JPH0679163A - Water-and oil-repellent composite powder and cosmetic containing the powder - Google Patents

Abstract

PURPOSE:To obtain cosmetic powder which has excellent water- and oil- repellency, does not cause a dissolution of cosmetic makeup and gives a comfortable feeling to a user by mixing the plate-like powder and microgranular powder of a specific granular group and treating their surface using a specific surface treatment agent. CONSTITUTION:The plate-like powder with an average cubic cumulative diameter of 1 to 50mum of mica or sericite and the microgranular powder with an average cubic cumulative diameter of 0.001 to 1mum of titanium oxide or zinc oxide are mixed together, and the compound powder thus obtained is subjected to a surface treatment using phosphoric ester as shown in formula [R<1>(CnH2nO)m]yPO(OM)3-y (R<1> is a 6 to 21C linear or branched chain perfluoroalkyl group or perfluorallkyloxy group; M is H<+>, alkali metal atom, n=1 to 4, m=1 to 10, y=1 to 3). The dosage of this phosphoric ester is 0.01 to 30wt.% for the compound powder.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a water- and oil-repellent composite powder composed of a plate-like powder and a fine particle powder. Consisting of a fine powder with a cumulative average diameter of 0.001 to 1 μm, it has no squeaky or rough feeling when blended into cosmetics, exhibits excellent spreadability and adhesion on the skin, and is powdery. The present invention relates to a water- and oil-repellent composite powder, which has a characteristic that it has a fine finish and does not easily cause the makeup to be damaged by sebum, and a cosmetic containing the same.

[0002]

BACKGROUND OF THE INVENTION Cosmetics containing powder for cosmetics are currently used as makeup cosmetics such as foundation, white powder, blusher, eye shadow, eyebrow, hoddy powder, baby powder. Body cosmetics and the like are commercially available. In these cosmetics, 80% or more of the ingredients are generally powder for cosmetics. Therefore, the properties of the cosmetic powder have a great influence on each makeup performance, and in addition to the excellent spreadability and adhesion on the skin, the cosmetic powder has a property for preventing makeup breakdown due to sebum. Oil repellency is required.

In recent years, it has been proposed to treat the powder with a fluorine compound to impart water repellency and oil repellency for the purpose of preventing makeup from being damaged by sebum (Japanese Patent Laid-Open No. 55-16720).
9, JP-A-62-250074, JP-A-1-18081
1, U.S. Pat. No. 3,632,744).

However, fine particles of titanium oxide, zinc oxide, iron oxide, etc., which are usually used as powders for cosmetics, having a volume cumulative average diameter of 1 μm or less have extremely strong cohesive force by themselves, so that the fluorine compound is used. However, there is a problem in terms of usability, such as a squeaky feeling and a poor spread due to the fine powder remaining in the cosmetics containing it.

On the other hand, as a general method for improving the usability of powder cosmetics containing fine particle powder, it is possible to use fine particle powder in combination with spherical powder having a volume cumulative average diameter of 1 μm or more. To be

However, also in this method, the compounding ratio of the spherical powder in the powder cosmetic is increased by compounding the fine particle powder and the spherical powder, but the squeaky feeling and the poor spreadability are improved. However, there is a drawback that the adhesion to the skin is reduced and the powderyness is increased.

Therefore, in order to improve the adhesiveness of the powder cosmetics and eliminate the powderiness, it is necessary to combine the fine particle powder with the plate-like powder such as mica, talc, and sericite.

However, Hybridizer (Ltd.)
When compounded by an air impact method using Nara Machinery, etc., or a powder mixing method using a ball mill, Ong Mill (made by Hosokawa Micron Co., Ltd.), the above-mentioned plate-like powder is crushed and powder makeup It does not improve the usability of the food.

Therefore, it is desired to develop a powder for cosmetics which is excellent in water repellency and oil repellency, does not cause makeup disintegration due to sebum, etc., and does not cause squeaky feeling or powdery feeling and has a good usability. Was there.

[0010]

Under these circumstances, the inventors of the present invention have conducted extensive studies and as a result, as a result, mixed a plate-like powder having a specific particle diameter and a fine particle powder and using a specific surface treatment agent. We have found that the above problems can be solved by surface treatment, and completed the present invention.

