JP3276660B2 - Water / oil repellent powder and cosmetics containing it - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION The present invention has excellent water and oil repellency,
The present invention relates to a powder for cosmetics which does not lose makeup, has good elongation on the skin, and has a good feel upon use, and a cosmetic containing the same.

[0002]

2. Description of the Related Art Cosmetics containing powders include makeup cosmetics such as foundations, white powders, blushers, eye shadows, eye blows, and the like, body cosmetics such as body powders and baby powders. Are commercially available. Cosmetics containing these powders for cosmetics are required to have good cosmetic properties such as good stretch on the skin, good use feeling such as smoothness, and little change in makeup due to sebum.

[0003] In recent years, powders have been treated with fluorine compounds for the purpose of preventing makeup collapse due to sebum or the like, and have been used for water repellency.
It has been proposed to impart oil repellency (Japanese Unexamined Patent Publication No.
167209, JP-A-62-275074, JP-A-1-180811, U.S. Pat. No. 3,632,744).

[0004] However, these water- and oil-repellent powders have a drawback that the smoothness during use becomes extremely poor as compared to before the treatment with a fluorine compound. Therefore,
It has been desired to provide a cosmetic powder having both excellent oil repellency and smooth feel.

[0005]

Under these circumstances, the present inventors have conducted intensive studies and as a result, have found that the above-mentioned problems can be solved by subjecting powder to surface treatment by a specific method. completed.

That is, the present invention provides the following (a)
It is intended to provide a water-repellent / oil-repellent powder obtained by performing a surface treatment with the agent and the agent (b). (A) Agent: a monoalkyl or alkenyl zinc alkali metal salt represented by the general formula (1).

[0007]

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Wherein A represents an alkali metal. R: represents a linear or branched alkyl group or alkenyl group having 8 to 32 carbon atoms. (B) Agent: A compound having, in the molecule, a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom.

The powder used in the present invention (the one not subjected to the surface treatment with the agents (a) and (b); hereinafter, referred to as "raw powder") is not particularly limited. However, for example, silicic acid, silicic anhydride, magnesium silicate, talc, sericite, mica, kaolin, montmorillonite, clay, bentonite, titanium oxide film mica (titanium mica), bismuth oxychloride, boron nitride, zirconium oxide, oxidation Magnesium, zinc oxide, titanium oxide, lower titanium oxide, aluminum oxide,
Inorganic powders such as calcium sulfate, barium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate, red iron oxide, black iron oxide, yellow iron oxide, ultramarine, navy blue, chromium oxide, chromium hydroxide, calamine, carbon black, and composites thereof A polyamide, a polyethylene, a polypropylene, a polystyrene, a polyurethane, a vinyl resin, a urea resin, a melamine resin, an epoxy resin, a polycarbonate resin, a divinylbenzene / styrene copolymer, a silk powder, a cellulose, a metal soap, a tar pigment and a lake pigment thereof. And organic powders such as natural pigments; composites of these inorganic powders and organic powders. These powders are used alone or in combination of two or more. The shape of the raw powder is not particularly limited, and a flat, massive, flaky, spherical powder or the like can be used regardless of the presence or absence of pores. Particularly preferred. The primary particle diameter of the raw powder is not particularly limited as long as the outer shape of the powder is kept, but from the viewpoint of feeling of use, it is 0.01 to
80 μm, particularly preferably 0.1 to 20 μm.

