JP7078402B2 - Surface-treated inorganic powder, method for producing the surface-treated inorganic powder, and cosmetics containing the surface-treated inorganic powder. - Google Patents

Description

The present invention relates to a surface-treated powder having greatly improved slipperiness and squeaky feeling, a method for producing the surface-treated inorganic powder, and a cosmetic containing the surface-treated inorganic powder.

Conventionally, in make-up cosmetics such as foundations and lipsticks, in order to conceal dullness, stains, freckles, etc. and produce beautiful-looking skin, other inorganic pigments such as titanium oxide and iron oxide have high coloring power. By adding a colorant such as a pigment or an organic pigment, the morphology and color tone of the skin are corrected.

As the colorant, titanium oxide or iron oxide pigment having a high refractive index and having a hiding power and a coloring power is often used. However, these titanium oxides and iron oxides have a particle size in the submicron range in order to maximize the hiding power and coloring power, and the particle shape is rod-shaped or substantially spherical, so that they have poor slipperiness and stay on the skin. It gives a squeaky feeling and often makes the cosmetic film uneven.

The cosmetic having an ultraviolet blocking effect contains metal oxides such as titanium oxide, zinc oxide, and cerium oxide having high refraction as inorganic powder. The powder has a particle size of less than submicron in order to bring out the ultraviolet shielding effect, and the particle size is in the nano region regardless of the particle shape. There are many. There is a need to develop high-quality powder cosmetics that have a comfortable slipperiness and a more uniform cosmetic film and have an ultraviolet blocking effect. In order to solve these problems, a method of making the particle shape into a straw bundle shape or a plate shape having a specific size and shape and various surface treatments are being studied. (Patent Documents 1 to 5)

JP-A-2010-173863 Japanese Unexamined Patent Publication No. 2000-191325 Japanese Patent Application Laid-Open No. 2008-56535 Japanese Unexamined Patent Publication No. 2000-86433 JP 2015-180614

However, these techniques have not yet been sufficient to achieve smooth, non-staining slipperiness and a uniform decorative film for colored pigments having a high refractive index and powders having an ultraviolet blocking effect.

A surface-treated inorganic powder with greatly improved slipperiness and squeaky feeling for colored pigments having a high refractive index and an inorganic powder having an ultraviolet blocking effect, a method for producing the surface-treated inorganic powder, and the surface-treated inorganic powder are blended. The purpose is to provide the powdered cosmetics.

As a result of diligent research to solve the above problems, the present inventor has obtained the above problems by surface-treating an inorganic powder having a high refractive index and a specific average particle size with a specific dimethylpolysiloxane and a specific aminosilane. We have found that it is possible to solve the problem, and have completed the present invention.

（ｍは３～１００、ｎは０～１００、ｍ＋ｎ＝２０～２００である。）

（Ｒ^３はエトキシ基で、Ｒ^４はアミノプロピル基である。）
（請求項２）
表面処理される無機粉体と表面処理剤である成分（１ー１）と（２）の和の配合比が粉体／表面処理剤＝９４／６～７０／３０（重量％）である、請求項１記載の表面処理無機粉体。
That is, the present invention relates to the following surface-treated inorganic powder.
(Claim 1)
Inorganic powder with a refractive index of 2.0 or more and an average particle size of 0.01 to 3.0 μm is a component (1) Methylhydrogenpolykiloxane of the following components [Chemical Formula 1-1] and (2) The following. A surface-treated inorganic powder coated with the surface-treating agent of the component [Chemical Formula 2] and having a dynamic friction coefficient of less than 0.5.

(M is 3 to 100, n is 0 to 100, and m + n = 20 to 200.)

(R ³ is an ethoxy group and R ⁴ is an aminopropyl group.)
(Claim 2)
The compounding ratio of the sum of the inorganic powder to be surface-treated and the components (1-1) and (2) which are surface-treating agents is powder / surface-treating agent = 94/6 to 70/30 (% by weight). The surface-treated inorganic powder according to claim 1.

(Claim 3)
Claim 1 in which the compounding ratio of the component (1-1) and the component (2), which are the surface treatment agents, is component ( 1-1 ) / component (2) = 85/15 to 40/60 (% by weight). Or the surface-treated inorganic powder according to 2.
(Claim 4)
The surface-treated inorganic powder according to any one of claims 1 to 3, wherein the inorganic powder is a metal oxide selected from the group consisting of titanium oxide, zinc oxide, iron oxide, and cerium oxide.