That is, in the present invention, the volume cumulative average diameter is 1 to 5
One or more types of plate-like powder of 0 μm and volume cumulative average diameter 0.00
A water- and oil-repellent composite powder, characterized in that the composite powder obtained by mixing one or more kinds of fine particle powder of 1 to 1 μm is surface-treated with a phosphoric acid ester represented by the following general formula (1). The present invention provides a body and a cosmetic containing the same.

The plate-like powder used in the present invention is used for ordinary cosmetics having a volume cumulative average diameter of 1 to 50 μm and is not particularly limited as long as it is plate-like, and mica, sericite, talc, kaolin, Montmorillonite, bentonite, plate barium sulfate, plate silica, clay, calcium carbonate,
Boron nitride etc. are mentioned.

The fine particle powder to be composited with the plate-like powder is not particularly limited as long as it has a volume cumulative average diameter of 0.001 to 1 μm and is used in ordinary cosmetics. Examples include iron, zirconium oxide, ultramarine blue, dark blue, red No. 202, and cerium oxide.

In the present invention, the mixing ratio of the plate-like powder and the fine particle powder is a weight ratio of plate-like powder / fine particle powder = 100/1.
˜100 / 80 is preferable, and the particle size ratio is a volume cumulative average diameter of plate-like powder / fine particle powder = 2/1 to 1
It is preferably 000/1.

A mixer such as a Henschel mixer, a Nauta mixer or a rocking mixer is used for mixing the plate-like powder and the fine particle powder used in the water- and oil-repellent composite powder of the present invention, and the mixture is dry mixed. Alternatively, a wet process may be performed using a suitable dispersion medium.

Further, the surface treating agent used for the surface treatment of the composite powder of the plate-like powder and the fine particle powder obtained as described above is represented by the following general formula (1) [R ¹ (C _n H _2n O) _m ] _y PO (OM) _3-y (1) [In the formula, R ^{1 is a} linear or branched perfluoroalkyl group having 6 to 21 carbon atoms or a perfluoroalkyloxy group. Indicates. M: represents a hydrogen atom, an alkali metal atom, an ammonium ion or a substituted ammonium. n: shows the number of 1-4. m: shows the number of 0-10. y: shows the number of 1-3. ] It is a phosphoric acid ester represented by these, For example, the following compounds can be illustrated.

That is, diheptadecafluorodecylphosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (═O) (OH)], heptadecafluorodecylphosphate [(C ₈ F ₁₇ C ₂ H ₄ O)
P (= O) (OH) 2 ], sesqui a mixture of heptadecafluorodecyl phosphoric acid and di-heptadecafluorodecyl phosphoric acid heptadecafluorodecyl phosphoric acid [(C ₈ F _{1 7
C 2 H 4 O) r P} (= O) (OH) 3-r, 2>r> 1 ], in the general formula (1), R ¹ is perfluoroalkyl of 6 to 18 carbon atoms (average 9) in group, phosphoric acid ester of M is a hydrogen atom in y is about 1.5 _{[(C s F 2s + 1 C} 2 H 4 O) 1.5
P (= O) (OH) _1.5 , s = 6 to 18], and alkali metal salts, ammonium salts, and substituted ammonium salts of these phosphoric acid esters (for example, monoethanol ammonium salt, diethanol ammonium salt, triethanol ammonium salt) Alkanol ammonium salts such as and salts of basic amino acids).

In the present invention, the amount of the phosphoric acid ester (1) used is preferably 0.01 to 30% by weight, more preferably 0.5 to 15% by weight based on the composite powder to be treated. If the amount used is less than 0.01% by weight, sufficient water repellency
Oil repellency cannot be obtained, and if it exceeds 30% by weight, the feeling of use becomes poor, which is not preferable.

As the surface treatment method of the composite powder for obtaining the water- and oil-repellent composite powder of the present invention, either a direct dry method or a wet method using an appropriate solvent can be used.

Of these, the dry method is a simple and effective method. According to this method, the fine powder of the phosphoric acid ester (1) as the surface treatment agent and the composite powder are mixed by stirring, Alternatively, the surface of the composite powder can be easily treated by mixing the phosphoric acid ester (1) and the composite powder and then co-milling.