In the general formula (1), which represents the agent (a) used for the surface treatment of the raw powder, ie, an alkali metal salt of a monoalkyl or alkenyl zinc phosphate, R is, for example, octyl, nonyl, decyl , Dodecyl, undecyl, tridecyl, tetradecyl, pentadecyl,
Hexadecyl, heptadecyl, octadecyl, nonadecyl, eicosyl, heneicosyl, docosyl, tricosyl, tetracosyl, pentacosyl, hexacosyl, heptacosyl, octacosyl, nonacosyl, triacontyl, hentriacontyl, dotriacontyl, etc., among which monoalkyl or zinc alkenyl phosphate In order for the alkali metal salt to have better performance in surface treatment of the powder than the shape and size of the particles, a linear alkyl group having 12 to 18 carbon atoms is preferable. Examples of the alkali metal serving as a counter ion include lithium, potassium, and sodium. The preferred molar ratio of each atom in the monoalkyl or alkenyl zinc alkali metal (1) is zinc: alkali metal: phosphorus = 0.8-1.2: 0.8-
1.2: 2.

It is preferable that the alkali metal salt of a monoalkyl or alkenyl zinc phosphate (1) is mainly composed of plate-like crystal particles. Here, the plate-like crystal particles are a general term for particles having a shape of a square plate, an ellipsoid, a disk, a hexagon, a rhombus, or the like. Regarding the size and the like of the plate-like crystal particles, when observed with a scanning electron microscope, (i) the length (plate diameter) of one side in the plate-like direction is 0.1 to 50 μm, and (ii) the plate diameter / Thickness (plate ratio) is 2 or more, and (iii) longest diameter / shortest diameter (plate diameter ratio)
Is preferably 10 or less.

Further, as the agent (b), a linear or branched perfluoroalkyl group having 6 or more carbon atoms, preferably 6 to 21 carbon atoms, or one of the fluorine atoms of the perfluoroalkyl group is contained in the molecule. The compound is not particularly limited as long as it has a group substituted with a hydrogen atom, and includes compounds (b-1), (b-2), (b-3), (b-4) and (b-5) shown below. One or more selected from the group consisting of

Compound (b-1): a phosphate ester represented by the general formula (2). _{[Rf (CH 2) m O} (AO) n] y PO (OM) 3-y (2) wherein, Rf: straight-chain or perfluoroalkyl group or the perfluoro carbon number 6 to 21 branched A group in which one of fluorine atoms of an alkyl group is substituted with a hydrogen atom. A: The same or different and represents an alkylene group having 2 to 3 carbon atoms. M: represents a hydrogen atom, an alkali metal, an ammonium group or a substituted ammonium group. m: Indicates the number of 0 to 12. n: Indicates a number from 0 to 10. y: Indicates the number of 1 to 3. ]

As a specific example of the phosphate (2),
Is diheptadecafluorodecyl phosphate [(C₈F₁₇C_TwoH_FourO)
_TwoP (= O) (OH)], heptadecafluorodecyl phosphate [(C₈F
₁₇C_TwoH_FourO) P (= O) (OH)_Two], Heptadecafluorodecyl phosphorus
A mixture of acid and diheptadecafluorodecyl phosphate
Sesquiheptadecafluorodecyl phosphate [(C₈F₁₇C_TwoH _FourO)
_rP (= O) (OH)_3-r(2> r> 1), smell of the general formula (1)
And Rf is a perfluoro group having 6 to 18 carbon atoms (average of 9)
An alkyl group, y is approximately 1.5 and M is a hydrogen atom
Phosphate ester [(C_lf_{2l + 1}C_TwoH_FourO)_1.5P (= O) (OH)_1.5]
(L = 6-8 (average 9)) and their phosphoric acid
Stell alkali metal salts, ammonium salts, substituted ammo
Ammonium salts (eg, monoethanolammonium salts, die
Tananol ammonium salt, triethanol ammonium
Alkanol ammonium salts such as salts and basic amino acid salts
And the like.

Compound (b-2): an epoxy compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom.

Specific examples of the epoxy compound include the following compounds.

[0017]

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Compound (b-3): a silane compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom.

Specific examples of this silane compound include the following compounds.

[0020]

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Compound (b-4): Titanium having a straight-chain or branched-chain perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom. Compound.

Specific examples of the titanium compound include the following compounds.

[0023]

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Compound (b-5): a polysiloxane compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom. .