（ｍは３～１００、ｎは０～１００、ｍ＋ｎ＝２０～２００である。）

（Ｒ^３はエトキシ基で、Ｒ^４はアミノプロピル基である。）
（請求項６）
表面処理される無機粉体と表面処理剤である成分（１ー１）と（２）の和の配合比が無機粉体／表面処理剤＝９４／６～７０／３０（重量％）である、請求項５記載の表面処理無機粉体の製造方法。
The present invention also relates to a method for producing the surface-treated inorganic powder.
(Claim 5)
Inorganic powder with a refractive index of 2.0 or more and an average particle size of 0.01 to 3.0 μm is mixed with the methylhydrogenpolykiloxane of the following component [Chemical formula 1-1] and (2) the following component [Chemical formula 2 ]. ] , Which is a method for producing a surface-treated inorganic powder which is dried and pulverized by contacting with], and which has a dynamic friction coefficient of less than 0.5.

(M is 3 to 100, n is 0 to 100, and m + n = 20 to 200.)

(R ³ is an ethoxy group and R ⁴ is an aminopropyl group.)
(Claim 6)
The compounding ratio of the sum of the inorganic powder to be surface -treated and the components (1-1 ) and (2) which are surface-treating agents is inorganic powder / surface-treating agent = 94/6 to 70/30 (% by weight). , The method for producing a surface-treated inorganic powder according to claim 5.

(Claim 7)
5. Claim 5 that the compounding ratio of the component ( 1-1 ) and the component (2) which are the surface treatment agents is the component ( 1-1 ) / component (2) = 85/15 to 40/60 (% by weight). Alternatively, the method for producing a surface-treated inorganic powder according to 6.
(Claim 8)
The method for producing a surface-treated inorganic powder according to any one of claims 5 to 7, wherein the inorganic powder is a metal oxide selected from the group consisting of titanium oxide, zinc oxide, iron oxide, and cerium oxide.
(Claim 9)
A cosmetic containing 0.1 to 99% by weight of the surface-treated inorganic powder according to any one of claims 1 to 4 with respect to the total amount.

The surface-treated inorganic powder according to the present invention is a powder obtained by surface-treating a colored pigment having a refractive index of 2.0 or more or an ultraviolet shielding powder, and has good slipperiness and a surface treatment that greatly improves the squeaky feeling on the skin. It is an inorganic powder. By blending this powder in a cosmetic, it is possible to achieve a smooth and smooth cosmetic film without a feeling of stain.

Hereinafter, the present invention will be described in detail.
INDUSTRIAL APPLICABILITY The present invention is an inorganic powder having a refractive index of 2.0 or more, which has poor slipperiness and a strong squeaky feeling on the skin, for example, a surface-treated inorganic powder having greatly improved slipperiness and squeaky feeling such as titanium oxide and zinc oxide. It is an object of the present invention to provide a method for producing the surface-treated inorganic powder and a cosmetic containing the surface-treated inorganic powder.

Regarding the invention of the product according to claim 1 of the present application, a method for producing a surface-treated inorganic powder "coated with a surface treatment agent" and the product is described, but this description is impossible or impractical. I had no choice but to adopt it.
Although the prior art has not yet been sufficient to achieve smooth, non-staining slipperiness and a uniform decorative film for colored pigments having a high refractive index and powders having an ultraviolet blocking effect, the present invention is ". A surface-treated inorganic powder obtained by coating an inorganic powder having a refractive index of 2.0 or more and an average particle size of 0.01 to 3.0 μm with the surface treatment agents of the following components (1) and (2). , Surface-treated inorganic powder with a dynamic friction coefficient of less than 0.5 ”, which greatly improves the slipperiness and squeaky feeling of colored pigments having a high refractive index and inorganic powders having an ultraviolet blocking effect. It is the invention of powder.
In order to identify the features of the present invention which are not present in the prior art, as described in claim 1, "... surface-treated inorganic powder coated with the surface-treating agents of the components (1) and (2)". ", Which describes the matters specifying the invention. By providing this invention-specific item, a surface-treated inorganic powder that solves the problems of the prior art is obtained as described above (see Examples of the present specification).

However, although the above-mentioned characteristics of the present invention are defined by the characteristics that the dynamic friction coefficient of the surface-treated inorganic powder is less than 0.5, it cannot be directly specified by the structure of the object.
First, in the "... surface-treated inorganic powder coated with the surface treatment agents of component (1) and component (2)", the starting material inorganic powder has an average particle size of 0.01 to 3.0 μm. It is an aggregate of very fine particles, and the analysis and identification of the surface layer of the surface-treated inorganic powder coated with the surface treatment agent may have changed at the surface treatment stage of the inorganic powder itself. Also, it is difficult because each of the surface-treated inorganic powder particles is very fine and varies. Therefore, it is almost impossible to formally specify the structure of the surface layer of the surface-treated inorganic powder coated with the surface-treating agents of the components (1) and (2).