In the case of the wet method, the phosphoric acid ester (1) which is a surface treating agent is used in a suitable solvent (for example, water, ethanol, isopropyl alcohol, chloroform, Freon R113 and a mixed solvent thereof). (1) is dissolved in a solvent), and a composite powder consisting of a plate-like powder and fine particle powder is dispersed in this solution, and the solvent is removed by solvent topping or filtration at room temperature or after heating, and then dried. To do. Further, a solvent in which the phosphoric acid ester (1) is dissolved may be added by spraying or dropping, and the mixture may be uniformly dispersed and then dried.

In carrying out the dry method and the wet method in such surface treatment, a mixing and stirring device such as a Henschel mixer or a super mixer can be used.

The water- and oil-repellent composite powder of the present invention thus obtained is suitable for use as a powder for cosmetics, and can be added in an amount of 0.1 to 99.0% by weight in the total amount of the cosmetic.

In addition to the above-mentioned essential components, the cosmetic composition of the present invention may contain, if necessary, components used in ordinary cosmetic compositions. For example, solid / semi-solid oils such as petrolatum, lanolin, ceresin, microcrystalline wax, carnauba wax, candelilla wax, higher fatty acids and higher alcohols; liquid oils such as squalane, liquid paraffin, ester oils, diglycerides, triglycerides, silicone oils; Fluorine-based oil agents such as perfluoropolyether, perfluorodecalin and perfluorooctane; inorganic and organic pigments; inorganic and organic pigments surface-treated with silicone, metal soap, lecithin, amino acids, collagen, polymers, fluorine compounds, etc. Tar dyes,
Coloring agents such as natural pigments; other than water-soluble and oil-soluble polymers,
Surfactants, ethanol, preservatives, antioxidants, thickeners, pH adjusters, fragrances, UV absorbers, moisturizers, blood circulation promoters, cooling sensations, antiperspirants, bactericides, skin activating agents, water Etc. can be blended within a qualitative and quantitative range that does not impair the object and effect of the present invention.

The cosmetics of the present invention can be manufactured by a conventional method, and are the basis for powders, foundations, creamy foundations, dual-use foundations, make-up cosmetics such as white powder, eye shadows and blushers, emulsions, creams and the like. It can be applied to cosmetics and body cosmetics such as body powder and baby powder.

[0026]

The water- and oil-repellent powder of the present invention is rich in water repellency and oil repellency, and is excellent in feeling in use. Therefore, the cosmetics containing this have extremely good water resistance and oil resistance, have good makeup retention to prevent makeup deterioration due to sebum, etc., and have good spreadability and adhesion on the skin, Gives a good feel and fine finish.

[0027]

The present invention will be described in more detail with reference to examples, but the present invention is not limited thereto. In the following, "average diameter" means "volume cumulative average diameter".

Example 1 50 g of sericite (average diameter 8 μm, plate-like powder) and 50 g of titanium oxide (average diameter 0.3 μm, fine particle powder) were put in a Henschel mixer and mixed for 3 minutes. Next, 100 g of the obtained composite powder was placed in a round bottom flask, and diheptadecafluorodecylphosphoric acid [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ was added thereto.
A solution prepared by heating 5.0 g of P (═O) (OH)] in 500 g of isopropyl alcohol was added and mixed at 60 ° C. for 4 hours. Then, isopropyl alcohol was distilled off under reduced pressure, and the residue was dried to obtain 105 g of a target water / oil repellent composite powder.

Example 2 100 g of sericite (average diameter 8 μm, plate powder) and 100 g of titanium oxide (average diameter 0.3 μm, fine particle powder) were put in a Henschel mixer and mixed for 3 minutes. Next, 100 g of the obtained composite powder was placed in a round bottom flask, 500 ml of ion-exchanged water was added, and then perfluoroalkyl phosphate ester dioxyethylamine salt [(C _n H
_{2n + 1} C ₂ H ₄ O) _y P (= O) (ONH ₂ (CH ₂ CH ₂ O
33 g of an approximately 17.5% aqueous solution of (H) ₂ ) _3-y ] (n = 6 to 18, n = 9, 2>y> 1) was added, and the mixture was stirred at 40 ° C.
Next, 1N-hydrochloric acid 40 ml was added to lower the pH of the aqueous solution to 3 or less, and perfluoroalkylphosphoric acid was precipitated on the powder surface, which was then filtered, washed with water and dried to obtain the desired water- and oil-repellent composite powder. 105 g of body was obtained.

