triisostearate, POE-cured castor oil monopyroglutamic acid monoisostearic acid diester, POE-hardened castor oil maleic acid, etc.); POE-mitsurou lanolin derivative (eg, POE-Solbit Mitsurou, etc.); Arcanolamide (eg, coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, etc.); POE-propylene glycol fatty acid ester; POE-alkylamine; POE-fatty acid amide; sucrose fatty acid. Examples include ester; alkylethoxydimethylamine oxide; trioleyl phosphate and the like.

Examples of the moisturizing agent include polyethylene glycol, propylene glycol, glycerin, 1,3-butylene glycol, xylitol, sorbitol, martitol, chondroitin sulfate, hyaluronic acid, mucoitin sulfate, caronic acid, atelocollagen, and cholesteryl-12-hydroxystearate. , Sodium lactate, bile acid salt, dl-pyrrolidone carboxylate, alkylene oxide derivative, short chain soluble collagen, diglycerin (EO) PO adduct, Izayoi rose extract, sardine extract, melilot extract and the like.

Natural water-soluble polymers include, for example, plant-based polymers (eg, Arabic gum, tragacanto gum, galactan, guar gum, carob gum, karaya gum, carrageenan, pectin, canten, quince seed (malmero), algae colloid (cassow extract), starch. (Rice, corn, potato, wheat), glycyrrhizinic acid); Micromolecular macromolecules (eg, xanthan gum, dextran, succinoglucan, burran, etc.); Animal macromolecules (eg, collagen, casein, albumin, gelatin, etc.), etc. Can be mentioned.

Examples of the semi-synthetic water-soluble polymer include starch-based polymers (for example, carboxymethyl starch, methyl hydroxypropyl starch, etc.); cellulose-based polymers (methyl cellulose, ethyl cellulose, methyl hydroxypropyl cellulose, hydroxyethyl cellulose, cellulose sulfate, etc.). , Hydroxypropyl cellulose, carboxymethyl cellulose, sodium carboxymethyl cellulose, crystalline cellulose, cellulose powder, etc.); Examples thereof include alginic acid-based polymers (for example, sodium alginate, propylene glycol alginate, etc.).

Examples of the synthetic water-soluble polymer include vinyl polymers (for example, polyvinyl alcohol, polyvinyl methyl ether, polyvinyl pyrrolidone, carboxyvinyl polymer, etc.); polyoxyethylene polymers (for example, polyethylene glycol 20,000, 40). , 000, 60,000 polyoxyethylene polyoxypropylene copolymer, etc.); Acrylic polymers (eg, sodium polyacrylate, polyethyl acrylate, polyacrylamide, etc.); Polyethyleneimine; Cationic polymers and the like.

Examples of the thickener include Arabic gum, carrageenan, carrageenan, tragacanto gum, carob gum, quince seed (malmero), casein, dextrin, gelatin, sodium pectinate, sodium aragnate, methyl cellulose, ethyl cellulose, CMC, hydroxyethyl cellulose, hydroxypropyl. Cellulose, PVA, PVM, PVP, Sodium Polyacrylate, Carrageenan Polymer, Locust Bean Gum, Gua Gum, Tamarinto Gum, Dialkyldimethylammonium Sulfate Cellulose, Xanthan Gum, Aluminum Magnesium Phosphate, Bentonite, Hectrite, A1Mg Phosphate (Bea Gum), Examples thereof include laponite and silicic anhydride.

