JPH0632991A - Modified powder, and cosmetic containing the same - Google Patents

Abstract

PURPOSE:To obtain a modified powder excellent in water repellency and suitably controlled in secondary agglomeration under mild reaction conditions by mixing a powder, a methylhydrogenpolysiloxane, and a cyclic methylhydrogenpoly siloxane and thermally treating the resulting mixture. CONSTITUTION:A powder, a methylhydrogenpolysiloxane of formula I (wherein k is the mean number and is 7-30), and a cyclic methylhydrogenpolysiloxane of formula II are mixed and thermally treated at 80-200 deg.C for 0.5-5hr to give a modified powder. The modified powder is incorporated into a cosmetic to give it stable qualities and excellent feel. Examples of the cosmetic which can be thus improved are a face powder, a foundation, a breast powder, a water- base foundation, an oily foundation, an emulsified foundation, a lipstick, etc.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION The present invention relates to a mixture of powders and methylhydrogenpolysiloxane having a specific average degree of polymerization and cyclic methylhydrogenpolysiloxane,
The present invention relates to a modified powder obtained by heat treatment and a cosmetic material containing the powder. More specifically, the present invention relates to a modified powder having less secondary aggregation, excellent water repellency and catalytic activity blocking ability, and a cosmetic having excellent quality stability and a moist feel.

[0002]

2. Description of the Related Art Conventionally, the problems to be solved by the invention
When the powders are coated with methylhydrogenpolysiloxane, the structures of methylhydrogenpolysiloxane used are those having the structures shown in Chemical formulas 3 and 4. After methylhydrogenpolysiloxane is coated on the pigment surface, by heat treatment, 2Si-H + 1 / 2O 2 = Si-O-Si +
A reaction such as H ₂ occurs to polymerize and form a film on the pigment surface.

[0003]

[Chemical 3] (However, a = 30 to 50)

[0004]

[Chemical 4] (However, m = n, m + n = 30 to 50)

In the conventional methyl hydrogen polysiloxane, in order to sufficiently carry out this polymerization reaction, 170
It was necessary to react at high temperature for a long time, such as heating at ℃ for 5 hours. However, depending on the pigment, quality deterioration such as deterioration and discoloration occurs under these heating conditions, so that it is necessary to lower the reaction temperature and there is a problem that the polymerization reaction becomes incomplete.

Then, the inventors analyzed the factors affecting the polymerization of methylhydrogenpolysiloxane, and found that
(1) reaction conditions (reaction temperature, time), (2) average degree of polymerization and structure of methylhydrogenpolysiloxane,
(3) It was found that the main factor is the catalytic activity of the pigment itself.

As a result of earnest research on the relationship between the reaction conditions of (1) and the average degree of polymerization and structure of (2) methylhydrogenpolysiloxane, the one having the structure shown in Chemical formula 5 has the highest reactivity. I found out that

[0008]

[Chemical 5] (However, k is an average number, and k = 7 to 30)

[0009] Then, by performing a coating treatment using the methylhydrogenpolysiloxane specified in the present invention by a dry method without using a solvent, the agglomeration of the powder can be minimized under lower reaction conditions. It succeeded in carrying out reforming.

Here, JP-A-59-76009 describes the use of methylhydrogenpolysiloxane having a degree of polymerization of 40 or less, and JP-A-59-14.
Although Japanese Patent No. 4709 describes the use of methylhydrogenpolysiloxane having a degree of polymerization of 3 to 500, there is no description about the properties recognized in the present invention, and only a general expression is given.

On the other hand, the modified powder prepared by a dry method without using a solvent has a characteristic of less agglomeration, and when blended into a makeup cosmetic, a dry feel is obtained. On the other hand, the modified powder created by the wet method using a solvent is
It has a moist feel. As a result of intensive research using the former method for the purpose of obtaining a moist feel, it was found that a moist feel can be obtained by forming loose aggregates. Furthermore, as a method of forming loose aggregates, it was found that a method of blending the cyclic methyl hydrogen polysiloxane shown in Chemical formula 6 and controlling the vaporization rate using specific heating conditions is preferable.