Specific examples of the polysiloxane compound include the following compounds.

[0026]

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In the surface treatment of the raw powder for obtaining the water / oil repellent powder of the present invention, the agent (a) and the agent (b) may be used at the same time. After the surface treatment of the raw powder, the surface treatment may be performed with the agent (b),
The surface treatment may be performed in the reverse order. this house,
The inner layer of the water- and oil-repellent powder obtained by performing the surface treatment with the agent (a) and then the surface treatment with the agent (b) is (a)
When the agent and the outer layer are the agent (b), the feeling in use is good and particularly preferred.

The treatment amount of the agent (a) with respect to the raw powder is preferably 0.05 to 20% by weight, more preferably 0.5 to 20% by weight.
15% by weight. If it is less than 0.05% by weight, the surface treatment effect is not sufficient, and if it exceeds 20% by weight, the treatment effect is not so improved, so that there is not much benefit from the viewpoint of economy. The processing amount of the agent (b) to the raw powder is 0.01 to 30% by weight, more preferably 0.5 to 30% by weight.
１５15% by weight. If it is less than 0.01% by weight, sufficient water resistance and oil resistance cannot be obtained, and if it exceeds 30% by weight, the feeling in use becomes poor, which is not preferable.

The surface treatment method of the raw powder with the agent (a)
There is no particular limitation, and either a dry method using a known direct treatment 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 surface of the powder can be easily adjusted to (a) by stirring and mixing the agent (a) and the raw powder, or by mixing the agent (a) and the raw powder and then grinding them together. ) Agent.

In the case of the above wet method, since the agent (a) hardly dissolves in water near neutrality, a soluble alkali metal salt of monoalkyl or alkenyl phosphoric acid is dissolved in water and brought into contact with powder. Thereafter, an aqueous solution of a water-soluble zinc salt is added, and a monoalkyl or alkenyl zinc phosphate alkali metal salt is precipitated and adhered on the powder by salt exchange,
The surface of the powder can be treated by removing the salt generated by the salt exchange by washing with water and drying. As the water-soluble zinc salt used here, for example, zinc chloride, zinc sulfate,
Zinc acetate, zinc nitrate and the like can be mentioned. By changing the reaction conditions such as the addition time of the water-soluble zinc salt, the particle size of the agent (a) deposited on the powder can be controlled.

The method of surface-treating the raw powder with the agent (b) or the powder surface-treated with the agent (a) is not particularly limited, either a dry method or a wet method can be used.
In the case of the dry method, it is performed by mixing the raw powder or the powder surface-treated with the (a) agent and the (b) agent in a mixing and stirring device. In the case of the wet method, the raw powder or the powder surface-treated with the agent (a) is placed in a mixing and stirring device, while the agent (b) is mixed with a suitable solvent [for example, water, ethanol, isopropyl alcohol, chloroform, Fluorocarbon R113 and a mixed solvent thereof], and the mixture is added by spraying or dropping, uniformly dispersed by mixing and stirring, and then dried at room temperature or after heating. However, when the number of carbon atoms of the perfluoroalkyl group in the agent (b) is 8 or more, the fluidity of the compound is significantly reduced. Therefore, mixing is performed in a heated state or an ether solvent such as diethyl ether, diisopropyl ether, or the like. It is preferable to dry at room temperature or after heating by using a mixed solvent system of a fluorine-based solvent such as Freon R113 and hexafluorometa-xylene and an alcohol such as methanol, ethanol, and isopropanol.

In performing the surface treatment with the (a) agent and the (b) agent, for example, a Henschel mixer,
A mixing and stirring device such as a vibrating ball mill, a rotary ball mill, and a super mixer can be used.

The water- and oil-repellent powder of the present invention thus obtained exhibits excellent water- and oil-repellency and can be suitably used as a compounding component of cosmetics. The amount of the water-repellent / oil-repellent powder of the present invention in the cosmetic of the present invention is not particularly limited, but is preferably 0.1 to 99% by weight.

