JPH05287214A - Modified powder and cosmetic containing the same - Google Patents

Abstract

PURPOSE:To provide a powder scarcely contg. secondary agglomerates, having a stable quality and an excellent touch and suitable for cosmetics by mixing a powder with a specific methylhydrogenpolysiloxane and a specific cyclic methylhydrogenpolysiloxane in a specified wt. ratio and thermally treating the mixture under specified conditions. CONSTITUTION:100 pts.wt. powder, 1-15 pts.wt. compd. of formula I and 1-10 pts.wt. compd. of formula II are mixed, thermally treated at 60-130 deg.C for 0.5-5hr, and thermally treated further at a temp. higher than that in the first thermal tretment and at 110-200 deg.C for 1-8hr. Examples of the powder are an org. pigment, a white pigment, a body pigment, a metal salt, a polymer powder, an inorg. powder, and a lake pigment.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a modified powder having a small amount of secondary aggregation, excellent water repellency and excellent ability to block catalytic activity, and a cosmetic having excellent quality stability and feel.

[0002]

2. Description of the Related Art Conventionally, the problems to be solved by the invention
When coating powders with methylhydrogenpolysiloxane, treatment methods such as a dry treatment method, a wet treatment method, a vapor phase treatment method and a mechanochemical method have been studied. However, little research has been conducted on film-forming properties, easiness of polymerization, changes in the agglomeration of powders, etc. due to the structure of the treatment agent, methylhydrogenpolysiloxane.

Conventionally used methyl hydrogen polysiloxanes are, for example, KF-99 (manufactured by Shin-Etsu Chemical Co., Ltd.), SH1107 (manufactured by Toray Dow Corning Silicone Co., Ltd.), TSF484 (Toshiba Silicone ( Co., Ltd.) and the like. These structures are shown in Chemical formula 5.

[Chemical 5] (However, k = 30-40)

Since methyl hydrogen polysiloxane having such a skeleton has a large proportion of molecules having a high degree of polymerization, steric hindrance is apt to occur when it is heated and polymerized, and the reaction is difficult to proceed.

Further, since the main skeleton is composed of methyl hydrogen siloxane, the degree of freedom of the main chain decreases with the polymerization, and the resulting film is brittle and has the property of being easily cracked. Therefore, the modified powder obtained by coating powders with these methyl hydrogen polysiloxanes and polymerizing them has a high rate of film destruction when a pulverizer such as an atomizer is used. And problems such as deterioration of dispersion and deterioration of dispersibility may occur.

On the other hand, in the methylhydrogenpolysiloxane of the type having a dimethylsiloxane unit as shown in Chemical formula 6, since the dimethyl unit has no reactivity, the degree of freedom of the main chain is increased, and the obtained film has the above-mentioned structure. It is more flexible and less prone to cracking than a film of methyl hydrogen polysiloxane.

[Chemical 6] (However, a and b are arbitrary numerical values.)

However, as a result of the decrease in the proportion of methylhydrogensiloxane units, it becomes difficult to proceed with the polymerization, and stronger reaction conditions are required as compared with methylhydrogenpolysiloxane having no dimethylsiloxane units.

Further, since the cyclic methylhydrogenpolysiloxane having the structure shown in Chemical formula 7 has a low boiling point, a modified powder having good performance can be obtained by a method using a closed container such as a gas phase method. However, when using an open system heating device,
Even if the powders were treated with only the cyclic methyl hydrogen polysiloxane, a modified powder having sufficient properties such as water repellency and film strength could not be obtained.

[Chemical 7]

In view of the above problems, the inventors of the present invention have conducted extensive studies and as a result, combined methylhydrogenpolysiloxane and cyclic methylhydrogenpolysiloxane having a specific degree of polymerization and a specific proportion of dimethylsiloxane units. It has been found that the reaction conditions can be relaxed and the performance of the polymer film can be improved by further improving the heating conditions and the use.

Further, when fine particle titanium oxide having a property of easily aggregating is coated and heat-treated by using the methylhydrogenpolysiloxane and the method specified in the present invention, the degree of secondary aggregation of fine particle titanium oxide by the treatment is determined. I found what I could do less.