[0012]

[Chemical 6]

Conventionally, as described in JP-A-59-76009 and JP-A-55-136213, by treating a methylhydrogenpolysiloxane and a silicone oil or an oil agent into powder at the same time, a characteristic touch is obtained. It is known that a modified powder having However, these inventions control the composition and structure of the silicone film, and are not intended to control the aggregation of powder. Further, Japanese Patent Application Laid-Open No. 63-113082 discloses a method of treating powder using the cyclic methylhydrogenpolysiloxane shown in Chemical formula 6, but this method is a gas phase which minimizes agglomeration. The present invention relates to a method and is different from the method for controlling the feeling by generating loose agglomerates according to the present invention.

That is, the object of the present invention is to obtain a modified powder excellent in water repellency, in which secondary agglomeration is appropriately controlled, under milder reaction conditions, and to compound this modified powder. It is to provide cosmetics with excellent quality stability and feel.

[0015]

The present invention is a modified powder obtained by mixing powders with methylhydrogenpolysiloxane and cyclic methylhydrogenpolysiloxane and then surface-treating the mixture under the specific heating conditions described below. And cosmetics containing the same.

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,
Color 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 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, fine particle iron oxide, fine particle low Examples thereof include fine particles of titanium oxide, alumina-coated fine particles of titanium oxide, silica-coated fine particles of titanium oxide and the like, bentonite, amino acid-based organic pigments and the like. Particularly, the fine particle titanium oxide may have a primary particle size of 5 to 50 nm and a crystal form of rutile type, anatase type, or amorphous type. Further, the amorphous type may or may not be subjected to treatments such as removal of impurities and reduction of catalytic activity.

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

[0018]

[Chemical 7] (However, k is an average number and k = 7 to 30) 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 is represented by the following general chemical formula.

[0020]

[Chemical 8] Hereinafter, the cyclic methyl hydrogen polysiloxane having this structure will be referred to as a treating agent B. Examples of the treating agent B include KF-9902 (produced by Shin-Etsu Chemical Co., Ltd.).

In the present invention, the ratio of coating of the treating agent A and the treating agent B on the powder is 100 parts by weight of the powder.
Treatment agent A is 0.5 to 20 parts by weight, treatment agent B is 0.3 to 5
Parts by weight, more preferably 1 to 12 parts by weight of treating agent A and 0.5 to 2 parts by weight of treating agent B.

The condition for heating the mixture of the powders and the treating agent A and the treating agent B is such that the heat treatment at 80 to 200 ° C. is 0.5.
~ 5 hours heat treatment method or 60 ~ 120 ℃
The primary heat treatment is performed for 0.5 to 4 hours, and then the secondary heat treatment is performed at a temperature higher than that of the primary heat treatment at 80 to 200 ° C. for 0.2 to 3 hours. If the heating conditions are constant within this temperature range,
It may change over time.

The coating method of the treating agent used in the present invention includes (1) a method of stirring and mixing powders and a treating agent without using a solvent. (2) A method in which a treatment agent dissolved in a small amount of a 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 treatment agent using a spray dryer or an air blender. Etc. However, the method (2) is not preferable because hard agglomerates are generated and the feel of the powder is deteriorated, and the method (3) has a large proportion of the treatment agent B being removed when the solvent is distilled off.

Further, when the treating agents A and B are charged, it is preferable to make the droplets of the treating agent as small as possible by using an air brush or the like. Also, when handling fine particle powder, hard agglomerates are likely to occur, so plate-like powder such as sericite or talc is mixed at a ratio of 10 to 60 parts of plate-like powder to 100 parts by weight of fine particle powder. It is effective in preventing the formation of hard agglomerates.

Examples of the cosmetics of the present invention include white powder, foundation, pressed powder, water-based foundation, oil-based foundation, emulsified foundation,
A dual-purpose foundation, lipstick, blusher, eye shadow, eyebrow, eyeliner, mascara, nail color, cheek color, base foundation, sunscreen agent, emulsion, lotion, preshave lotion and the like can be mentioned.