Further, in addition to the water-repellent and oil-repellent powder of the present invention, the cosmetics of the present invention may contain, if necessary, components to be added to ordinary cosmetics. For example, petrolatum, lanolin, ceresin, microcrystalline wax, carnauba wax, candelilla wax, higher fatty acids, solid and semi-solid oils such as higher alcohols; squalane, liquid paraffin, ester oil, diglyceride, triglyceride,
Fluid oils such as silicone oil; perfluoropolyether,
Fluorinated oils such as perfluorodecalin and perfluorooctane; water-soluble and oil-soluble polymers, surfactants, inorganic and organic pigments, silicone, soaps, lecithin,
Inorganic and organic pigments surface-treated with amino acids, collagen, polymers, fluorine compounds, etc., coloring agents such as tar pigments and natural pigments, ethanol, preservatives, antioxidants, pigments, thickeners, pH adjusters, fragrances, An ultraviolet absorber, a humectant, a blood circulation promoter, a cooling agent, an antiperspirant, a bactericide, a skin activator, water and the like can be blended within a qualitative and quantitative range that does not impair the effects of the present invention. The cosmetic of the present invention can be produced by a usual method, and can be used as a foundation for makeup cosmetics such as a powder foundation, a creamy foundation, an oily foundation, a dual-use foundation, a whitening face, an eye shadow, a blusher, and the like, a milky lotion, a cream and the like. The present invention can be applied to body cosmetics such as cosmetics, body powder, and baby powder.

[0035]

Next, the present invention will be described in detail with reference to Examples, but it should not be construed that the invention is limited thereto.

Example 1 100 g of sericite and 5.0 g of sodium monocetyl zinc phosphate, which is a plate-like powder having an average particle size of about 3 μm, were placed in a Heischel mixer and mixed for 10 minutes to carry out the surface treatment of the sericite. Then, 105 g of sericite treated with sodium monocetyl phosphate sodium salt was obtained. Next, the obtained monocetyl phosphate sodium salt-treated sericite 105
g was placed in a round bottom flask, and 5.0 g of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)] was dissolved by heating in 500 g of isopropyl alcohol. The solution was added and mixed at 60 ° C. for 4 hours. Thereafter, isopropyl alcohol was distilled off under reduced pressure and dried to obtain 110 g of the desired water / oil repellent powder.

Example 2 5.0 g of monosodium monocetyl phosphate was dissolved in 500 ml of a 30% aqueous ethanol solution at 80 ° C., 100 g of sericite was added and, while mixing, 100 ml of 2.2 g of zinc sulfate heptahydrate was added. Dissolved in ion-exchanged water was added. After mixing for 30 minutes, 3% sodium hydroxide 1
0 ml was added dropwise to adjust the pH to around 5, and the mixture was further stirred for 1 hour. After the treatment, the mixture was cooled, filtered, and washed with water to remove water-soluble salts, and then dried to obtain 105 g of monocetyl zinc phosphate sodium salt-treated sericite. Next, the obtained monocetyl phosphate sodium salt-treated sericite 10
5 g was placed in a round bottom flask, and sesquiheptadecafluorodecyl phosphate [(C), which was a mixture of heptadecafluorodecyl phosphate and diheptadecafluorodecyl phosphate, was added thereto.
_{8 F 17 C 2 H 4 O} ) r P (= O) (OH) 3-r, 2>r> 1 ], in the general formula (2), Rf par having 6 to 18 carbon atoms (average 9) A fluoroalkyl group, y is approximately 1.5 and M is hydrogen phosphate [(C _n H _{2n + 1} C ₂ H ₄ O) _1.5 P (= 0) (OH) _1.5 ]
A solution prepared by heating and dissolving 5.0 g of isopropyl alcohol in 500 g was added and mixed at 60 ° C. for 4 hours. Thereafter, isopropyl alcohol was distilled off under reduced pressure and dried to obtain 110 g of the desired water / oil repellent powder.