That is, the object of the present invention is to provide a modified powder which is more mild in reaction conditions, has less secondary aggregation, and is excellent in water repellency and catalytic activity blocking ability, and this modified powder. By blending the body, it is to provide a cosmetic having excellent quality stability and feel.

Among conventional commercially available silicones, KF-9
901 (manufactured by Shin-Etsu Chemical Co., Ltd.) contains a small amount of silicone having the structure defined in the present invention, but its main component has the skeleton shown in Chemical formula 8 and thus has poor reactivity. I know.

[Chemical 8] (However, m + n = 20-30, m = 10-15)

Since silicone is a polymer, it has a molecular weight distribution. The methylhydrogenpolysiloxane having a specific structure referred to in the present invention defines the molecular structure that forms the center of the molecular weight distribution.

[0014]

Means for Solving the Problems In the present invention, after mixing powders, methylhydrogenpolysiloxane having a specific structure and cyclic methylhydrogenpolysiloxane described below, primary heat treatment is performed at 60 to 130 ° C. A modified powder, which is obtained by performing a secondary heat treatment for 1 to 8 hours at a temperature of 110 to 200 ° C., which is performed for 0.5 to 5 hours, and subsequently at a temperature higher than that of the primary heat treatment. And a cosmetic containing the modified powder.

The details of the configuration of the present invention will be described below. The powders used in the present invention include, for example, yellow iron oxide, red iron oxide, black iron oxide, chromium oxide, carbon black,
Colored pigments such as ultramarine blue, white pigments such as zinc oxide, titanium oxide, cerium oxide and zirconium oxide, talc, mica,
Extender pigments such as sericite, kaolin, mica, montmorillonite, pearl pigments such as titanium mica, barium sulfate, calcium carbonate, magnesium carbonate, aluminum silicate,
Metal salts such as magnesium silicate, organic substance-coated pigments such as mica coated with N-acyl aspartic acid and pigments treated with metal soap, nylon powder, silk powder, urethane powder, Teflon powder, cellulose powder, silicone powder, gold-dyed silk powder, polyethylene powder Polymer powders such as silica, inorganic powders such as silica and alumina, dyes such as blue No. 404, lake pigments such as red No. 2 Al lake, and fine particle titanium oxide, fine particle zinc oxide, alumina-coated fine particle titanium oxide, Examples of the silica-coated fine particles include fine particles of titanium oxide and the like, bentonite, and the like. Especially for fine titanium oxide particles, the primary particle size is 7
And a crystal form of rutile type, anatase type, or amorphous type.

The methylhydrogenpolysiloxane used in the present invention may be used alone or in combination of two or more selected from those having a structure represented by the following general formula 9.

[Chemical 9] (However, m and n are average numbers, and m + n = 7 to 25,
m: n = 1: 2 to 1: 4) Hereinafter, the methylhydrogenpolysiloxane having this structure will be referred to as a treating agent A.

The cyclic methyl hydrogen polysiloxane used in the present invention has a structure represented by the following chemical formula 10.

[Chemical 10] Hereinafter, the cyclic methyl hydrogen polysiloxane having this structure will be referred to as a treating agent B.

In the present invention, the coating ratio of the treating agent A and the treating agent B on the powders is 1 to 15 parts by weight of the treating agent A and 1 to 10 parts by weight of the treating agent B to 100 parts by weight of the powders. Parts by weight, more preferably 2 to 10 parts by weight of treating agent A and 1.5 to 6 parts by weight of treating agent B. The mixing ratio of the treating agent A and the treating agent B is arbitrary, but it is preferable that the treating agent B is 1/2 amount or less of the weight of the treating agent A.

The condition for heating the mixture of the powders and the treating agents A and B is 60 to 130.degree.
It is carried out for 5 hours, and subsequently, the secondary heat treatment is carried out at a temperature higher than that of the primary heat treatment and at 110 to 200 ° C. for 1 to 8 hours. Further, the time of the primary heat treatment is preferably 1 hour or more because there are many low boiling point components.