Examples of the ultraviolet absorber include a benzoic acid-based ultraviolet absorber (for example, paraaminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglycerin ester, N, N-dipropoxy PABA ethyl ester, N, N-diethoxyPABA ethyl ester). , N, N-dimethyl PABA ethyl ester, N, N-dimethyl PABA butyl ester, N, N-dimethyl PABA ethyl ester, etc.); Anthranilic acid-based ultraviolet absorbers (eg, homomentyl-N-acetylanthranilate, etc.); Salicylic acid-based UV absorbers (eg, amil salicylate, menthyl salicylate, homomentyl salicylate, octyl salicylate, phenyl salicylate, benzyl salicylate, p-isopropanol phenyl salicylate, etc.); -4-Isopropyl cinnamate, Methyl-2,5-diisopropyl cinnamate, Ethyl-2,4-diisopropyl cinnamate, Methyl-2,4-diisopropyl cinnamate, propyl-p-methoxy cinnamate, isopropyl-p-methoxy Sinnamate, Isoamyl-p-Methoxysinamate, Octyl-p-methoxysinamate (2-ethylhexyl-p-methoxysinamate), 2-ethoxyethyl-p-methoxysinamate, Cyclohexyl-p-methoxysinamate, Ethyl -Α-Cyano-β-phenyl cinnamate, 2-ethylhexyl-α-cyano-β-phenyl cinnamate, glycerylmono-2-ethylhexanoyl-diparamethoxycinnamate, etc.; 2,4-Dihydroxybenzophenone, 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzophenone, 2,2', 4,4'-tetrahydroxybenzophenone, 2- Hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfonate, 4-phenylbenzophenone, 2-ethylhexyl-4'-phenyl- Benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone, etc.); 3- (4'-methylbenzylidene) -d, l-campayl, 3 -Benzylidene-d, l-Phenyl; 2-phenyl-5-methylbenzoxazole; 2,2'-hydroxy-5-methylphenylbenzotriazole; 2- (2'-hydroxy-5'-t-octylphenyl) Benzotriazole; 2- (2'-hydroxy-5'-methylphenylbenzotriazole; dibenzalazine; dianisoilmethane; 4-methoxy-4'-t-butyldibenzoylmethane; 5- (3,3-dimethyl-2-) Norbornylidene) -3-pentan-2-one, dimorpholinopyridazino; 2-ethylhexyl-2-cyano-3,3-diphenylacrylate; 2,4-bis-{[4- (2-ethylhexyloxy) -2 -Hydroxy] -phenyl} -6- (4-methoxyphenyl)-(1,3,5) -triazine and the like.

Examples of the metal ion sequestering agent include 1-hydroxyethane-1,1-diphosphonic acid, 1-hydroxyethane-1,1-diphosphonic acid tetrasodium salt, disodium edetate, trisodium edetate, and tetrasodium edetate. , Sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, phosphoric acid, citric acid, ascorbic acid, succinic acid, edetic acid, ethylenediamine hydroxyethyl triacetate trisodium and the like.

Examples of the lower alcohol include ethanol, propanol, isopropanol, isobutyl alcohol, t-butyl alcohol and the like.

Examples of the polyhydric alcohol include divalent alcohols (eg, ethylene glycol, propylene glycol, trimethylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, tetramethylene glycol, 2,3-butylene glycol, and the like. Pentamethylene glycol, 2-butene-1,4-diol, hexylene glycol, octylene glycol, etc.; trivalent alcohol (eg, glycerin, trimethylolpropane, etc.); tetravalent alcohol (eg, 1,2,6) -Pentaerythritol such as hexanetriol); pentavalent alcohol (eg, xylitol, etc.); hexavalent alcohol (eg, sorbitol, mannitol, etc.); polyhydric alcohol polymer (eg, diethylene glycol, dipropylene glycol, triethylene glycol, etc.) Polypylene glycol, tetraethylene glycol, diglycerin, polyethylene glycol, triglycerin, tetraglycerin, polyglycerin, etc.; divalent alcohol alkyl ethers (eg, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, etc.) Ethylene glycol monophenyl ether, ethylene glycol monohexyl ether, ethylene glycol mono2-methylhexyl ether, ethylene glycol isoamyl ether, ethylene glycol benzyl ether, ethylene glycol isopropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, etc. ); Divalent alcohol alkyl ethers (eg, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol butyl ether, diethylene glycol methyl ethyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl). Ether, Propylene Glycol Monomethyl Ether, Propylene Glycol Monoethyl Ether, Propylene Glycol Monobutyl Ether, Propylene Glycol Isole Ether, Dipropylene Glycol Methyl Ether, Dipropylene Glycol Ethyl Ether, Dipropylene Glycol Lubutyl ether, etc.); Dihydric alcohol ether esters (eg, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol monophenyl ether acetate, ethylene glycol diazibate, ethylene glycol disakushi) Nate, diethylene glycol monoethyl ether acetate, diethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propylene glycol monophenyl ether acetate, etc.; glycerin monoalkyl ether (eg, xyl). Alcohols, cerakil alcohols, batyl alcohols, etc.); Sugar alcohols (eg, sorbitol, martitol, maltotriose, mannitol, sucrose, erythritol, glucose, fructose, starch-degrading sugar, maltose, xylitos, starch-degrading sugar-reducing alcohol, etc.) ); Glysolid; Tetrahydroflufuryl alcohol; POE-Tetrahydrofurfuryl alcohol; POP-butyl ether; POP / POE-butyl ether; Tripolyoxypropylene glycerin ether; POP-glycerin ether; POP-glycerin ether phosphoric acid; POP / POE -Pentane erythritol ether, polyglycerin and the like can be mentioned.