Example 3 Mica 100 g and a plate-like powder having an average particle size of about 10 μm
5.0 g of sodium monocetyl phosphate sodium salt
In a shell mixer, mix for 10 minutes and mix
Surface treatment of sodium nitrite monocetyl phosphate
105 g of salt treated sericite was obtained. Next, the resulting model
Round bottom of sericite treated with zinc nocetyl phosphate sodium salt
Place in a flask and add diheptadecafluorodecyl sulfate
Acid ((C ₈F₁₇C_TwoH_FourO)_TwoP (= O) (OH)] and heptadecafluoro
Decyl phosphate [(C₈F₁₇C_TwoH_FourO) P (= O) (OH)_Two1: 1
5 g of the mixture is heated to 500 g of isopropyl alcohol
The dissolved solution was added and mixed at 60 ° C. for 4 hours. afterwards,
The isopropyl alcohol is distilled off under reduced pressure, dried and
110 g of a water / oil repellent powder was obtained.

Example 4 In Example 1, the following heptadecafluoroundecene was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)]. Example 1 except that oxide was used
To obtain the desired water- and oil-repellent powder.

[0040]

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Example 5 In Example 1, heptadecafluorodecyltriethoxysilane was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)]. ((C ₈ F ₁₇ CH ₂ CH ₂ Si (OC
Except for using ₂ H ₅ ) ₃ ], treatment was performed under substantially the same conditions as in Example 1 to obtain the desired water- and oil-repellent powder.

Example 6 In Example 1, diheptadecafluorodecyl phosphate was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P ((O) (OH)]. Triisopropoxy titanium salt [[(C ₈
F ₁₇ CH ₂ CH ₂₄ O) ₂ P (= O) O] Ti [OCH (CH ₃ ) ₂ ]] was used and treated under substantially the same conditions as in Example 1 to obtain the desired water-repellent property.
An oil-repellent powder was obtained.

Example 7 In Example 1, the following compound having a perfluoroalkyl group instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P ((O) (OH)] was used. The same water-repellent and oil-repellent powder was obtained by treating under substantially the same conditions as in Example 1 except that the polysiloxane compound was used.

[0044]

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Example 8 The procedure of Example 2 was repeated, except that barium sulfate (manufactured by Sakai Chemical Industry) was used in place of sericite. A powder was obtained.

COMPARATIVE EXAMPLE 1 100 g of sericite and 5.0 g of sodium monocetyl phosphate sodium salt, which is a plate-like powder having an average particle size of about 3 μm, were placed in a Henschel mixer and mixed for 10 minutes to perform the surface treatment of the sericite. Then, 105 g of sericite treated with sodium monocetyl phosphate sodium salt was obtained.

COMPARATIVE EXAMPLE 2 5.0 g of monosodium monocetyl phosphate was dissolved in 500 ml of a 30% aqueous ethanol solution at 80 ° C., 100 g of sericite was added, and 2.2 g of zinc sulfate heptahydrate was added in 100 ml while mixing. Dissolved in ion-exchanged water was added. After mixing for 30 minutes, 10 ml of 3% sodium hydroxide was added dropwise to adjust the pH to around 5, and the mixture was further stirred for 1 hour. After the treatment, the mixture was cooled, filtered, and washed with water to remove water-soluble salts, and then dried to obtain 105 g of monocetyl zinc phosphate sodium salt-treated sericite.

Comparative Example 3 Diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)] in a 1 liter round bottom flask (or kneader).
100 g of sericite was added to a solution obtained by dissolving 0 g in 500 g of isopropyl alcohol, and mixed at 60 ° C. for 4 hours. Then, isopropyl alcohol was distilled off under reduced pressure and dried to obtain 105 g of a comparative powder.