The coating method of the treating agent used in the present invention includes (1) a method of stirring and mixing powders and treating agent without using a solvent. (2) A method in which a treatment agent dissolved in a small amount of solvent is stirred and mixed with powders. (3) A method of forming a slurry of a powder obtained by dissolving a treating agent in a large amount of a solvent, and then distilling the solvent off. (4) A method of coating powders with a treating agent using a spray dryer or an air blender. Etc. However, if a solvent is used in the step of coating the treatment agent on the powders,
Care must be taken as aggregation often occurs.

Further, when the treating agents A and B are introduced, it is preferable to make the droplets of the treating agent as small as possible by using an air brush or the like. Further, when handling the fine particle powder, agglomeration easily occurs, so that the plate-like powder such as sericite or talc should be added to the plate-like powder 10 to 100 parts by weight of the fine particle powder.
Mixing at a ratio of 60 parts is effective for preventing aggregation.

The modified powder of the present invention can be used as cosmetics, resins, paints, and UV protectants. In particular, examples of cosmetics include white powder, foundation, pressed powder, water foundation, oil foundation, emulsification foundation, lipstick, blusher, eye shadow, eyebrow, eyeliner, mascara, nail color, cheek color, base foundation, sunscreen. Agents and the like.

As the cosmetics, as long as the object of the present invention is achieved, oils, powders, etc. usually used in cosmetics,
Solvents, surfactants, ultraviolet absorbers, preservatives, bactericides, preservatives, antioxidants, hormones, vitamins, moisturizers, fragrances and the like can be added at the same time.

Examples of the oil agent in this case include higher fatty acids, higher alcohols, synthetic esters, waxes, vegetable fats and oils, animal fats and oils, hydrocarbons, fluorocarbons, perfluoropolyethers, fluoroalkoxyphosphazenes and the like. Examples of the silicone oil include dimethylpolysiloxane, methylphenylpolysiloxane, polyether-modified silicone, fluorine-modified silicone, methylcetyl-modified silicone, amino-modified silicone and cyclic dimethylpolysiloxane. Examples of the powders include powders, resins, fibers and the like which are usually used in cosmetics. These powders may or may not be subjected to surface treatment such as coupling agent treatment, silicone treatment, fluorine treatment, metal soap treatment, silica treatment, alumina treatment, amino acid treatment, metal coating treatment and plasma treatment. . As the solvent, cyclic silicone and the like can be used in addition to the solvents such as water, alcohol and propylene glycol which are usually used in cosmetics. Examples of the surfactant include anionic surfactants, cationic surfactants, amphoteric surfactants, nonionic surfactants and the like.

[0025]

EXAMPLES The present invention will be described in detail below with reference to examples and comparative examples. The evaluation methods of secondary aggregation, water repellency, blocked state of catalytic activity, and feel of cosmetics described in Examples are as follows. 1. Evaluation method of secondary aggregation of powders (1-1) Evaluation method for powders having an average particle diameter of 0.1 μm or more Particle size distribution meter (PRO-7000, PRO
-9000 (manufactured by Seishin Enterprise Co., Ltd.), ethanol was used as a dispersion solvent, and the volume average particle size of the powders in an ultrasonically dispersed state was measured. Let D be the average particle size of the powders in the untreated state and D1 be the average particle size of the treated powder.
Table 13 shows the results of evaluation based on the criteria shown in Table 1 by the cube value of D).

[0026]

[Table 1]

(1-2) Evaluation method for powders having an average particle diameter of 0.1 μm or less: To 50 g of dimethylpolysiloxane (30000 cs), 150 mg of fine particle powder was added and well stirred,
Dispersion was performed using a roller. The thickness of this sample was set to 40 μm, and the spectral distribution at a wavelength of 700 to 190 nm was measured using a spectrophotometer (MPS-2000 type, manufactured by Shimadzu Corporation). When the wavelength at which the absorbance of the untreated fine particle powder is maximum is A and the wavelength at which the absorbance of the treated powder is maximum is B, the value of B-A is C, and the value of C is shown in Table 2. The evaluation was performed based on the standard. The results are shown in Table 12.