Examples of the monosaccharide include tricarbose (eg, D-glycerylaldehyde, dihydroxyacetone, etc.); tetracarbose (eg, D-erythrose, D-elittlerose, D-treose, erythritol, etc.); , L-arabinose, D-xylose, L-lyxose, D-arabinose, D-ribose, D-librose, D-xylrose, L-xylrose, etc.); -Bushicose, D-galactose, D-fluctose, L-galactose, L-mannose, D-tagatose, etc.); Seven-carbon sugar (eg, aldoheptose, heprose, etc.); For example, 2-deoxy-D-ribose, 6-deoxy-L-galactose, 6-deoxy-L-mannose, etc.; amino sugars (eg, D-glucosamine, D-galactosamine, sialic acid, aminouronic acid, muramic acid, etc.) ); Uronic acid (for example, D-glucuronic acid, D-mannuronic acid, L-gluuronic acid, D-galacturonic acid, L-isulonic acid, etc.) and the like.

Examples of oligosaccharides include sucrose, gunthianose, umbelliferose, lactose, planteose, isolikunoses, α, α-trehalose, raffinose, lycnoses, umbilicin, stachyose velvas and the like.

Examples of polysaccharides include cellulose, quince seed, chondroitin sulfate, starch, galactan, dermatan sulfate, glycogen, Arabic gum, heparan sulfate, hyaluronic acid, tragant gum, keratan sulfate, chondroitin, xanthan gum, mucoitin sulfate, guagam, dextran, and keratosulfate. , Locust bean gum, succinoglucan, caronic acid and the like.

Examples of amino acids include neutral amino acids (eg, threonine, cysteine, etc.); basic amino acids (eg, hydroxylysine, etc.) and the like. Examples of the amino acid derivative include acyl sarcosine sodium (lauroyl sarcosine sodium), acyl glutamate, acyl β-alanine sodium, glutathione, pyrrolidone carboxylic acid and the like.

Examples of the organic amine include monoethanolamine, diethanolamine, triethanolamine, morpholine, triisopropanolamine, 2-amino-2-methyl-1,3-propanediol, 2-amino-2-methyl-1-propanol and the like. Can be mentioned.
Examples of the polymer emulsion include an acrylic resin emulsion, an ethylpolyacrylic acid emulsion, an acrylic resin liquid, a polyacrylic alkyl ester emulsion, a polyvinyl acetate resin emulsion, and a natural rubber latex.

Examples of the pH adjuster include buffers such as lactic acid-sodium lactate, citric acid-sodium citrate, and succinate-sodium succinate.
Examples of vitamins include vitamins A, B1, B2, B6, C, E and their derivatives, pantothenic acid and its derivatives, biotin and the like.
Examples of the antioxidant include tocopherols, dibutylhydroxytoluene, butylhydroxyanisole, gallic acid esters and the like.

Examples of the antioxidant aid include phosphoric acid, citric acid, ascorbic acid, maleic acid, malonic acid, succinic acid, fumaric acid, kephalin, hexametaphosphate, phytic acid, ethylenediamine tetraacetic acid and the like.

Other compoundable components include, for example, preservatives (ethylparaben, butylparaben, chlorphenesin, phenoxyethanol, etc.); anti-inflammatory agents (eg, glycyrrhizinic acid derivative, glycyrrhetinic acid derivative, salicylic acid derivative, hinokithiol, zinc oxide, allantin, etc.) ); Whitening agents (eg, placenta extract, yukinoshita extract, albutin, etc.); Various extracts (eg, Oubaku, Ouren, Shikon, Shakuyaku, Senburi, Birch, Sage, Biwa, Carrot, Aloe, Zeniaoi, Iris, Grape , Yokuinin, Hechima, Yuri, Saffron, Senkyu, Shokyu, Otogirisou, Ononis, Garlic, Togarashi, Chimpi, Touki, Seaweed, etc.), Activators (eg, Royal Jelly, Photosensitizer, Cholesterol Derivatives, etc.); , Nonylic acid valenylamide, nicotinic acid benzyl ester, nicotinic acid β-butoxyethyl ester, capsaicin, zingeron, cantalistinki, ictamol, tannic acid, α-borneol, tocopherol nicotinate, inositol hexanicotinate, cyclanderate, cinnaridine, Examples thereof include trazoline, acetylcholine, verapamil, cepharanthin, γ-orizanol, etc.; anti-lipid leaking agents (eg, sulfur, thiantol, etc.); anti-inflammatory agents (eg, salicylic acid, thiotaurine, hypotaurine, etc.).