Comparative Example 4 In Comparative Example 3, heptadecafluoroundecene oxide (heptadecafluoroundecene oxide) was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)]. Comparative Example 3 was treated under substantially the same conditions as in Comparative Example 3 except that Example 4 was used.

Comparative Example 5 In Comparative Example 3, heptadecafluorodecyltriethoxysilane was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)]. ((C ₈ F ₁₇ CH ₂ CH ₂ Si (OC
Except for using the ₂ H _{5) 3]} to obtain a comparative powder was treated in substantially the same conditions as Comparative Example 3.

Comparative Example 6 In Comparative Example 3, diheptadecafluorodecyl phosphate was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P (= O) (OH)]. Triisopropoxy titanium salt [[(C ₈
F ₁₇ CH ₂ CH ₂ O) ₂ P (= 0) O] Ti [OCH (CH ₃ ) ₂ ] ₃ ], except that Comparative Example 3 was treated under substantially the same conditions as in Comparative Example 3 to obtain a comparative powder. Was.

COMPARATIVE EXAMPLE 7 In Comparative Example 3, the polyhedral polymer having a perfluoroalkyl group was used instead of diheptadecafluorodecyl phosphate [(C ₈ F ₁₇ C ₂ H ₄ O) ₂ P () O) (OH)]. A comparative powder was obtained by treating under substantially the same conditions as in Comparative Example 3 except that a siloxane compound (same as in Example 7) was used.

Comparative Example 8 A comparative powder was obtained by treating under substantially the same conditions as in Comparative Example 1 except that barium sulfate (manufactured by Sakai Chemical Industry) was used instead of sericite.

Test Example 1 Each of the powders obtained in Examples 1 to 8 and Comparative Examples 1 to 8 was evaluated for water repellency, oil repellency and feel in use by the following evaluation methods. The results are shown in Table 1 below. (Evaluation method of water repellency) Put 15 ml of water in a 30 ml beaker, float about 0.05 g of each powder on the water, shake the beaker, observe the dispersibility of the powder in water, and evaluate the following. The evaluation was based on criteria.

Evaluation Criteria 0: The powder was immediately dispersed in water. 1: When the beaker was shaken, the powder was almost completely dispersed in water within 30 seconds. 2: When the beaker was shaken, the water became white and cloudy after 1 minute, but powder floating in the water was also observed. 3: When the beaker was shaken, the water became cloudy and white after 1 minute, but there were many powders floating on the water. 4: One minute after the beaker was shaken, the water was not white and cloudy, and no powder dispersed in the water was observed. Even when the beaker was shaken for 5: 1 minutes or more, no powder dispersed in water was observed.

(Evaluation Method of Oil Repellency) Evaluation was performed in the same manner as in the evaluation method of water repellency except that squalane was placed in a 30 ml beaker instead of water. (Evaluation Method of Feeling) The feeling of powder, such as smoothness, squeaking, and roughness, was evaluated by five professional panelists on a scale of 1 to 5 shown below, and the average value was shown.
The feel of untreated powder of sericite A (manufactured by Horie Kako Co., Ltd.) having an average particle size of 7 μ was set to a standard value of 3.0. 1: The feeling such as smoothness is poor. 2: The touch such as smoothness is slightly poor. 3: Normal (equivalent to Sericite A) 4: Feeling such as smoothness is slightly good. 5: Good feeling such as smoothness.

[0057]

[Table 1]

According to Table 1, the water- and oil-repellent powder of the present invention contains at least one monoalkyl or alkenyl zinc alkali metal salt (1) or at least one perfluoroalkyl group having 6 or more carbon atoms in the molecule. It can be seen that, compared to the case where the treatment was carried out using any of the compounds alone, both the water repellency, the oil repellency and the feel were excellent.

Example 9 Pressed Face Powders Pressed face powders having the compositions shown in Table 2 below were produced by the following production methods, respectively, and the makeup durability and use feeling against sweat and sebum were evaluated by the following evaluation methods. Table 3 shows the results. (Preparation method) The powder components were mixed and pulverized, transferred to a Henschel mixer, and an oil agent and a fragrance were added and mixed so as to be uniform. This was press-molded on a metal plate to obtain a product.