[0028]

[Table 2]

2. Evaluation method of water repellency 30 mg of the treated powder is weighed and put in a test tube containing 10 mL of an aqueous ethanol solution prepared to have a concentration of 0 to 100 vol%, and then an ultrasonic cleaner (BRANSON2200).
Type BRANSON CLEANING EQUIPM
Ultrasonic waves were radiated for 1 minute using ENT COMPANY. After ultrasonic irradiation, the concentration of ethanol at which the treated powder started to disperse in the aqueous ethanol solution was measured. Table 12 and Table 13 show the results of evaluation based on the criteria shown in Table 3, where E is the concentration of ethanol at which dispersion starts. Incidentally, E
The higher the value of, the better the water repellency.

[0030]

[Table 3]

3. Evaluation method of catalytic activity blocked state It is known that fine particle powder having a primary particle diameter of 0.1 μm or less has a strong catalytic activity. In particular, titanium oxide has a strong photocatalytic activity although it has an anatase-type or amorphous-type structure, and causes discoloration of titanium oxide due to the transition to low-order titanium oxide and deterioration of perfume in cosmetics. In this evaluation method, the blocked state of catalytic activity was tested from the discolored state of titanium oxide when exposed to light in the presence of water. Sample 0.3g
Was dispersed in 1 g of ethanol, 10 g of a glycerin solution containing 10 wt% of water was added, and the mixture was stirred and transferred to a transparent glass container. The transparent glass container was placed under sunlight to examine the state of discoloration after 1 week. Table 12 shows the results of evaluation based on the criteria shown in Table 4. It should be noted that the more the discoloration occurs, the worse the blocked state of the catalytic activity is.

[0032]

[Table 4]

4. Evaluation Method of Feeling of Cosmetics Using the cosmetics prepared in Examples and Comparative Examples of each cosmetic, the feeling was evaluated for 10 men and women aged 22 to 38 years. The results are shown in Table 14. In Table 14, the numerical values show how many people out of 10 judged each evaluation item, and if 10 means all 10 people, and if 1 means 1 out of 10 people.

Examples of the modified powder will be shown in Examples 1 to 11 below. Example 1 100 g of fine particle titanium oxide (primary particle size 35 nm, anatase type) was coated with a mixed solution of 10 g of a treating agent having the structure shown in Chemical formula 11 and 6 g of a treating agent B using an air blender (air temperature 50 ° C.). 60 ° C using a blast dryer
To 100 ° C., primary heat treatment was performed at a rate of 0.4 ° C./min (total 100 minutes), and subsequently, the temperature was raised to 150 ° C., and then heat treatment was performed for 3 hours.

Comparative Example 1 A solution prepared by dissolving 16 g of a treating agent having the structure shown in Chemical formula 11 in 100 g of fine particle titanium oxide (primary particle size 35 nm, anatase type) in 20 g of 1,1,1-trichloroethane was mixed with an air blender (air temperature: 30). C.) to obtain a coated powder. The obtained powder was mixed with a blow dryer 6
From 0 ℃ to 100 ℃, a speed of 0.4 ℃ per minute (total 100
The heat treatment was performed for 3 hours after the temperature was raised to 150 ° C.

[Chemical 11] (However, the average values of m and n are m = 4 and n = 16.)

Example 2 A treating agent 120 having the structure shown in Chemical formula 12 in 1000 g of fine particle titanium oxide (primary particle diameter 15 nm, amorphous type)
g and a treating solution B (10 g) were added using an air blender (air temperature 60 ° C.). Using a blast dryer, 60 ° C to 110 ° C at a rate of 0.4 ° C / min (total 12
Primary heat treatment was performed for 5 minutes, followed by heating to 160 ° C. and then heat treatment for 2 hours.

[Chemical 12] (However, the average values of m and n are m = 7 and n = 14)

Comparative Example 2 100 g of fine particle titanium oxide (primary particle size 15 nm, amorphous type), 10 g of a treating agent having the structure shown in Chemical formula 13 and 180 g of 1,1,1-trichloroethane were added, and the mixture was stirred and mixed using a mixer. After that, the solvent was distilled off, and then heat treatment was performed at 180 ° C. for 6 hours.