Example 3 80 g of mica (average diameter 10 μm, plate-like powder) and 20 g of fine particle titanium oxide (average diameter 0.05 μm, fine particle powder) were put in a Henschel mixer and mixed for 5 minutes. Then
100 g of the obtained composite powder was placed in a round bottom flask, and diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H
₄ O) ₂ P (= O) (OH)] 5.0 g was dissolved by heating in 500 g of isopropyl alcohol, and the mixture was added at 60 ° C. for 4 hours.
Mixed for hours. Then, isopropyl alcohol was distilled off under reduced pressure, and the residue was dried to obtain 105 g of a target water / oil repellent composite powder.

Example 4 120 g of mica (average diameter 10 μm, plate-like powder) and fine particles
Titanium oxide (average diameter 0.05μm, fine particle powder) 30g
Was placed in a Henschel mixer and mixed for 5 minutes. Next
Then, add 100 g of the obtained composite powder to a round bottom flask.
After adding 500 ml of deionized water, add perfume to it.
Oroalkyl phosphate dioxyethylamine salt
[(C_nH_{2n + 1}C₂H_FourO)_yP (= O) (ONH₂(CH₂
CH₂OH)₂) _3-y] (N = 6 to 18, n = 9, 2> y
Add 33 g of a 17.5% aqueous solution of> 1) and stir at 40 ° C.
I stirred. Then, 40 ml of 1N hydrochloric acid was added to form an aqueous solution.
Lower the pH to 3 or less and apply perfluoroalkyl
After the acid is precipitated, it is filtered, washed with water and dried to obtain the desired
105 g of the water- and oil-repellent composite powder of

Example 5 The titanium oxide of Example 1 was replaced with red iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Example 6 The titanium oxide of Example 2 was replaced with red iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Example 7 The titanium oxide of Example 1 was replaced with yellow iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Example 8 The titanium oxide of Example 2 was replaced with yellow iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Example 9 The titanium oxide of Example 1 was replaced with black iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Example 10 The titanium oxide of Example 2 was replaced with black iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 1 50 g of sericite (average diameter 8 μm, plate-like powder) and 50 g of titanium oxide (average diameter 0.3 μm, fine particle powder) are put in a Henschel mixer and mixed for 3 minutes. To this, 5 g of methyl hydrogen polysiloxane was added and further mixed for 5 minutes to obtain 105 g of methyl hydrogen polysiloxane coated composite powder.

Comparative Example 2 100 g of sericite (average diameter 8 μm, plate-like powder) and 100 g of titanium oxide (average diameter 0.3 μm, fine particle powder) are put in a Henschel mixer and mixed for 3 minutes. 100 g of the obtained composite powder was placed in a 1-liter round bottom flask, 5 g of methylhydrogenpolysiloxane and 100 g of hexane were added thereto, and the mixture was stirred for 10 minutes. After heating and drying at 8 ° C. for 8 hours, 105 g of methylhydrogenpolysiloxane-coated composite powder was obtained.

Comparative Example 3 80 g of mica (average diameter 10 μm, plate-like powder) and 20 g of fine particle titanium oxide (average diameter 0.05 μm, fine particle powder) are put in a Henschel mixer and mixed for 3 minutes. To this, 5 g of methyl hydrogen polysiloxane was added and further mixed for 5 minutes to obtain 105 g of methyl hydrogen polysiloxane coated composite powder.

Comparative Example 4 120 g of mica (average diameter 10 μm, plate-like powder) and 30 g of fine particle titanium oxide (average diameter 0.05 μm, fine particle powder)
In a Henschel mixer and mix for 3 minutes. 100 g of the obtained composite powder was placed in a 1 liter round bottom flask,
To this, 5 g of methyl hydrogen polysiloxane and 100 g of hexane were added, and the mixture was stirred for 10 minutes, then hexane was distilled off under reduced pressure, and dried by heating in an electric dryer at 180 ° C. for 8 hours to obtain a composite powder coated with methyl hydrogen polysiloxane. 105 g were obtained.