[0060]

[Table 2]

(Evaluation Method) Sensory evaluation of the following products was carried out by a panel of 10 experts for the cosmetic durability and feeling of use, and the results were shown by the following criteria. ：: 8 or more good △: 4 to 7 good ×: Less than 4 good

[0062]

[Table 3]

As is evident from Table 3, the product of the present invention was a pressed face powder which was more excellent in cosmetic durability and use feeling than the comparative product.

Example 10 Powder foundation A powder foundation having the following composition was produced in the same manner as in Example 9. (Composition) (% by weight) (1) Water-repellent and oil-repellent cosmetic powder (the one treated in the same manner as in Example 1 is later mixed)-Sericite 45.0-Mica 23.0-Kaolin 5.0・ Titanium oxide 10.0 ・ Bengara 2.0 ・ Yellow iron oxide 2.5 ・ Black iron oxide 0.1 (2) Perfluoropolyether (FOMBLIN HC-04, manufactured by Monteflors) 10.0 (3) Dimethylpoly Siloxane 2.0 (4) Preservative 0.2 (5) Fragrance 0.2

Example 11 Blush A blusher having the following composition was prepared in the same manner as in Example 9. (Composition) (% by weight) (1) Water-repellent / oil-repellent pigment (treated in the same manner as in Example 1 and later mixed) Kaolin balance Mica 13.0 Titanium oxide 12.0 Red 202 0.4 ・ Iron oxide (red, black, yellow) 5.0 (2) Squalane 7.5 (3) Dimethylpolysiloxane 7.5 (4) Preservative 0.05 (5) Fragrance 0.05

Example 12 Powder Eye Shadow Pigments other than titanium mica were mixed and ground first, and then titanium mica was mixed. Otherwise, in the same manner as in Example 11, a powder eye shadow having the following composition was produced. (Composition) (% by weight) (1) Water-repellent / oil-repellent pigment (treated in the same manner as in Example 1 and subsequently mixed) • Titanium mica 4.9 • Sericite balance • Mica 24.7 • Iron oxide ( (Red, yellow, black) 2.0-Ultramarine blue 9.8-Dark blue 14.6 (2) Dimethylpolysiloxane 1.9 (3) Squalane 1.9 (4) Vaseline 1.9 (5) Sorbitan trioleate 1. 0 (6) Preservative 1.0 (7) Fragrance 0.1

Example 13 Dual-Use Powder Foundation A double-use powder foundation having the following composition was prepared in Example 12.
It was manufactured in the same manner as described above. (Composition) (% by weight) (1) Water-repellent / oil-repellent pigment (treated in the same manner as in Example 1 and mixed later) • Mica balance • Talc 4.8 • Titanium oxide 14.0 • Titanium mica 5 Iron oxide (red, yellow, black) 8.2 Zinc oxide 4.5 Aluminum oxide 10.0 Barium sulfate 5.0 Polyethylene powder 1.0 (2) Dimethylpolysiloxane 4.0 (3 ) Lanolin 6.0 (4) Vaseline 1.0 (5) Liquid paraffin 1.0 (6) Isopropyl myristate 1.0 (7) Preservative 1.5 (8) Fragrance 0.1

Example 14 Loose type face powder A powder component was mixed and pulverized, transferred to a Henschel mixer, added with an oil agent and a fragrance and mixed so as to be uniform.
Through a sieve, a loose type face powder having the following composition was produced. (Composition) (% by weight) (1) Processed powder of Example 8 50.0 (2) Talc balance (3) Bengala 0.1 (4) Liquid paraffin 1.0 (5) Fragrance 0.1