In addition, metal sequestering agents such as disodium edetate, trisodium edetate, sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, and ascorbic acid, caffeine, tannin, verapamil, tranexamic acid and its derivatives, licorice, Various crude drug extracts such as carin and ichiyakuso, drugs such as tocopherol acetate, glycyrrhetinic acid, glycyrrhizinic acid and its derivatives or salts thereof, vitamin C, magnesium ascorbic acid phosphate, ascorbic acid glucoside, arbutin, whitening agents such as kodiic acid, etc. Amino acids such as arginine and lysine and derivatives thereof, saccharides such as fructose, mannose, erythritol, trehalose and xylitol can also be appropriately blended.

As the product form of the solid powder cosmetic according to the present invention, any product form in the category of powder cosmetic can be taken. Specifically, it can take product forms such as foundation, eye shadow, cheek color, body powder, perfume powder, baby powder, pressed powder, deodorant powder, and face powder.

[Manufacturing method of solid powder cosmetics]
<Dry manufacturing method>
Inorganic powder components, oily components and other components are mixed in advance with a Henschel mixer, and then crushed twice with a palperizer. Then, the obtained mixture is filled in a resin inner plate container and dry press-molded by a known method to obtain a solid powder cosmetic containing the titanium oxide of the present invention in the cosmetic.
<Other manufacturing methods>
As a method for producing by blending titanium oxide of the present invention with cosmetics, a known method can be used. For example, the production method for producing by drying a slurry using a volatile solvent according to Patent No. 542209, and the production method for producing by removing a slurry using a volatile solvent according to Patent No. 5972437 after filling. It can be preferably obtained.

The present invention will be described in more detail below with reference to examples, but the present invention is not limited thereto. Unless otherwise specified, the blending amount is shown in mass% with respect to the system in which the component is blended.
Prior to the description of the examples, the evaluation method of the titanium dioxide test used in the present invention will be described.

Evaluation (1): Method for measuring average crystallite diameter The sample was measured by an X-ray diffractometer (Geigerflex, manufactured by Rigaku Denki Co., Ltd.), and the average crystallite diameter was calculated by applying the Scherrer equation.

（評価基準）
×：25＜ΔＥ
△：２２ ＜ΔＥ≦25
○：ΔＥ≦２２ Evaluation (2): Evaluation of hiding power Titanium dioxide powder was dispersed and mixed with nitrocellulose lacquer so as to have a concentration of 5%, and the obtained dispersion was placed on a black-and-white hiding power test paper JIS-K5400 at 0.101 μm. A test sample was obtained by applying and drying to the thickness of. The obtained test sample was colorimetrically measured on the surface of the coating film on white and black paper with a spectrophotometer (CM-2600, manufactured by Konica Minolta). The color difference (ΔE) in the Hunter Lab color space was calculated and evaluated as the hiding power. The higher the ΔE, the smaller the hiding power, and the lower the ΔE, the higher the hiding power.
ΔE =

(Evaluation criteria)
×: 25 <ΔE
Δ: 22 <ΔE ≦ 25
◯: ΔE ≦ 22

Evaluation (3): Evaluation of red transparency Red transparency is the reflectance and wavelength at a wavelength of 450 nm among the spectral reflectances at each wavelength obtained by measurement on black paper, similar to the above-mentioned hiding power. The reflectance ratio at 650 nm (reflectance at a wavelength of 450 nm / reflectance at 650 nm: R450 / R650) was calculated.
The higher the R450 / R650, the higher the red transparency, and the lower the R450 / R650, the lower the red transparency.
(Evaluation criteria)
×: R450 / R650 ≦ 1.3
Δ: 1.3 <R450 / R650 ≦ 1.35
◯: 1.35 <R450 / R650 ≦ 1.4
◎: 1.4 <R450 / R650

Evaluation (4): Method for measuring specific surface area The specific surface area per unit mass is the Journal of the American Chemical Society, Vol. 60, p. 309, February 1938, which corresponds to the international standard ISO 5794/1 (Appendix D). It can be determined by the nitrogen adsorption method known as the described BET (Brunauer-Emmett-Teller) method.

Evaluation (5): Measurement method of apparent average particle diameter By the method shown in FIG. 1, the average value of the lengths of the major axis and the minor axis of the particles is taken.

[Selection of titanium oxide used for the mother nucleus]

First, the present inventors evaluated by the above evaluation method using pigment-grade rutile-type and anatase-type titanium oxides available as commercially available products. The results are shown in Table 1.