Secondly, it is almost impossible to analyze the structure of the surface layer of the surface-treated inorganic powder coated with the surface-treating agent having the above-mentioned invention characteristics based on a specific measurement from the analysis technique at the time of filing the present application. I think that the. Specifically, as a method for measuring the existence state of the material in detail, for example, a scanning electron microscope (SEM) or the like can be mentioned, but in consideration of the presence or absence of reaction, variation, surface treatment state, etc. of individual inorganic particles. And such a method alone is not suitable for structural identification. Even if an analytical instrument such as X-ray diffraction (XRD) is used, accurate general data cannot be obtained because the individual surface-treated inorganic powder particles are very fine and varied. As described above, the actual situation is that there is no appropriate means for measuring and analyzing the surface-treated inorganic powder.
It takes a significant amount of trial and error to repeat such difficult measurements many times, perform statistical processing, and find an index that identifies the structure of the surface-treated inorganic powder described above. Not the target.

1. 1. Surface-coated powder The surface-coated inorganic powder used in the present invention refers to an inorganic powder having a refractive index of 2.0 or more, and refers to zinc oxide, cerium oxide, iron oxide, metal oxides of titanium oxide, and SiC (refractive index). It is selected from the group of compounds such as carbides and nitrides such as rate 2.635), Si3N4 (refractive index 2.023) and AlN (refractive index 2.165). The inorganic powder may be one kind or two or more kinds of inorganic powders selected from the group. The reason why the refractive index is 2.0 or more is that the squeaky feeling of the powder is improved by applying a known surface treatment to the inorganic powder having a refractive index of less than 2.0 without applying the surface treatment of the present invention. Things are possible.
Further, the titanium oxide and zinc oxide may be coated with an oxide such as Al (OH) ₃ , Al ₂ O ₃ , and SiO ₂ in order to suppress the catalytic activity of the powder particles. The composite powder can also be used in the present invention as long as the refractive index is 2.0 or more. Among the above-mentioned inorganic powders, metal oxides of zinc oxide, cerium oxide, iron oxide, and titanium oxide are generally available at low prices and are preferable.
Inorganic powders of these types and above are usually blended in cosmetics as coloring pigments and ultraviolet shielding agents. A particle size having a primary particle size of submicron to several tens of nm is generally used, and the inorganic powder used in the present invention has an average particle size of 0.01 to 3.0 μm. The particle diameter referred to in the present invention refers to the primary particle diameter, and can be obtained as an average value by measuring the diameter of the vertical * horizontal * height from an image obtained by SEM, TEM, or the like. If the average particle size is less than 0.01, the amount of surface treatment becomes excessive in order to obtain the effect of the present invention, which makes it difficult to industrially manufacture and costly. A known surface treatment is sufficient because there is little stain when the thickness is larger than 3.0 μm.

（Ｒ¹はメチル基で、Ｒ^２は水素原子またはメトキシ基、エトキシ基のいずれかであり、ｍは、３～１００、ｎは０～１００、ｍ＋ｎ＝２０～２００のである。）
成分（１）の表面処理剤は、一般的に入手可能なものとしては化学名でメチルハイドロジェンポリシロキサンがあり、例えばＫＦ９９Ｐ、ＫＦ－９９０１、Ｘ－２１－５７５４Ｐ（以上、信越化学工業社製）が挙げられる。ＫＦ９９ＰやＫＦ－９９０１やＸ－２１－５７５４Ｐは、それぞれ分子内のＳｉ－Ｈ基率が異なる製品の名称である。これらの表面処理剤のみで本発明でいう粉体を表面処理しても本発明の効果は得られない。 2. 2. Surface treatment agent 2-1) Ingredient 1
In the present invention, the inorganic powder is surface-treated by contacting the following polysiloxane (1) and the following aminosilane (2).
The component (1), which is a surface treatment agent used in the present invention, has a structure having a hydrolyzable group in the side chain of linear dimethylpolysiloxane, and is represented by the following general formula.

(R ¹ is a methyl group, R ² is either a hydrogen atom, a methoxy group, or an ethoxy group, m is 3 to 100, n is 0 to 100, and m + n = 20 to 200.)
The surface treatment agent for component (1) is generally available under the chemical name of methylhydrogenpolysiloxane, for example, KF99P, KF-9901, X-21-5754P (all manufactured by Shin-Etsu Chemical Co., Ltd.). ). KF99P, KF-9901, and X-21-5754P are the names of products having different intramolecular Si—H groups. Even if the powder referred to in the present invention is surface-treated with only these surface treatment agents, the effect of the present invention cannot be obtained.

（Ｒ^３は、水酸基、メトキシ基、エトキシ基で、Ｒ^４はアミノエチル基、アミノプロピル基、アミノエチルアミノプロピル基のいずれかである。）
成分（２）の表面処理剤として一般に入手可能なものとしては、ＫＢＭ－９０３（アミノプロピルトリメトキシシラン）やＫＢＥ－９０３（アミノプロピルトリエトキシシラン）、ＫＢＭ－６０３（アミノエチルアミノプロピルトリメトキシシラン）（以上、信越化学工業社製）が挙げられる。これらの表面処理剤で本発明で言う粉体を表面処理しても本発明の効果は得られない。また、化粧料に適用可能な分子片末端に３官能の加水分解性基を有するアルキルシランやシリコーン化合物があるがこれらの表面処理剤で本発明で言う粉体を表面処理した場合でも本発明の効果は得られない。 2-2) Ingredient 2
The component (2), which is another surface treatment agent used in the present invention, is an aminosilane having a hydrolyzable group at the terminal of a molecular piece, and is represented by the following general formula.