[Chemical 13] (However, the average values of m and n are m = 15 and n = 15)

Example 3 Fine particle titanium oxide (primary particle size 50 nm, rutile type) 5
75 g of sericite, 29 g of treating agent having the structure shown in Chemical formula 14 and 11 g of treating agent B were added to 00 g, and the mixture was stirred and mixed using a mixer. 4 at 85 ° C using blast dryer
After the primary heat treatment for 1 hour, the temperature was raised to 145 ° C., and then the heat treatment was performed for 4 hours.

Comparative Example 3 Fine particle titanium oxide (primary particle diameter 50 nm, rutile type) 5
25 g of the treating agent having the structure shown in Chemical formula 14
A solution dissolved in 60 g of 1,1-trichloroethane was added using an air blender (air temperature 25 ° C). The obtained powder was heat-treated at 145 ° C. for 4 hours using a blow dryer.

[Chemical 14] (However, the average value of m and n is m = 5, n = 15)

Example 4 Treatment agent 25 having 1 kg of sericite and the structure shown in Chemical formula 15
g and treating agent B10 g were mixed and stirred using a Henschel mixer. Then, using a dryer, 1 at 70 ℃
After heat treatment for 2 hours, heat treatment was performed at 180 ° C. for 2 hours.

Comparative Example 4 Treatment agent 25 having 1 kg of sericite and the structure shown in Chemical formula 15
g, 10 g of the treating agent B and 70 g of 1,1,1-trichloroethane were mixed and stirred. Then, using a dryer,
After heat treatment at 0 ° C. for 1 hour, heat treatment was performed at 180 ° C. for 2 hours.

[Chemical 15] (However, the average values of m and n are m = 3 and n = 12)

Example 5 After mixing 100 g of yellow iron oxide (primary particle diameter 0.7 μm) and 25 g of sericite, 3.9 g of the treating agent having the structure shown in Chemical formula 16 and 1.5 g of the treating agent B were sprayed. Mixed. Then, using a blast dryer, primary heat treatment was performed from 60 ° C. to 90 ° C. at a rate of 0.4 ° C. per minute (75 minutes in total), followed by heating to 120 ° C. and then heat treatment for 3 hours. ..

Comparative Example 5 100 g of yellow iron oxide (primary particle size 0.7 μm) and 25 g of sericite were mixed, and then 3.9 g of the treating agent having the structure shown in Chemical formula 16 was mixed using a spray. Then, heat treatment was carried out at 120 ° C. for 3 hours using a blow dryer.

[Chemical 16] (However, the average values of m and n are m = 2 and n = 6)

Example 6 900 g of titanium oxide (primary particle size: 0.6 μm) was mixed with 100 g of sericite, 30 g of a treating agent having the structure shown in Chemical formula 17 and 30 g of a treating agent B were added using an air spray, and a mixer was used. Stir and mix using. After heating from 60 ° C to 130 ° C at a rate of 0.3 ° C / min (total of 233 minutes) using a blower dryer, primary heat treatment was further performed at 130 ° C for 1 hour, and then the temperature was raised to 150 ° C. rear,
Heat treatment was performed for 8 hours.

Comparative Example 6 900 g of titanium oxide (primary particle size: 0.6 μm) was mixed with 100 g of sericite, and then 30 g of the treating agent having the structure shown in Chemical formula 17 was dissolved in 200 g of treating agent B, and a mixer was used. Stir and mix. Then, heat treatment was performed at 150 ° C. for 8 hours using a blow dryer.

[Chemical 17] (However, the average values of m and n are m = 7 and n = 14)

Example 7 An experiment was conducted using the same conditions as in Example 4 except that the sericite of Example 4 was replaced with talc. The obtained powder was rich in water repellency.

Example 8 Example 4 was repeated except that kaolin was used instead of sericite in Example 4.
Experiments were performed using the same conditions as. The obtained powder was rich in water repellency.

Example 9 An experiment was conducted under the same conditions as in Example 4 except that the mica titanium was used in place of the sericite of Example 4. The obtained powder was rich in water repellency.

Example 10 Red iron oxide of Example 5 was replaced with red iron oxide (primary particle diameter 0.6 μm).
The experiment was conducted using the same conditions as in Example 5 except that the m) was changed. The obtained powder was rich in water repellency.