As the cosmetics, as long as the object of the present invention is achieved, oils, powders, etc. which are 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.

[0028]

EXAMPLES The present invention will be described in detail below with reference to examples and comparative examples. The method for evaluating the polymerizability of the methylhydrogenpolysiloxane used in the examples is as follows. 1. Method for Evaluating Polymerizability of Methyl Hydrogen Polysiloxane 7 g of methyl hydrogen polysiloxane having each average degree of polymerization was put in a glass petri dish having a diameter of 9 cm.
The film is placed in a blast dryer set at 0 to 180 ° C. for 1 to 8 hours, and the state of the formed film is observed. Then, the minimum heating condition for forming a film was examined. The results are shown in Table 5.

Since the present test method does not consider the catalytic activity of the powder, the heating conditions for actually coating the powder with methylhydrogenpolysiloxane and heating are as follows:
It should be noted that it is often looser than the minimum heating conditions obtained in this test.

The evaluation methods for secondary aggregation, water repellency, and catalytically active blocked state described in the examples are as follows. 2. Evaluation method of secondary aggregation of powders 2-1 Evaluation method for powders having an average particle size of 0.1 μm or more Particle size distribution meter (PRO-7000, PRO-9000
Using Seishin Enterprise Co., Ltd., ethanol was used as a dispersion solvent, and the volume average particle diameter of the powders in an ultrasonically dispersed state was measured. The average particle diameter of the powders in the untreated state is D, the average particle diameter of the treated powder is D1, and the result of evaluation based on the criteria shown in Table 1 by the cube value of (D1 / D) Is shown in Table 13.

[0031]

[Table 1]

2-2 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). 300n of untreated fine powder
When the transmittance (%) at m is A and the transmittance (%) at 300 nm of the treated powder is B, the value of B-A is C.
And the value of C was evaluated based on the criteria shown in Table 2. The results are shown in Table 12.

[0033]

[Table 2]

3. Evaluation method of water repellency After weighing 30 mg of the treated powder and placing it in a test tube containing 10 mL of an aqueous ethanol solution prepared to have a concentration of 0 to 100 vol%, an ultrasonic cleaner (BRANSON2200) was used.
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.

[0035]

[Table 3]

4. Evaluation method of catalytic activity blocking 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 even though 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 0.03
g in 1 g of ethanol and then water content (10 wt%)
10 g of glycerin was added, stirred and transferred to a synthetic quartz cell. Then a black light with a wavelength of 254 nm (4 W tube)
Was used to measure the discoloration of the solution when it was irradiated with ultraviolet rays from a distance of 1 cm for 30 minutes. 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.

[0037]

[Table 4]

The evaluation method of the feel of the cosmetics described in the examples is as follows. 5. Evaluation Method of Feeling of Cosmetics Using the cosmetics prepared in Examples and Comparative Examples of each cosmetic, the feeling was evaluated for a total of 10 men and women aged 22 to 36. The results are shown in Table 14. In Table 14, the numerical values show how many people out of 10 judged for each evaluation item, and if 10 means all 10 people, and if 1 means 1 out of 10 people.

The characteristics of methylhydrogenpolysiloxane will be described below by evaluating the polymerizability of methylhydrogenpolysiloxane. Table 5 shows the relationship between the average degree of polymerization, the structure, and the minimum heating condition, which were examined according to the evaluation method.

[0040]

[Table 5]

[0041]

[Chemical 9] (However, m = n, m + n = 30 to 50)

[0042]

[Chemical 10] (However, a = 30 to 50)

[0043]

[Chemical 11] (However, k = 21 to 30)

[0044]

[Chemical 12] (However, k = 15 to 20)

[0045]

[Chemical 13] (However, k = 7 to 10)

[0046]

[Chemical 14]

From Table 5, the conventional methyl hydrogen polysiloxanes represented by Chemical formulas 9 and 10 have the minimum heating conditions as compared with the methyl hydrogen polysiloxanes represented by Chemical formulas 11 to 13 used in the present invention. It turns out to be tough. Further, among the methylhydrogenpolysiloxanes used in the present invention, those having the average degree of polymerization shown in Chemical formulas 11 and 12 are found to be more reactive. Furthermore, it can be seen that the cyclic methylhydrogenpolysiloxane represented by Chemical formula 14 (Treatment B) has high volatility even at low temperatures. In addition, Chemical formula 11, Chemical formula 12 and Chemical formula 13 are respectively referred to as MHPS-1, MHPS-2 and MHPS- below.
It is abbreviated as 3.