(R ³ is a hydroxyl group, a methoxy group, or an ethoxy group, and R ⁴ is any of an aminoethyl group, an aminopropyl group, and an aminoethylaminopropyl group.)
Generally available surface treatment agents for component (2) include KBM-903 (aminopropyltrimethoxysilane), KBE-903 (aminopropyltriethoxysilane), and KBM-603 (aminoethylaminopropyltrimethoxysilane). ) (The above is manufactured by Shin-Etsu Chemical Co., Ltd.). Even if the powder referred to in the present invention is surface-treated with these surface treatment agents, the effect of the present invention cannot be obtained. Further, although there are alkylsilanes and silicone compounds having a trifunctional hydrolyzable group at the terminal of a molecular piece applicable to cosmetics, the present invention can be used even when the powder referred to in the present invention is surface-treated with these surface treatment agents. No effect is obtained.

3. 3. Blending amount
3-1) Blending ratio of surface-treated powder and component that is a surface treatment agent The blending ratio of the surface-treated inorganic powder and the component that is a surface treatment agent depends on the particle size of the powder, but is preferably inorganic powder. / Surface treatment agent (= component (1) + (2)) = 94/6 to 70/30 (% by weight). More preferably, in the case of an inorganic powder of submicron or more, the powder / surface treatment agent = 94/6 to 88/15 (% by weight). When the particle size is less than submicron, the inorganic powder / surface treatment agent = 90/10 to 70/30 (% by weight). If the amount of the surface treatment agent is smaller than the above, the surface treatment powder has poor slipperiness and a squeaky feeling. Further, if the amount of the surface treatment agent is larger than the above-mentioned compounding ratio, the powder particles aggregate in the surface treatment process and become agglomerates or clays, which cannot be recovered as the surface treatment powder, and the effect of the present invention can be obtained. I can't.

3-2) Blending ratio of component (1) and component (2), which are surface treatment agents The blending ratio of component (1) and component (2), which are the two types of surface treatment agents in the present invention, is the component ( 1) / component (2) = 85/15 to 40/60 (% by weight) is preferable. More preferably, the component (1) / component (2) = 70/30 to 50/50 (% by weight). Even if the amount of the component (1) is smaller or larger than the above, the smooth and non-staining surface-treated powder which is the effect of the present invention cannot be obtained.

4. Dynamic friction coefficient The dynamic friction coefficient (MIU value) of the surface-treated powder of the present invention is less than 0.5. This value is not preferable when the coefficient of dynamic friction is 0.5 or more because it lacks a smooth sliding feel and causes a squeaky feeling when applied to the skin.

For the measurement of the dynamic friction coefficient, for example, a static / dynamic friction measuring instrument TL201Tt (manufactured by Trinity Lab) can be used. Spread the measurement powder evenly on artificial leather (Suprale: manufactured by Idemitsu Technofine Co., Ltd.) with a sponge puff so that it becomes 0.5 mg / cm ² , and use a tactile contact (contact area: 15 x 10 mm; made of polyurethane). It can be obtained under the condition of a load of 100 g.

5. Powder surface treatment method The method for surface-treating the powder of the present invention is not particularly limited, and the surface treatment agent can be brought into contact with the surface of the powder particles for treatment. Examples of the dry method and the slurry method using a mixer such as a mixer include a method of treating in water or an organic solvent. As the slurry method, there are known methods such as a method of removing the treatment liquid and then drying and pulverizing the treatment liquid, and a method of spray-drying and pulverizing the treatment liquid in water or an organic solvent.
The following methods can be exemplified as the procedure for surface treatment.
<1> Method of mixing the component (1) and the component (2) and contacting them with the inorganic powder particles <2> The component (1) is first brought into contact with the inorganic powder particles, and then the component (2) is added. Method <3> Method of adding component (1) by first contacting component (2) with inorganic powder particles <4> ”Half amount of component (1) is first contacted with inorganic powder particles to add component (1). Method of adding the remaining half of the component (1) after adding the entire amount of 2) <5> First contact the half amount of the component (2) with the inorganic powder particles to add the entire amount of the component (1). Method of adding the other half of the component (2) From these methods, a method in which the dynamic friction coefficient is less than 0.5 is appropriately selected in consideration of the surface activity, acidity and basicity of the inorganic powder particles. You can select it.