＊１：タイペーク ＣＲ－５０（石原産業社製、見掛け上の平均粒子径:200ｎｍ、形状:不定形）
＊２：バイエルチタンＡ（バイエル社製、見掛け上の平均粒子径：400ｎｍ、形状：不定形）

* 1: Typake CR-50 (manufactured by Ishihara Sangyo Co., Ltd., apparent average particle size: 200 nm, shape: amorphous)
* 2: Bayer Titanium A (manufactured by Bayer, apparent average particle size: 400 nm, shape: amorphous)

Both the rutile-type pigment-grade titanium oxide and the anatase-type pigment-grade titanium oxide had low red transparency. Moreover, even when these were fired at a high temperature, the red transparency was low.

The present inventors have investigated whether it is possible to produce a material having excellent hiding power by using rutile-type titanium oxide having high red permeability.
The present inventors used the method of Patent Document (Japanese Unexamined Patent Publication No. 2010-173863) to synthesize two kinds of titanium dioxide having different particle sizes and having needle-like protrusions on the surface of particles in which needle-like particles are radially oriented and aggregated. did.
Each of the obtained titanium oxides was used as titanium oxide A (specific surface area: 101 m2 / g, crystallite diameter: 5 nm, apparent average particle diameter: 0.2 to 0.3 μm, needle-like protrusion shape), and titanium oxide B (specific surface area). : 117 m2 / g, crystallite diameter: 11 nm, apparent average particle diameter: 0.3 μm, needle-like protrusion shape).

Further, titanium dioxide having needle-like protrusions on the surface of particles in which needle-shaped particles, which are commercially available products (ST-730; manufactured by Titanium Kogyo Co., Ltd.) are radially oriented and aggregated, is formed into titanium oxide C (specific surface area: 98 m2 / g, crystallized). Child diameter: 6 nm, apparent average particle diameter: 0.5 μm, needle-like protrusion shape).
Further, titanium dioxide having needle-like protrusions on the surface of particles in which needle-shaped particles, which are commercially available products (ST-750: manufactured by Titanium Kogyo Co., Ltd.) are radially oriented and aggregated, is obtained from titanium oxide D (84 m2 / g, crystallite diameter: 8.6 nm, apparent average particle size: 1.0 μm, needle-like protrusion shape).
In addition, titanium oxide, which is a commercially available product (MT062; manufactured by TAYCA CORPORATION) and whose particles are needle-shaped, is titanium oxide E (specific surface area: 47 m2 / g, crystallite diameter: 23.3 nm, apparent average particle diameter). : 65 nm, needle-like protrusion shape).

Using each titanium dioxide, titanium dioxide powder was obtained by the following method. The obtained titanium dioxide powder was evaluated by the above evaluation method, and the relationship between the type of titanium dioxide before firing and the firing temperature was examined. The results are shown in Tables 2 to 6.

(Manufacturing method of titanium dioxide powder)
Titanium dioxide powder was obtained by placing 100 g of titanium dioxide used for the mother nucleus in a quartz crucible and firing at each temperature for 1 hour in a muffle furnace.

Titanium oxide A (specific surface area: 101 m2 / g, crystallite diameter: 5 nm, apparent average particle size: 0.2 to 0.3 μm, needle-like protrusion shape)

Titanium oxide B (specific surface area: 117 m2 / g, crystallite diameter: 11 nm, apparent average particle size: 0.3 μm, needle-like protrusion shape)

Titanium oxide C (specific surface area: 98 m2 / g, crystallite diameter: 6 nm, apparent average particle size: 0.5 μm, needle-like protrusion shape)

Titanium oxide D (specific surface area: 84 m2 / g, crystallite diameter: 8.6 nm, apparent average particle diameter: 1 μm, needle-like protrusion shape)

Titanium oxide E (specific surface area: 47 m2 / g, crystallite diameter: 23.3 nm, apparent average particle diameter: 65 nm, needle-like protrusion shape)

In all of titanium oxides A to C, the hiding power was improved by raising the firing temperature. Since the specific surface area decreases as the temperature rises, it is possible that the emptiness present in the particles is reduced by the condensation of the radially oriented and aggregated needle-like particles that existed before firing. Recognize. This causes an apparent increase in the refractive index, and the hiding power is improved. However, the red permeability gradually decreased. In particular, when fired at a high temperature, excessive sintering occurred and the initial red transparency was significantly reduced.
In particular, for titanium oxide C having a large average particle size, the red permeability was almost lost at 700 ° C.
Further, as in the case of titanium oxides A to C, the specific surface area of titanium oxide D in which needle-shaped particles are radially oriented and aggregated decreases as the firing temperature rises, but the apparent particle size is the same as that of titanium oxides A to C. The improvement in hiding power was extremely small because of the extremely large amount. Further, the red transparency also remained low regardless of before and after firing because the apparent particle size was extremely large, and the desired red transparency could not be obtained.
Further, for titanium oxide E having a small average particle diameter before firing and consisting of a single needle-shaped particle, the shape did not change significantly even after firing and the red transparency was maintained, but the hiding power did not improve at all. rice field.