Comparative Example 5 The titanium oxide of Comparative Example 1 was replaced with red iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 6 The titanium oxide of Comparative Example 2 was replaced with red iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 7 The titanium oxide of Comparative Example 1 was replaced with yellow iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 8 Titanium oxide of Comparative Example 2 was replaced with yellow iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 9 The titanium oxide of Comparative Example 1 was replaced with black iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 10 The titanium oxide of Comparative Example 2 was replaced with black iron oxide (average diameter 0.3 μm,
Instead of the fine particle powder), 105 g of the target water- and oil-repellent composite powder was obtained by the same operation.

Comparative Example 11 Titanium oxide (average diameter 0.2 μm, fine particle powder) was placed in a round bottom flask, and diheptadecafluorodecylphosphoric acid [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P ( = O) (OH)] 5.0
A solution obtained by heating and dissolving 500 g of isopropyl alcohol in 500 g was added and mixed at 60 ° C. for 4 hours. Then, isopropyl alcohol was distilled off under reduced pressure, and the residue was dried to obtain 105 g of the desired water / oil repellent powder.

Comparative Example 12 Titanium oxide (average diameter 0.2 μm, fine particle powder) was placed in a 1 liter round bottom flask, and 500 ml of deionized water was added,
It perfluoroalkyl phosphoric acid esters dioxy ethylamine salt _{[(C n H 2n + 1 C} 2 H 4 O) y P (= O) (O
_{NH 2 (CH 2 CH 2 OH} ) 2) 3-y ] (n = 6~18, n
= 9,2>y> 1) about 33% of a 17.5% aqueous solution was added, and the mixture was stirred at 40 ° C. Next, 40 ml of 1N hydrochloric acid was added to lower the pH of the aqueous solution to 3 or less, and perfluoroalkylphosphoric acid was precipitated on the powder surface, which was then filtered, washed with water and dried to obtain the desired water- and oil-repellent powder. 105 g were obtained.

Comparative Example 13 Fine Titanium Oxide (Average Diameter 0.05 μm, Fine Particle Powder)
100 g was placed in a round-bottomed flask, and diheptadecafluorodecylphosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) was added thereto.
(OH)] 5.0 g to isopropyl alcohol 500 g
The solution dissolved by heating was added to and mixed at 60 ° C. for 4 hours. Then, isopropyl alcohol was distilled off under reduced pressure, and the residue was dried to obtain 105 g of the desired water / oil repellent powder.

Comparative Example 14 Fine Titanium Oxide (Average Diameter 0.05 μm, Fine Particle Powder)
Put 100g in a round bottom flask and deionized water 500ml
And then the perfluoroalkyl phosphate ester dioxyethylamine salt [(C _n H _{2n + 1} C ₂ H ₄ O) _y P
_{(= O) (ONH 2 (} CH 2 CH 2 OH) 2) 3-y ] (n =
33 g of an approximately 17.5% aqueous solution of 6-18, n = 9, 2>y> 1) was added, and the mixture was stirred at 40 ° C. Next, 40 ml of 1N hydrochloric acid was added to lower the pH of the aqueous solution to 3 or less, and perfluoroalkylphosphoric acid was precipitated on the powder surface, which was then filtered, washed with water and dried to obtain the desired water- and oil-repellent powder. 105 g were obtained.

Comparative Example 15 The titanium oxide of Comparative Example 11 was replaced with red iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 16 The titanium oxide of Comparative Example 12 was replaced with red iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 7 Titanium oxide of Comparative Example 11 was replaced with yellow iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 18 Titanium oxide of Comparative Example 12 was replaced with yellow iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 19 The titanium oxide of Comparative Example 11 was replaced with black iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 20 The titanium oxide of Comparative Example 12 was replaced with black iron oxide (average diameter 0.3 μm).
m, fine particle powder) to obtain 105 g of the target water- and oil-repellent powder by the same operation.

Comparative Example 21 The sericite of Example 1 was converted to nylon powder (average diameter 6 μm).
m, spherical powder) to obtain 105 g of the target water / oil repellent composite powder by the same operation.