After the surface treatment, a pulverization step is required for the purpose of adjusting the particle size of the dried powder and eliminating agglomerated particles having a certain size or more. As a crusher at this time, a crusher with a classifier is preferable when productivity, durability and the like are taken into consideration. For example, a ceramic JET crusher, a ceramic crusher with a hammer, a dry media crusher, or the like is suitable. Examples of commercially available products include the counter jet mill 200AFG-CRS (Hosokawa Micron Co., Ltd.), the V turbo (Freund Turbo Co., Ltd.), and the fine mill SF type (Nippon Coke Industries Co., Ltd.).

The cosmetics in the present invention are not particularly limited as long as they contain a powder having a refractive index of 2.0 or more, and examples thereof include skin care cosmetics, makeup cosmetics, sun care cosmetics, hair care cosmetics and the like. Can be mentioned.

Examples of the present invention are given below, but these examples are merely examples of the present invention, and the present invention is not limited thereto.
(Example 1)
Put 5 kg of titanium oxide (PFC-407: average particle size 0.35 μm: Ishihara Sangyo Co., Ltd.) into a 20-liter heater hensyl mixer (HM-20 type: Nippon Coke Co., Ltd.) and stir _N2 gas at low speed as seal air. Below, KF9901 (Methylhydrogenpolysiloxane: Shin-Etsu Chemical Co., Ltd.) 333.3 g (processing amount of 6 wt% by internal division) and KBE903 (Aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) 222.2 g (internal division) A liquid mixed with a treatment amount of 4 wt%) is added dropwise. After the dropping, the mixture is stirred at low speed for 10 minutes, the mixed powder is taken out, dried in a hot air dryer at 40 ° C. for 3 hours, and further dried at 130 ° C. for 5 hours. This powder was pulverized with V-Turbo (Freund Turbo) to obtain surface-treated titanium oxide.

(Example 2)
The titanium oxide of Example 1 was replaced with iron yellow oxide (Yellow LL-100P: average particle diameter 0.07 × 0.8 μm; Titanium Kogyo Co., Ltd.) and treated in the same manner with a powder amount of 3 kg for surface treatment yellow oxidation. I got iron.

(Example 3)
The titanium oxide of Example 1 was replaced with red iron oxide (Red R-516PS: average particle diameter 0.08 × 0.8 μm: Titanium Kogyo Co., Ltd.) and treated in the same manner to obtain surface-treated red iron oxide.

(Example 4)
The titanium oxide of Example 1 was replaced with black iron oxide (BL-100P: average particle diameter 0.42 μm; Titanium Kogyo Co., Ltd.), and KF9901 (methylhydrogenpolysiloxane: Shin-Etsu Chemical Co., Ltd.) 217.3 g (internal division). A treatment amount of 4 wt%) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) 217.3 g (treatment amount of 4 wt% by internal division) were treated in the same manner to obtain surface-treated black iron oxide.

(Example 5)
Titanium oxide of Example 1 was replaced with titanium oxide (MP-100: average particle size; 1.0 μm; TAYCA), and KF99P (methylhydrogenpolysiloxane: Shin-Etsu Chemical Co., Ltd.) 260.8 g (4 in the internal division). .8 wt% treatment amount) and KBM903 (aminopropyltrimethoxysilane: Shin-Etsu Chemical Co., Ltd.) 173.9 g (processing amount of 3.2 wt% by internal division) were treated in the same manner to obtain surface-treated titanium oxide. ..

(Example 6)
Replace the titanium oxide of Example 1 with zinc oxide (fine zinc oxide: average particle diameter 0.1 μm; Sakai Chemical Industry Co., Ltd.) and replace it with X-21-5754P (methylhydrogenpolysiloxane: Shinetsu Chemical Industry Co., Ltd.) 260.8 g. (Processing amount of 4.8 wt% by internal division) and KBM603 (Aminoethylaminopropyltrimethoxysilane: Shin-Etsu Chemical Industry Co., Ltd.) 173.9 g (Processing amount of 3.2 wt% by internal division) , A counter jet mill (Hosokawa Micron) was used to grind to obtain surface-treated zinc oxide.

(Example 7)
The titanium oxide of Example 1 was replaced with fine particle titanium oxide (STR-100C: average particle diameter 0.01 × 0.09 μm; Sakai Chemical Industry Co., Ltd.), the amount of powder was set to 3 kg, and KF9901 (hydrogen dimethicone: Shinetsu Chemical Industry Co., Ltd.) was used. (Company) 700 g (processing amount of 17.5 wt% by internal division) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Industry Co., Ltd.) 300 g (processing amount of 7.5 wt% by internal division), and the same treatment is performed by dropping. Then, it was pulverized with a counter jet mill (Hosokawa Micron Co., Ltd.) to obtain surface-treated fine particle titanium oxide.

(Example 8)
The titanium oxide of Example 1 was replaced with fine particle zinc oxide (MZ-300: average particle diameter 0.035 μm; Teika Co., Ltd.), the amount of powder was 4 kg, and KF9901 (hydrogen dimethicone: Shinetsu Chemical Industry Co., Ltd.) 600 g (internal division). 12.0 wt% treatment amount) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Industry Co., Ltd.) 300 g (8.0 wt% treatment amount by internal division), and then counter jet mill (Hosokawa Micron Co., Ltd.) ) To obtain surface-treated fine particle zinc oxide.