Furthermore, different shapes of titanium dioxide were examined.

Further, titanium dioxide, which is a commercially available product (TTO55 (A); manufactured by Ishihara Sangyo Co., Ltd.) and whose particles are granular, is titanium oxide F (specific surface area: 37 m2 / g, crystallite diameter: 24.8 nm, apparent average). Particle size: 50 nm, granular).
Further, titanium dioxide, which is a commercially available product (ST643: manufactured by Titanium Kogyo Co., Ltd.) in which rod-shaped particles are oriented and aggregated in a straw bundle shape, is obtained from titanium oxide G (specific surface area: 132 m2 / g, crystallite diameter: 8.6 nm, apparently). Average particle size: 200 nm, straw bundle-like).

Titanium oxide F (specific surface area: 37 m2 / g, crystallite diameter: 24.8 nm, apparent average particle diameter: 50 nm, granular)

As can be seen from Test Examples 6-1 to 6-4, when granular titanium oxide is calcined at 350 ° C. to 720 ° C., the crystallite diameter does not change, and the specific surface area and the crystallite diameter are both calcined according to the present invention. It does not become titanium oxide later.
Therefore, although it has red transparency, the desired hiding power was not obtained.

It is referred to as titanium oxide G (specific surface area: 132 m2 / g, crystallite diameter: 8.6 nm, apparent average particle diameter: 200 nm, straw bundle shape).

The titanium oxide used in Test Example 7-1 has (a) an apparent average particle size and (b) an average crystallite measured by an X-ray diffraction method, similarly to the titanium dioxide used for the mother nucleus of the present invention. It satisfies the diameter and (c) specific surface area, but does not have needle-like protrusions on the surface of the particles. Furthermore, since the ratio of the minor axis to the major axis is as large as 2.5, sufficient red transparency and hiding power cannot be realized even after firing.

From these studies, titanium oxide B having a wide allowable temperature range was suitable as the mother nucleus titanium oxide used in the present invention from the viewpoint of improving concealment and maintaining red transparency.

FIG. 2 shows the results of measuring the spectral reflectances of rutile-type pigment grade titanium oxide (* 1) and titanium oxide B (not fired, firing temperature: 700 ° C., 900 ° C.). In the measurement, titanium dioxide powder was dispersed and mixed with nitrocellulose lacquer so as to have a concentration of 5%, and the obtained dispersion was applied on a black and white concealment test paper JIS-K5400 with a film thickness of 0.101 μm. -Dried to obtain a test sample. The obtained test sample was colorimetrically measured on the surface of the coating film on black paper with a spectrophotometer (CM-2600, manufactured by Konica Minolta) to obtain spectral reflectance.

Therefore, TEM images of unfired and fired titanium dioxide B (firing temperatures: 300 ° C., 500 ° C., 700 ° C., 900 ° C.) were taken. The results are shown in FIG.
Further, for titanium dioxide B, the hiding power and red transparency due to the change in firing temperature in the rotary kiln were measured. The results are shown in FIGS. 4 and 5, respectively.

From the above results, when firing in a muffle furnace, an appropriate temperature range is more preferably 500 to 800 ° C, particularly 500 to 700 ° C.

Next, the present inventors finely examined the firing temperature in the range of 500 ° C. to 800 ° C. with titanium oxide B as the mother nucleus. That is, the present inventor evaluated the titanium dioxide powder in which the firing temperature was changed by the above evaluation method. The results are shown in Tables 5 and 6.

The firing was performed in a rotary firing furnace (rotary kiln), which is closer to mass production and has high firing efficiency.
In general, it is known that a rotary firing furnace has high firing efficiency and can obtain a similar firing state at a lower temperature than when firing in a muffle furnace that fires in a stationary state.

The specific surface area is an index showing a decrease in the porosity of the obtained titanium oxide particles and the progress of sintering, and the titanium dioxide used in the present invention has a specific surface area obtained by firing a titanium dioxide powder as a mother nucleus. Is preferably in the range of 8 to 30% as compared with that before firing (100%).

From these results, it was found that the firing temperature is preferably 550 to 700 ° C., and more preferably 575 to 660 ° C., for the excellent hiding power and red transparency.