Hereinafter, the method for producing the modified powder will be described in Examples 1 to 10. Example 1 100 g of fine particle titanium oxide (primary particle size 35 nm, anatase type) has a chemical formula of MHPS-2, A1
7 g and 0.5 g of treating agent B were mixed using a mixer. Primary heat treatment was performed at 80 ° C. for 2 hours using a blower dryer, followed by heating to 105 ° C. and then heat treatment for 1 hour.

Comparative Example 1 100 g of fine particle titanium oxide (primary particle size 35 nm, anatase type) was mixed with 17 g of methyl hydrogen polysiloxane (KF-9901, manufactured by Shin-Etsu Chemical Co., Ltd.) and 0.5 g of treating agent B using a mixer. Primary heat treatment was performed at 80 ° C. for 2 hours using a blower dryer, followed by heating to 105 ° C. and then heat treatment for 1 hour.

Example 2 1000 g of fine particle titanium oxide (primary particle size: 17 nm, amorphous type) was mixed with 300 g of sericite, and then 130 g of treating agent A having a chemical formula of MHPS-3 and 13 g of treating agent B were added using an air spray. . Using a blast dryer, a temperature of 1 ℃ per minute from room temperature to 95 ℃ (total 70
The heat treatment was performed for 0.5 hours after the primary heat treatment was performed for 10 minutes, followed by raising the temperature to 130 ° C.

Example 3 100 g of mica and a treating agent A having a chemical formula of MHPS-3
8 g and treating agent B5 g were mixed and stirred using a mixer. Then, heat treatment was performed at 130 ° C. for 5 hours using a dryer.

Example 4 1 kg of sericite, 20 g of treating agent A and 20 g of treating agent B having a chemical formula of MHPS-3 were mixed and stirred using a Henschel mixer. Then, using a dryer, 110
After heat treatment at 4 ° C for 4 hours, heat treatment was performed at 180 ° C for 3 hours.

Example 5 Treatment agent A3 having 1 Kg of talc and a chemical formula of MHPS-1
0 g and treating agent B5 g were mixed and stirred using a Henschel mixer. Then, using a dryer, heat treatment was performed at 110 ° C. for 4 hours and then at 190 ° C. for 3 hours.

Example 6 After mixing 100 g of yellow iron oxide (primary particle size 0.7 μm) and 25 g of sericite, 3.8 g of treating agent A having the chemical formula of MHPS-2 and 1.25 g of 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./min (75 minutes in total), followed by heating to 105 ° C. and then heat treatment for 1 hour. .

Comparative Example 2 100 g of yellow iron oxide (primary particle size 0.7 μm) and 25 g of sericite were mixed, and then 3.8 g of a treating agent having a chemical formula of MHPS-2 was mixed by using a spray. Then, using a blast dryer, primary heat treatment was performed at a rate of 0.4 ° C / min (total 75 minutes) from 60 ° C to 90 ° C, followed by 10
After heating to 5 ° C., heat treatment was performed for 1 hour.

Comparative Example 3 After mixing 100 g of yellow iron oxide (primary particle size 0.7 μm) and 25 g of sericite, 3.8 g of methyl hydrogen polysiloxane (KF-99P, manufactured by Shin-Etsu Chemical Co., Ltd.) was sprayed. Mixed. Then, using a blast dryer, a speed of 0.4 ° C / min from 60 ° C to 90 ° C (75 minutes in total)
The heat treatment was performed for 1 hour after the temperature was raised to 105 ° C.