Example 11 The yellow iron oxide of Example 5 was replaced with black iron oxide (having a primary particle size of 0.6 μm).
The experiment was conducted using the same conditions as in Example 5 except that the m) was changed. The obtained powder was rich in water repellency.

Examples of cosmetics using the modified powders prepared in Examples 1 to 11 will be described below in Examples 12 to 14.

[Table 5] Ingredient A was placed in a Henschel mixer and mixed for 5 minutes, to which ingredient B, which had been uniformly mixed and dissolved in advance, was gradually added and subsequently mixed for 10 minutes. Then, this was crushed with a crusher. Then, the product was press-filled to obtain a product. The product was left in the sun for 1 week, but no discoloration or odor was observed.

[0052]

[Table 6] Ingredient A was placed in a Henschel mixer and mixed for 5 minutes, to which ingredient B, which had been uniformly mixed and dissolved in advance, was gradually added and subsequently mixed for 10 minutes. Then, this was crushed with a crusher. Then, the product was press-filled to obtain a product. This product lacked water resistance and was easily broken. In addition, when this product was left in the sun for 1 week, discoloration and odor were observed.

[0053]

[Table 7] Ingredient A was placed in a Henschel mixer and mixed for 5 minutes, to which ingredient B, which had been uniformly mixed and dissolved in advance, was gradually added and subsequently mixed for 10 minutes. Then, this was crushed with a crusher. Then, the product was press-filled to obtain a product. The color of this product was intense.

[0054]

[Table 8] Ingredient A was placed in a Henschel mixer and mixed for 5 minutes, to which ingredient B, which had been uniformly mixed and dissolved in advance, was gradually added and subsequently mixed for 10 minutes. Then, this was crushed with a crusher. Then, the product was press-filled to obtain a product.

[0055]

[Table 9] Ingredient A was placed in a Henschel mixer and mixed for 5 minutes, to which ingredient B, which had been uniformly mixed and dissolved in advance, was gradually added and subsequently mixed for 10 minutes. Then, this was crushed with a crusher. Then, the product was press-filled to obtain a product.

[0056]

[Table 10] The component A was gradually added to the component B which was uniformly mixed and dissolved, and mixed for 15 minutes using a homomixer to obtain a product.

[0057]

[Table 11] The component A was gradually added to the component B which was uniformly mixed and dissolved, and mixed for 15 minutes using a homomixer to obtain a product.

[0058]

[Table 12]

[0059]

[Table 13]

[0060]

[Table 14]

From Table 12, it was confirmed that the modified fine particle powder of the present invention had less secondary aggregation and excellent water repellency, and the catalytic activity of fine particle titanium oxide was also blocked. From Table 13, it was confirmed that the modified powder of the present invention had less secondary aggregation and was excellent in water repellency. From the results of Table 12 and Table 13, it was found that the modified powder treated by the method of the present invention showed good performance regardless of the size of the powder. Further, from the comparison between Example 1 and Comparative Example 1 and between Example 4 and Comparative Example 4, it can be seen that the presence of the solvent has an adverse effect such as secondary aggregation. Further, from the results of Table 14, it was confirmed that when the modified powder of the present invention was blended with a cosmetic, a cosmetic having an excellent feel, no roughness due to the aggregation of powders, and a good texture was obtained. .. Further, comparing the results of the light resistance of Example 12 and Comparative Example 7, it can be seen that the light resistance of Example is extremely improved.

[0062]

As described above, according to the present invention, after the powders are coated with methylhydrogenpolysiloxane having a specific structure and cyclic methylhydrogenpolysiloxane, primary heat treatment is performed at 60 to 130 ° C. For 0.5 to 5 hours, and subsequently at a higher temperature than the primary heat treatment,
Further, by carrying out the secondary heat treatment at 110 to 200 ° C. for 1 to 8 hours, there is provided a modified powder in which secondary aggregation is small, water repellency is excellent, and further catalytic activity is blocked. It is clear that the blending of the fine powder provides a cosmetic having excellent quality stability and feel.