[Manufacturing method of talc treated with decyltrisiloxane zinc carboxylate]
First, the present inventors prepared a surface-treated powder by subjecting talc (trade name JA68R, manufactured by Asada Flour Milling Co., Ltd.) to a surface treatment using the Zn salt of the above formula 4 as an organosiloxane derivative. did.

[Manufacturing method of elastomer-treated talc]
To a henshal mixer, (C) talc and a silicone polymer having a carboxyl group are added, and the mixture is mixed at low speed for 10 minutes. Then, a silicone polymer having an amino group was added thereto, mixed at a low speed for 10 minutes, and heated to obtain an elastomer-treated talc.

[Solid powder cosmetics]
Further, the present inventor always uses the titanium dioxide obtained at the firing temperature of 660 ° C. in Table 6 to prepare a solid powder cosmetic containing the hydrophobized titanium dioxide obtained by the following surface treatment method. Adjusted by law. Then, the obtained cosmetics were evaluated by the following evaluation method.

[Surface treatment method for titanium dioxide powder]
The obtained titanium dioxide powder was dispersed in ion-exchanged water, heated, adsorbed by 3% by mass of stearic acid, and then dehydrated, washed, and dried to obtain surface-treated titanium dioxide.

[Manufacturing method of solid powder cosmetics]
[Manufacturing method of solid powder cosmetics]
<Dry manufacturing method>
Inorganic powder components, oily components and other components are mixed in advance with a Henschel mixer, and then crushed twice with a palperizer. Then, the obtained mixture is filled in a resin inner plate container and dry press-molded by a known method to obtain a solid powder cosmetic containing the titanium oxide of the present invention in the cosmetic.
<Other manufacturing methods>
As a method for producing by blending titanium oxide of the present invention with cosmetics, a known method can be used. For example, the production method for producing by drying a slurry using a volatile solvent according to Patent No. 542209, and the production method for producing by removing a slurry using a volatile solvent according to Patent No. 5972437 after filling. It can be preferably obtained.

[Evaluation method for solid powder cosmetics]
Evaluation (6): Natural finish Ten specialist panels applied the sample to the face and evaluated the usability after application.
A: More than 7 out of 10 panels answered that the finish was natural.
B: Of the 10 panels, 5 or more and less than 7 answered that the finish was natural.
C: Less than 5 out of 10 panels answered that the finish was natural.

Evaluation (7): Good elongation A 10 specialized panels applied the sample to the face and evaluated the usability after application.
A: More than 7 out of 10 panels answered that they have good growth.
B: Of the 10 panels, 5 or more and less than 7 answered that they had good growth.
C: Less than 5 out of 10 panels answered that they had good growth.

Evaluation (8): No whitening The sample was applied to the face by 10 specialist panels, and the feeling of use after application was evaluated.
A: More than 7 out of 10 panels answered that there was no whitening.
B: Of the 10 panelists, 5 or more and less than 7 responded with no whitening.
C: Less than 5 out of 10 panels answered that their pores were not white.

Evaluation (9): No color unevenness Ten specialist panels applied the sample to the face and evaluated the usability after application.
A: More than 7 out of 10 panels answered that there was no color unevenness.
B: 5 or more and less than 7 out of 10 panels answered that there was no color unevenness.
C: Less than 5 out of 10 panels answered that there was no color unevenness.

Evaluation (10): Impact-stable surname Solid powder cosmetics were set in a compact container for cosmetics, dropped from a height of 50 cm onto a metal plate with the cosmetic surface facing down, and the number of times until cracking was examined. It was evaluated that each cosmetic had sufficient impact resistance when the average value of the number of tests (N) = 3 was 5 times or more.
○ ・ ・ ・ 5 times or more × ・ ・ ・ less than 5 times

(* 1) BAE-talc JA-68R manufactured by Miyoshi Kasei, Inc.
(* 2) Asada Flour Milling Talc JA-68R
(* 3) PDM-9WA manufactured by Topy Industries, Ltd.
(* 4) PDM-FE manufactured by Topy Industries, Ltd.
(* 5) Ronaflair Boroneige SF-12 manufactured by Merck Group, Inc.
(* 6) Typake CR-50 manufactured by Ishihara Sangyo Co., Ltd.
(* 7) MT-100TV manufactured by TAYCA CORPORATION
(* 8) OTS-2 Bengala No. 216P manufactured by Daito Kasei Kogyo Co., Ltd.
(* 9) OTS-2 STN-1 manufactured by Daito Kasei Kogyo Co., Ltd.
(* 10) OTS-2 BL-100 manufactured by Daito Kasei Kogyo Co., Ltd.
(* 11) D-400 manufactured by Toiro Pigment Co., Ltd.
(* 12) KSP-100 manufactured by Shin-Etsu Chemical Co., Ltd.