Example 7 100 g of red iron oxide (primary particle diameter 0.7 μm) and 25 g of sericite were mixed, and then 3.8 g of treating agent A having the chemical formula of MHPS-2 and 1.25 g of treating agent B were mixed by using a spray. . Then, heat treatment was performed at 120 ° C. for 1 hour using a blower dryer.

Example 8 After mixing 100 g of black iron oxide (primary particle size 0.6 μm) and 25 g of sericite, 3.8 g of treating agent A having a chemical formula of MHPS-2 and 0.7 g of treating agent B were sprayed. Mixed. Then, using a blast dryer, the temperature is changed from 60 ° C to 9 ° C.
Primary heat treatment was performed at a rate of 0.4 ° C./min (total 75 minutes) up to 0 ° C., followed by heating to 100 ° C. and then heat treatment for 1 hour.

Example 9 900 g of titanium oxide (primary particle size: 0.6 μm) was mixed with 100 g of sericite, and then 40 g of treating agent A having a chemical formula of MHPS-3 and 2 g of treating agent B were added using an air spray, and a mixer was used. Stir and mix using. Using a blast dryer, perform primary heat treatment from 60 to 120 ° C at a rate of 2 ° C per minute (total 30 minutes), then 130 ° C.
After the temperature was raised to 2, the secondary heat treatment was performed for 0.4 hours.

Comparative Example 4 900 g of titanium oxide (primary particle size 0.6 μm) was mixed with 100 g of sericite, and then methylhydrogenpolysiloxane (KF-9901, manufactured by Shin-Etsu Chemical Co., Ltd.) 40
g and 20 g of the treating agent B are isopropyl alcohol 100
A solution dissolved in 0 g was added, and the mixture was stirred and mixed using a mixer. After distilling off the solvent, use a blast dryer to 60 ℃
To 120 ° C. at a rate of 2 ° C. per minute (total 30 minutes), primary heat treatment is performed, and then the temperature is raised to 130 ° C.
Secondary heat treatment was performed for 4 hours.

Example 10 100 g of mica titanium, 8 g of treating agent A having a chemical formula of MHPS-1 and 2 g of treating agent B were mixed and stirred using a mixer. The obtained powder is dried at 180 ° C using a blow dryer.
It heat-processed for 1 hour.

Comparative Example 5 100 g of mica titanium, 8 g of treating agent A having a chemical formula of MHPS-1 and 2 g of treating agent B were dispersed in 120 parts of trichlene, and then the solvent was distilled off. The obtained powder was pulverized using a mixer, and then heat-treated at 180 ° C. for 1 hour using a blow dryer.

Comparative Example 6 100 g of mica titanium and 8 g of treating agent B were mixed using a mixer. The obtained powder is dried with a blast dryer to 180
Heat treatment was performed at 0 ° C. for 1 hour.

Examples of cosmetics using the modified powders produced in Examples 1 to 10 will be described below in Examples 11 to 13.

Example 11 Foundation A foundation was prepared according to the following formulation.

[0066]

[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, it was crushed with a crusher. After that, it was pressed and filled into a product. The product was left in the sun for 1 week, but no discoloration or odor was observed.

Comparative Example 6 Foundation A foundation was prepared according to the following formulation.

[0069]

[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, it was crushed with a crusher. After that, it was pressed and filled into a product. This product lacked water resistance and was easily broken. When this product was left in the sun for 1 week, discoloration and odor were observed.

Example 12 Eye Shadow An eye shadow was prepared according to the following formulation.

[0072]

[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, it was crushed with a crusher. After that, it was pressed and filled into a product.

Comparative Example 7 Eye Shadow An eye shadow was prepared according to the following formulation.

[0075]

[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, it was crushed with a crusher. After that, it was pressed and filled into a product.

Example 13 Sun oil

[0078]

[Table 10]

Component A was gradually added to component B that had been uniformly mixed and dissolved, and mixed using a sand mill to obtain a product. The obtained product was excellent in transparency. In addition, it did not discolor under sunlight.

Comparative Example 8 Sun oil

[0081]

[Table 11]

Component A was gradually added to component B that had been uniformly mixed and dissolved, and mixed using a sand mill to obtain a product. The obtained product was excellent in transparency, but turned blue under sunlight.