(Example 9)
Titanium oxide of Example 1 was replaced with titanium oxide (MP-70: average particle diameter 0.7 μm; TAYCA), 444.4 g (treatment amount of 8 wt% by internal division) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) A liquid mixed with 111.1 g (a treatment amount of 2 wt% by internal division) was added dropwise and treated in the same manner to obtain surface-treated titanium oxide.

(Comparative Example 1)
Titanium oxide (PFC-407: Ishihara Sangyo Co., Ltd.) of Example 1 was mixed with 263.1 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) and 100 g of isopropyl alcohol (IPA). Drop the liquid. After the dropping, the mixture is stirred at low speed for 10 minutes, the mixed powder is taken out, dried in a hot air dryer at 40 ° C. for 3 hours, and further dried at 130 ° C. for 5 hours. This powder was similarly pulverized to obtain surface-treated titanium oxide.

(Comparative Example 2)
KF9901 (hydrogendimethicone: Shin-Etsu Chemical Co., Ltd.) 157.5 g (3 wt% treatment amount by internal division) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) 105.2 g (inside) in 5 kg of titanium oxide of Comparative Example 1. A liquid mixed with a treatment amount of 2 wt%) was added dropwise and treated in the same manner to obtain surface-treated titanium oxide.

(Comparative Example 3)
A mixture of 555.5 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) and 100 g of isopropyl alcohol (IPA) was added dropwise to 5 kg of titanium oxide of Comparative Example 1 and treated in the same manner. The surface-treated titanium oxide was obtained.

(Comparative Example 4)
KF9901 (hydrogendimethicone: Shin-Etsu Chemical Co., Ltd.) 444.4 g (treatment amount of 8 wt% by internal division) and KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) 111.1 g (inside) in 5 kg of titanium oxide of Comparative Example 1. A liquid mixed with a treatment amount of 2 wt%) was added dropwise and treated in the same manner to obtain surface-treated titanium oxide.

(Comparative Example 5)
A solution prepared by dropping 555.5 g of KBE903 (aminopropyltriethoxysilane: Shin-Etsu Chemical Co., Ltd.) and 100 g of isopropyl alcohol (IPA) in 5 kg of titanium oxide of Comparative Example 1 was added dropwise. The same treatment was performed to obtain surface-treated titanium oxide.

(Comparative Example 6)
A solution prepared by adding 263.1 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) (a treatment amount of 5 wt% by internal division) and 100 g of isopropyl alcohol (IPA) is added dropwise to 3 kg of yellow iron oxide of Example 2. After the dropping, the mixture is stirred at high speed for 10 minutes, the mixed powder is taken out, dried at 60 ° C. for 5 hours in a hot air dryer, and further dried at 130 ° C. for 5 hours. This powder was similarly pulverized to obtain surface-treated iron oxide.

(Comparative Example 7)
A solution prepared by adding 263.1 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) (a treatment amount of 5 wt% by internal division) and 100 g of isopropyl alcohol (IPA) is added dropwise to 5 kg of red iron oxide of Example 3. After the dropping, the mixture is stirred at high speed for 10 minutes, the mixed powder is taken out, dried at 60 ° C. for 5 hours in a hot air dryer, and further dried at 130 ° C. for 5 hours. This powder was similarly pulverized to obtain surface-treated red iron oxide.

(Comparative Example 8)
A solution prepared by adding 263.1 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) (a treatment amount of 5 wt% by internal division) and 100 g of isopropyl alcohol (IPA) is added dropwise to 5 kg of black iron oxide of Example 4. After the dropping, the mixture is stirred at high speed for 10 minutes, the mixed powder is taken out, dried at 60 ° C. for 5 hours in a hot air dryer, and further dried at 130 ° C. for 5 hours. This powder was similarly pulverized to obtain surface-treated black iron oxide.

(Comparative Example 9)
Similarly, the surface treatment agent of 3 kg of fine particle titanium oxide (STR-100C: Sakai Chemical Industry Co., Ltd.) of Example 7 was KF9901 (hydrogen dimethicon: Shinetsu Chemical Industry Co., Ltd.) 1000 g (with a treatment amount of 25 wt% by internal division). The treatment was performed to obtain surface-treated fine particle titanium oxide.

(Comparative Example 10)
The surface treatment agent of 4 kg of fine particle zinc oxide (MZ-300: TAYCA) of Example 8 was treated in the same manner with only 1000 g of KF9901 (hydrogen dimethicone: Shin-Etsu Chemical Co., Ltd.) (with a treatment amount of 20 wt% by internal division). Surface-treated fine zinc oxide was obtained.