Comparative Example 22 The sericite of Example 2 was converted into nylon powder (average diameter 6 μm).
m, spherical powder) to obtain 105 g of the target water / oil repellent composite powder by the same operation.

Comparative Example 23 The mica of Example 3 was treated with nylon powder (average diameter 6 μm,
Instead of the spherical powder), 105 g of the target water / oil repellent composite powder was obtained by the same operation as described below.

Comparative Example 24 The mica of Example 4 was mixed with nylon powder (average diameter 6 μm,
Instead of the spherical powder), 105 g of the target water / oil repellent composite powder was obtained by the same operation as described below.

Comparative Example 25 The sericite of Example 1 was converted into nylon powder (average diameter 6 μm).
titanium oxide to red iron oxide (average diameter of 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Comparative Example 26 The sericite of Example 2 was converted into nylon powder (average diameter 6 μm).
titanium oxide to red iron oxide (average diameter of 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Comparative Example 27 The sericite of Example 1 was converted into nylon powder (average diameter 6 μm).
m, spherical powder), titanium oxide was added to yellow iron oxide (average diameter 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Comparative Example 28 The sericite of Example 2 was converted to nylon powder (average diameter 6 μm).
m, spherical powder), titanium oxide was added to yellow iron oxide (average diameter 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Comparative Example 29 The sericite of Example 1 was converted to nylon powder (average diameter 6 μm).
m, spherical powder, titanium oxide was added to black iron oxide (average diameter 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Comparative Example 30 The sericite of Example 2 was converted to nylon powder (average diameter 6 μm).
m, spherical powder, titanium oxide was added to black iron oxide (average diameter 0.
(3 μm, fine particle powder), and 105 g of the target water- and oil-repellent composite powder was obtained by the same operation as described below.

Test Example 1 The water repellency, oil repellency and feeling of use of each of the powders obtained in Examples 1 to 10 and Comparative Examples 1 to 30 were evaluated by the following evaluation methods. The results are shown in Tables 1 to 4 below.

(Evaluation method of water repellency) 15 ml of water was put in a beaker for 30 ml, about 0.05 g of each powder was floated on the water, and the beaker was shaken to observe the dispersibility of the powder in water. It evaluated by the following evaluation criteria. Evaluation Criteria 0: The powder was immediately dispersed in water. 1: When the beaker was shaken, the powder was almost dispersed in water within 30 seconds. 2: After shaking the beaker, the water became cloudy after 1 minute, but some powder floated on the water. 3: After shaking the beaker, the water became cloudy after 1 minute, but many powders floated on the water. 4: When the beaker was shaken, the water did not turn cloudy after 1 minute, and no powder dispersed in water was observed. No powder dispersed in water was observed even if the beaker was shaken for 5 minutes or more.

(Evaluation Method of Oil Repellency) Evaluation was carried out in the same manner as in the evaluation method of water repellency except that squalane was placed in a beaker for 30 ml instead of water.

(Evaluation method of feeling of use) Ten professional panelists evaluated the squeaky feeling, the rough feeling, the adhesiveness on the skin, and the elongation on the skin according to the following criteria. Evaluation Criteria O: 8 or more people were judged to be good (no squeaky or rough feeling was judged). Δ: 7 to 5 people were judged to be good (no squeaky or rough feeling was judged). X: 0 to 4 people were judged to be good (no squeaky or rough feeling was judged).

From the results shown in Tables 1 to 4 below, the water- and oil-repellent composite powder of the present invention is excellent in both oil repellency and feeling of use as compared with the case of being treated with methylhydrogenpolysiloxane. Further, it can be seen that the usability is clearly superior to the case where the fine particle powder alone and the composite powder of the fine particle powder and the spherical powder are subjected to the same water and oil repellency treatment as in the present invention.

[0073]

[Table 1]

[0074]

[Table 2]

[0075]

[Table 3]

[0076]

[Table 4]

Example 11 Powder Foundation Powder foundations having the compositions shown in Table 5 below were produced by the following production methods, respectively, and the makeup persistence to sweat and sebum and squeaky feeling, rough feeling, adhesion to the skin, and adhesion on the skin were obtained. The fineness of elongation and finish was evaluated by the following evaluation methods. The results are shown in Table 6.