[0083]

[Table 12]

[0084]

[Table 13]

[0085]

[Table 14]

From Table 12, it was confirmed that the modified fine particle powder of the present invention has few hard secondary agglomerates and is excellent in water repellency, and that the catalytic activity of fine particle titanium oxide is also blocked. From Table 13, it was confirmed that the modified powder of the present invention had few hard secondary aggregates 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 results in Table 14, it was confirmed that when the modified powder of the present invention was blended with a cosmetic, a cosmetic having a moist feel and having a good feel was obtained. Furthermore, comparing the results of the light resistance of Example 11 and Comparative Example 7, it can be seen that the light resistance of Example is extremely improved.

From the above, from the result of measuring the agglomeration state of the modified powder of the present invention with a measuring instrument and the change in the feel when the modified powder was blended into cosmetics, a loose coagulation that could be broken by ultrasonic waves was obtained. It is considered that the aggregate is generated.

[0088]

As described above, according to the present invention, after the powders are coated with methylhydrogenpolysiloxane having a specific structure and cyclic methylhydrogenpolysiloxane, heat treatment is carried out under a specific temperature condition. This provides a modified powder that has loose agglomeration, excellent water repellency, and has blocked catalytic activity, and by blending this modified powder, excellent quality stability and a moist feel are obtained. It is clear to provide cosmetics that have.

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[Procedure amendment]

[Submission date] October 14, 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, k is an average number and k = 7 to 30) and cyclic methyl hydrogen polysiloxane having the following general chemical formula.

[Chemical 2] A modified powder obtained by mixing and with and heat-treated at 80 to 200 ° C. for 0.5 to 5 hours.

[Procedure Amendment 2]

[Document name to be amended] Statement

[Name of item to be corrected] 0003

[Correction method] Change

[Correction content]

[0003]

[Chemical 3] (However, a = 30 to 50)

[Procedure 3]

[Document name to be amended] Statement

[Correction target item name] 0008

[Correction method] Change

[Correction content]

[0008]

[Chemical 5] (However, k is an average number, and k = 7 to 30)

[Procedure amendment 4]

[Document name to be amended] Statement

[Correction target item name] 0018

[Correction method] Change

[Correction content]

[0018]

[Chemical 7] (However, k is an average number and k = 7 to 30) Hereinafter, the methylhydrogenpolysiloxane having this structure will be referred to as a treating agent A.

[Procedure Amendment 5]

[Document name to be amended] Statement

[Correction target item name] 0042

[Correction method] Change

[Correction content]

[0042]

[Chemical 10] (However, a = 30 to 50)

[Procedure correction 6]

[Document name to be amended] Statement

[Correction target item name] 0043

[Correction method] Change

[Correction content]

[0043]

[Chemical 11] (However, k = 21 to 30)

[Procedure Amendment 7]

[Document name to be amended] Statement

[Correction target item name] 0044

[Correction method] Change

[Correction content]

[0044]

[Chemical 12] (However, k = 15 to 20)

[Procedure Amendment 8]

[Document name to be amended] Statement

[Name of item to be corrected] 0045

[Correction method] Change

[Correction content]

[0045]

[Chemical 13] (However, k = 7 to 10)

Claims (3)

[Claims] 1. Powders and methylhydrogenpolysiloxane having the following general chemical formula: (However, k is an average number, k = 7 to 30) and a cyclic methyl hydrogen polysiloxane having the following general chemical formula: A modified powder obtained by mixing and with and heat-treated at 80 to 200 ° C. for 0.5 to 5 hours. 2. After mixing the powders with the methylhydrogenpolysiloxane according to claim 1 and the cyclic methylhydrogenpolysiloxane, a primary heat treatment is carried out at 60 to 120 ° C. for 0.5 to 4 hours, and subsequently. Modified powder having a temperature higher than that of the primary heat treatment and subjected to the secondary heat treatment at 80 to 200 ° C. for 0.2 to 3 hours. 3. A cosmetic comprising the modified powder according to claim 1 or 2.