─────────────────────────────────────────────────── ───

[Procedure amendment]

[Submission date] October 1, 1992

[Procedure Amendment 1]

[Document name to be amended] Statement

[Name of item to be corrected] Claim 1

[Correction method] Change

[Correction content]

[Chemical 1] (However, m and n are average numbers, and m + n = 7 to 25,
m: n = 1: 2 to 1: 4)

[Chemical 2]

[Procedure Amendment 2]

[Document name to be amended] Statement

[Name of item to be corrected] Claim 3

[Correction method] Change

[Correction content]

[Chemical 3] (However, m and n are average numbers, and m + n = 7 to 25,
m: n = 1: 2 to 1: 4)

[Chemical 4]

[Procedure 3]

[Document name to be amended] Statement

[Correction target item name] 0008

[Correction method] Change

[Correction content]

Further, since the cyclic methylhydrogenpolysiloxane having the structure shown in Chemical formula 7 has a low boiling point, a modified powder having good performance can be obtained by a method using a closed container such as a gas phase method. However, when using an open system heating device,
Even if the powders were treated with only the cyclic methyl hydrogen polysiloxane, a modified powder having sufficient properties such as water repellency and film strength could not be obtained.

[Chemical 7]

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0015

[Correction method] Change

[Correction content]

The details of the configuration of the present invention will be described below. The powders used in the present invention include, for example, yellow iron oxide, red iron oxide, black iron oxide, chromium oxide, carbon black,
Colored pigments such as ultramarine blue, white pigments such as zinc oxide, titanium oxide, cerium oxide and zirconium oxide, talc, mica,
Extender pigments such as sericite, kaolin, mica, montmorillonite, pearl pigments such as titanium mica, barium sulfate, calcium carbonate, magnesium carbonate, aluminum silicate,
Metal salts such as magnesium silicate, organic substance-coated pigments such as mica coated with N-acyl aspartic acid and pigments treated with metal soap, nylon powder, silk powder, urethane powder, Teflon powder, cellulose powder, silicone powder, gold-dyed silk powder, polyethylene powder Polymer powders such as silica, inorganic powders such as silica and alumina, dyes such as blue No. 404, lake pigments such as red No. 2 Al lake, and fine particle titanium oxide, fine particle zinc oxide, alumina-coated fine particle titanium oxide, Examples of the silica-coated fine particles include fine particles of titanium oxide and the like, bentonite, and the like. Especially for fine particle titanium oxide, the primary particle size is 1
A 0 up to 50 nm, the crystal form is rutile type, anatase type include those amorphous type. Furthermore
In addition, for the amorphous type, such as catalytic activity blocking treatment
It is preferable that pretreatment has been performed.

[Procedure Amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0017

[Correction method] Change

[Correction content]

The cyclic methyl hydrogen polysiloxane used in the present invention has a structure represented by the following chemical formula 10.

[Chemical 10] Hereinafter, the cyclic methyl hydrogen polysiloxane having this structure will be referred to as a treating agent B.

Claims (4)

[Claims] 1. Powders and compounds represented by the following general formulas 1 and 2 are mixed in a weight ratio of 100: 1: 1 to 100: 15: 10, and then primary heating is performed at 60 to 130 ° C. The modified powder obtained by performing the treatment for 0.5 to 5 hours, and subsequently performing the secondary heat treatment at 110 to 200 ° C. at a temperature higher than that of the primary heat treatment for 1 to 8 hours. body. [Chemical 1] (However, m and n are average numbers, and m + n = 7 to 25,
m: n = 1: 2 to 1: 4) 2. The modified powder according to claim 1, wherein the powder is fine particle titanium oxide having a primary particle diameter of 10 to 50 nm. 3. Powders and the compounds represented by the following general formulas 3 and 4 are mixed in a weight ratio of 100: 1: 1 to 100: 15: 10, and then primary heating is performed at 60 to 130 ° C. Blending the modified powder obtained by performing the treatment for 0.5 to 5 hours, and subsequently performing the secondary heat treatment at 110 to 200 ° C. for 1 to 8 hours at a higher temperature than the primary heat treatment. Cosmetics characterized by: [Chemical 3] (However, m and n are average numbers, and m + n = 7 to 25,
m: n = 1: 2 to 1: 4) 4. The cosmetic according to claim 3, wherein the powder is fine particle titanium oxide having a primary particle diameter of 10 to 50 nm.