(Measurement of dynamic friction coefficient)
The measurement powder was spread evenly on artificial leather with a sponge puff so as to be 0.5 mg / cm ² , and the measurement was performed under the following measurement conditions.
Device name: Static / dynamic friction measuring instrument TL201Tt (manufactured by Trinity Lab)
Contact: Tactile contact (area 15 x 10 mm = 1.5 cm ² )
Load: 100g
Measurement distance: 30 mm
Measurement speed: 30 mm / s

The MIU value and the like of the surface-treated powder are as follows.

(Evaluation of cosmetics)
The cosmetics obtained in each of the cosmetics of the following examples and comparative examples were subjected to an actual usability test by a specialized panel of 20 people. As evaluation items, smoothness at the time of application, no squeaky feeling, uniformity of cosmetic film, etc. were evaluated according to the following evaluation criteria.

(Evaluation point standard)
5 points: Very good.
4 points: Excellent.
3 points: Normal.
2 points: Inferior.
1 point: Very inferior.

[Example 10 and Comparative Examples 11 to 13] Powder foundation

(Production method)
1. 1. Mix the powder components evenly.
2. 2. Above 1. Add oily ingredients to the mixture, mix and crush, and pass through the fluid.
3. 3. Above 2. Was molded into an aluminum dish to obtain a powder foundation.
The cosmetic containing the surface-treated powder of the present invention is smoother and has no stain feeling as compared with the cosmetics of the comparative examples, and is excellent in the uniformity of the cosmetic film.

（製造方法）
１．粉体成分を均一に混合・粉砕した後フルイを通して粉白粉を得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較して滑らかできしみ感が無く化粧膜の均一性に優れている。 [Example 11 and Comparative Example 14] Powder white powder

(Production method)
1. 1. After the powder components were uniformly mixed and crushed, a powdery white powder was obtained through a fluid.
The cosmetic containing the surface-treated powder of the present invention is smoother and has no stain feeling as compared with the cosmetics of the comparative examples, and is excellent in the uniformity of the cosmetic film.

（製造方法）
１．油性成分を９０℃に加熱混合する。
２．水性成分を５０℃に加熱混合して溶解した。
３．前記１．を９０℃で撹拌下に前記２．を徐添して乳化し、冷却してＷ／Ｏ型日焼け止め化粧料を得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較して滑らかできしみ感が無く化粧膜の均一性に優れている。 [Example 12 and Comparative Examples 15 to 17] Liquid foundation

(Production method)
1. 1. The oily component is heated and mixed at 90 ° C.
2. 2. The aqueous component was heated and mixed at 50 ° C. to dissolve.
3. 3. The above 1. The above 2. Was gradually added and emulsified, and cooled to obtain a W / O type sunscreen cosmetic.
The cosmetic containing the surface-treated powder of the present invention is smoother and has no stain feeling as compared with the cosmetics of the comparative examples, and is excellent in the uniformity of the cosmetic film.

（製造方法）
１．油性成分を５０℃に加熱混合する。
２．水性成分を５０℃に加熱混合して溶解した。
３．攪拌下、前記１．に前記２．を徐添して乳化し、冷却してＷ／Ｏ型乳化日焼け止め化粧料を得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較して滑らかできしみ感が無く化粧膜の均一性に優れている。 [Example 13 and Comparative Example 18] W / O type sunscreen

(Production method)
1. 1. The oily component is heated and mixed at 50 ° C.
2. 2. The aqueous component was heated and mixed at 50 ° C. to dissolve.
3. 3. Under stirring, the above 1. In addition to the above 2. Was gradually added and emulsified, and cooled to obtain a W / O type emulsified sunscreen cosmetic.
The cosmetic containing the surface-treated powder of the present invention is smoother and has no stain feeling as compared with the cosmetics of the comparative examples, and is excellent in the uniformity of the cosmetic film.

（製造方法）
１．粉体成分を均一に混合する。
２．上記１．に油性成分を添加して混合・粉砕してフルイを通す。
３．上記２．をアルミ皿に採り成型してアイシャドウを得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較して滑らかできしみ感が無く化粧膜の均一性に優れている。 [Example 14 and Comparative Example 19] Eye shadow

(Production method)
1. 1. Mix the powder components evenly.
2. 2. Above 1. Add oily ingredients to the mixture, mix and crush, and pass through the fluid.
3. 3. Above 2. Was taken on an aluminum plate and molded to obtain an eye shadow.
The cosmetic containing the surface-treated powder of the present invention is smoother and has no stain feeling as compared with the cosmetics of the comparative examples, and is excellent in the uniformity of the cosmetic film.

（製造方法）
１．油性成分を混合・分散する。
２．水性成分を混合する。
３．前記２．に前記１．を徐添して乳化して制汗剤を得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較してのびが軽く、清涼感がありさっぱりとして、べたつきや油感のないものであった。 [Example 15 and Comparative Example 20] Antiperspirant

(Production method)
1. 1. Mix and disperse oily ingredients.
2. 2. Mix the aqueous components.
3. 3. 2. In addition to the above 1. Was slowly added and emulsified to obtain an antiperspirant.
The cosmetic containing the surface-treated powder of the present invention was lighter in spread than the cosmetics of the comparative examples, had a refreshing sensation, was refreshing, and was not sticky or oily.