From Test Examples 7-1 to 7-2, the solid powder cosmetics using the titanium dioxide of the present invention and the surface-treated talc of the present invention can contain a high amount of spherical powder and are excellent in usability and impact stability. However, it was found to have a natural finish and no whitening when applied to the skin.
When titanium dioxide used for the mother nucleus is used as it is, it is inferior to Test Example 7-3 in terms of the covering power of spots and freckles, and the conspicuous texture.
From Test Examples 7-4 to 7-5, when the powder without the surface treatment of the metal soap represented by the present invention is used, it is inferior in terms of impact stability.
From Test Examples 7-6 to 7-7, it was found that when the conventional pigment grade titanium was used, it was inferior in terms of natural finish and no whitening when applied to the skin.
From Test Examples 7-8, it was found that when the amount of titanium dioxide of the present invention was less than the range of the present invention, it was inferior in terms of covering stains and freckles, and a natural finish could not be obtained.
From Test Examples 7-9, it was found that when the amount of titanium dioxide of the present invention was larger than the range of the present invention, it was inferior in terms of natural finish and no whitening.
From Test Examples 7-10, it was found that when the amount of the spherical powder was smaller than the range of the present invention, it was inferior in terms of spreadability.
From Test Example 7-11, it was found that when the amount of the spherical powder was larger than the range of the present invention, the impact stability was inferior.
From Test Examples 7-12, it was found that when the amount of talc used after the eras otomer treatment or the metal soap treatment was less than the range of the present invention, the impact stability was inferior.

From Test Examples 7-13, it was found that when the amount of talc used after the eras otomer treatment or the metal soap treatment was larger than the range of the present invention, the cosmetics could not be easily removed and the spreadability was inferior.

Claims (4)

The apparent average particle size is 200 nm or more and less than 500 nm, the average crystallite diameter measured by X-ray diffractometry is 15 to 30 nm, the specific surface area is 10 to 30 m ² / g, and the needle shape is radially protruding. 1 to 1 to titanium dioxide powder having a shape in which the protrusions of the above are condensed, and the ratio of the minor axis to the major axis (major axis / minor axis) is 1.0 or more and less than 2.5. With 30% by mass,
Spherical powder 5 to 30% by mass,
A solid powder cosmetic containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) Amount of amino group contained in the component) The solid powder cosmetic according to claim 1, wherein the component (A) is a side chain type amino-modified silicone represented by the following general formula (1).

(In the general formula (1), X is an alkyl group having 1 to 18 carbon atoms, and R and R'are alkyl groups.) In the solid powder cosmetic according to claim 1, the component (B) is a silicone polymer having a carboxyl group represented by the following general formula (2) or an acrylic polymer having the following general formula (3) carboxyl group. A solid powder cosmetic characterized by.

(In the formula, R ¹ and R ² indicate a methyl group or a group represented by the following [Chemical formula 3], and the group is contained in one molecule from 1 to 100, and y is an integer of 1 to 50,000. show.)

The apparent average particle size is 200 nm or more and less than 500 nm, the average crystallite diameter measured by X-ray diffraction is 15 to 30 nm, the specific surface area is 10 to 30 m ² / g, and the reflectance value at 450 nm is , 1.3 times or more the value of the reflectance at 650 nm, and the color difference (ΔE) is 22 or less.
Spherical powder 5 to 30% by mass,
A solid powder cosmetic containing 5 to 40% by mass of an elastomer or metal soap surface-treated powder composed of the following components (A) and (B).
(A) A silicone polymer having an amino group and
(B) A silicone polymer having a carboxyl group or an acrylic polymer having a carboxyl group,
It is an elastomer composed of, and the molar ratio of amino group to carboxyl group is Y / X = 0.1 to 1.2 (Y is the molar amount of carboxyl group contained in the component (B), and X is (A). ) The amount of molar amount of amino group contained in the component).
The color difference (ΔE) was 0.101 μm on the black-and-white concealment test paper JIS-K5400 by dispersing and mixing titanium dioxide powder in a nitrocellulose lacquer so as to have a concentration of 5%. A test sample was obtained by applying and drying with a film thickness. The obtained test sample was colorimetrically measured on the surface of the coating film on white and black paper using a spectrophotometer. The color difference (ΔE) in the Hunter Lab color space was calculated.

Images