(Production Method) The powder was mixed and pulverized, transferred to a Henschel mixer, and the oil agent and the fragrance were added and mixed to obtain a uniform mixture. This was press-molded on a gold plate to obtain a product.

(Evaluation Method for Makeup Persistence) An appropriate amount was applied to the face, and 10 professional panelists made a judgment based on the following evaluation criteria for makeup continuity visually with reference to the degree of foundation, twist, and facial luster. I went. Evaluation Criteria ∘: It was determined that 8 or more people did not lose their makeup. Δ: It was determined that 7 to 5 people did not lose their makeup. X: It is determined that 0 to 4 people have not lost their makeup.

(Evaluation method of feeling of use) Ten professional panelists judged the squeaky feeling, the rough feeling, the adhesion on the skin, the elongation on the skin, and the fineness of the finish according to the following judgment criteria. It was Evaluation Criteria O: 8 or more people were judged to be good (no squeaky or rough feeling was judged). Δ: 7 to 5 people were judged to be good (no squeaky or rough feeling was judged). X: 0 to 4 people were judged to be good (no squeaky or rough feeling was judged).

[0081]

[Table 5]

[0082]

[Table 6]

From the above-mentioned evaluation results, the product of the present invention was a powder foundation excellent in the durability of the makeup and the feeling of use as compared with the comparative product.

[0084]

Table 7 Example 12 White powder A white powder having the following composition was produced in the same manner as in Example 11. (Composition) (wt%) (1) Treated powder of Example 1 2 (2) Treated powder of Example 5 1 (3) Treated powder of Example 7 0.1 (4) Treated of Example 9 Powder 0.05 (5) Talc balance (6) Fomblin HCO4 ^{* 1} 10 (7) Preservative 0.1 (8) Perfume 0.05 * 1: Perfluoropolyether (made by Montefluos)

[0085]

Table 8 Example 13 Cheek Red A cheek red having the following composition was produced in the same manner as in Example 11. (Composition) (wt%) (1) Red No. 202 5 treated in the same manner as in Example 2 (2) Treated powder of Example 2 15 (3) Treated powder of Example 6 6 (4) Example 8 Treated powder of 0.5 0.5 (5) Treated powder of Example 0.2 (6) Kaolin balance (7) Mica 10 (8) Dimethyl polysiloxane 10 (9) Preservative 0.1 (10) Perfume 0 .05

[0086]

[Table 9] Example 14 Powder eye shadow A powder eye shadow having the following composition was produced by the following production method. (Composition) (% by weight) (1) Mica titanium 10 (2) Sericite balance (3) Mica 10 (4) Example 6 treated powder 0.5 (5) Example 8 treated powder 0.4 (6) Treated powder of Example 10 0.1 (7) Ultramarine blue 20 treated as in Example 2 (8) Dark blue 20 (9) Dimethylpolysiloxane 10 (10) preservative treated as in Example 2. Agent 0.1 (11) Perfume 0.05

(Production method) The above (2) to (8) were mixed and pulverized, and this and (1) were transferred to a Henschel mixer, and (9)
(11) were added and mixed to be uniform, then, passed through a sieve and press-molded.

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[Procedure amendment]

[Submission date] October 2, 1992

[Procedure Amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0081

[Correction method] Change

[Correction content]

[0081]

[Table 5]

Claims (2)

[Claims] 1. A composite powder obtained by mixing one or more kinds of plate-like powder having a volume cumulative average diameter of 1 to 50 μm and one or more kinds of fine particle powder having a volume cumulative average diameter of 0.001 to 1 μm. A water- and oil-repellent composite powder, which is obtained by surface-treating with a phosphoric acid ester represented by the following general formula (1). [R ¹ (C _n H _2n O) _m ] _y PO (OM) _3-y (1) [In the formula, R ^{1 is a} linear or branched C 6-21 perfluoroalkyl group or perfluoroalkyl. Indicates an oxy group. M: represents a hydrogen atom, an alkali metal atom, an ammonium ion or a substituted ammonium. n: shows the number of 1-4. m: shows the number of 0-10. y: shows the number of 1-3. ] 2. A cosmetic containing the water- and oil-repellent composite powder according to claim 1.