（製造方法）
１．油性成分を７０℃に加熱混合・分散する。
２．水性成分を７０℃に加熱混合して溶解した。
３．攪拌下、前記１．に前記２．を徐添して乳化し、冷却して化粧水を得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較してのび広がりが軽くきしみ感がなく、べたつきがなくしっとりとしてみずみずしいものであった。 [Example 16 and Comparative Example 21] Toner

(Production method)
1. 1. The oily component is heated, mixed and dispersed at 70 ° C.
2. 2. The aqueous component was heated and mixed at 70 ° C. to dissolve.
3. 3. Under stirring, the above 1. In addition to the above 2. Was gradually added and emulsified, and cooled to obtain a lotion.
The cosmetic containing the surface-treated powder of the present invention had a lighter spread, no squeaky feeling, no stickiness, and was moist and fresh as compared with the cosmetics of the comparative examples.

（製造方法）
１．水性成分を７０℃に加熱混合する。
２．油性成分を混合する。
３．攪拌下、前記１．に前記２．を徐添して乳化してリンスインシャンプーを得た。
本発明の表面処理粉体を配合した化粧料は比較例の化粧料に比較して、使用時にべたつきや重さがなく、さらさら感、なめらかさ、及びボリューム感を付与するものであった。また、櫛通りの良い、使用性及び持続性に優れたものであった。

[Example 17 and Comparative Example 22] Rinse-in shampoo

(Production method)
1. 1. The aqueous component is heated and mixed at 70 ° C.
2. 2. Mix oily ingredients.
3. 3. Under stirring, the above 1. In addition to the above 2. Was gradually added and emulsified to obtain a rinse-in shampoo.
The cosmetic containing the surface-treated powder of the present invention is less sticky or heavy when used, and imparts a smoothness, smoothness, and volume as compared with the cosmetics of the comparative examples. In addition, it was easy to comb and had excellent usability and durability.

Claims (9)

Inorganic powder with a refractive index of 2.0 or more and an average particle size of 0.01 to 3.0 μm is a component (1) Methylhydrogenpolykiloxane of the following components [Chemical Formula 1-1] and (2) The following. A surface-treated inorganic powder coated with the surface-treating agent of the component [Chemical Formula 2] and having a dynamic friction coefficient of less than 0.5.

(M is 3 to 100, n is 0 to 100, and m + n = 20 to 200.)

(R ³ is an ethoxy group and R ⁴ is an aminopropyl group.)
The compounding ratio of the sum of the inorganic powder to be surface-treated and the components ( 1-1 ) and (2) which are surface-treating agents is powder / surface-treating agent = 94/6 to 70/30 (% by weight). The surface-treated inorganic powder according to claim 1.
Claim 1 or 2 in which the compounding ratio of the component (1-1) and the component (2), which are the surface treatment agents, is component ( 1 ) / component (2) = 85/15 to 40/60 (% by weight). The surface-treated inorganic powder described.
The surface-treated inorganic powder according to any one of claims 1 to 3, wherein the inorganic powder is a metal oxide selected from the group consisting of titanium oxide, zinc oxide, iron oxide, and cerium oxide.
Inorganic powder with a refractive index of 2.0 or more and an average particle size of 0.01 to 3.0 μm is mixed with the methylhydrogenpolykiloxane of the following component [Chemical formula 1-1] and (2) the following component [Chemical formula 2 ]. ] , Which is a method for producing a surface-treated inorganic powder which is dried and pulverized by contacting with], and which has a dynamic friction coefficient of less than 0.5.

(M is 3 to 100, n is 0 to 100, and m + n = 20 to 200.)

(R ³ is an ethoxy group and R ⁴ is an aminopropyl group.)
The compounding ratio of the sum of the inorganic powder to be surface -treated and the components (1-1 ) and (2) which are surface-treating agents is inorganic powder / surface-treating agent = 94/6 to 70/30 (% by weight). , The method for producing a surface-treated inorganic powder according to claim 5.
5. Claim 5 that the compounding ratio of the component ( 1-1 ) and the component (2) which are the surface treatment agents is the component ( 1-1 ) / component (2) = 85/15 to 40/60 (% by weight). Alternatively, the method for producing a surface-treated inorganic powder according to 6.
The method for producing a surface-treated inorganic powder according to any one of claims 5 to 7, wherein the inorganic powder is a metal oxide selected from the group consisting of titanium oxide, zinc oxide, iron oxide, and cerium oxide.
A cosmetic containing 0.1 to 99% by weight of the surface-treated inorganic powder according to any one of claims 1 to 4 with respect to the total amount.