Example 15 Two-Layer Separable Sunscreen Emulsion After dissolving the oil phase at room temperature, a pigment was added and dispersed by a disper. The aqueous phase was added with stirring and emulsified to produce a sunscreen emulsion having the following composition. (Composition) (% by weight) (1) Octamethylcyclotetrasiloxane 25.0 (2) Perfluoropolyether (FOMBLIN HC-04, manufactured by Montefros) 10.0 (3) Dimethylpolysiloxane / polyoxyalkylene Merged 1.0 (4) Glycerin 2.0 (5) Ethanol 12.0 (6) Residual amount of purified water (7) Octyl methoxycinnamate 2.0 (8) Zinc oxide (treated in the same manner as in Example 2) 7.5) (9) Talc (treated in the same manner as in Example 2) 7.0 (10) Perfume

Example 16 Sunscreen cream A homogeneous mixed solution of components 10 and 12 dispersed in component 9 and a component 6 to 8 and components 6 to 8 was added to the aqueous components of components 1 to 5 with stirring to emulsify. A sunscreen cream having the following composition was produced. (Composition) (% by weight) (1) Polyoxyethylene (50) hydrogenated castor oil 0.5 (2) Polyoxyethylene (20) sorbitan palmitate 1.0 (3) Glycerin 6.0 (4) 1, 3 -Butylene glycol 6.0 (5) purified water 15.5 (6) squalane 5.0 (7) jojoba oil 5.0 (8) octamethylcyclotetrasiloxane 18.0 (9) perfluoropolyether (FOMBLIN HC -04, manufactured by Montefros Co., Ltd. 35.0 (10) Titanium oxide (treated in the same manner as in Example 1) 1.0 (11) Talc (treated in the same manner as in Example 1) 5.0 ( 12) Octyl methoxycinnamate 2.0

Example 17 Two-layer separation type liquid foundation After dissolving the oil phase at room temperature, a pigment was added and dispersed with a disper. The aqueous phase was added with stirring and emulsified to produce a liquid foundation having the following composition. (Composition) (% by weight) (1) Pigment (treated in the same manner as in Example 1 and mixed later) • Titanium oxide 6.0 • Sericite 9.0 • Iron oxide (red, yellow, black) 2 (2) Octamethylcyclotetrasiloxane 20.0 (3) Dimethylpolysiloxane (KF-96A, 6cs, manufactured by Shin-Etsu Chemical Co., Ltd.) 2.0 (4) Dimethylpolysiloxane / polyoxyalkylene copolymer 1.0 ( 5) Perfluoropolyether (FOMBLIN HC-04 manufactured by Montefros) 10.0 (6) Glycerin 2.0 (7) Ethanol 15.0 (8) Remaining purified water (9) Appropriate amount of perfume

Each of the cosmetics of the present invention obtained in Examples 10 to 17 was excellent in use feeling and extremely long lasting.

[0073]

EFFECT OF THE INVENTION The water- and oil-repellent cosmetic powder of the present invention is
The cosmetic of the present invention, which is excellent in water repellency and oil repellency and excellent in use feeling, especially excellent in smoothness, and which contains the water repellent and oil repellent cosmetic powder of the present invention, is water-resistant. It has good sebum resistance and oil resistance, is excellent in the effect of preventing makeup collapse due to sebum and the like (makeup persistence), has good elongation on the skin, and has excellent use feeling, particularly excellent smoothness.

Continuation of the front page (51) Int.Cl. ⁷ Identification symbol FI C09K 3/18 104 B01J 13/02 Z (56) References JP-A-3-246211 (JP, A) JP-A-4-91008 (JP, A) (58) Field surveyed (Int. Cl. ⁷ , DB name) A61K 7/00 A61K 7/02 B01J 13/02

Claims (2)

(57) [Claims] 1. A water- and oil-repellent powder obtained by subjecting a powder to a surface treatment with the following agent (a) and then a surface treatment with the following agent (b): (a) agent: general formula (1) )) An alkali metal salt of a zinc monoalkyl or alkenyl phosphate represented by the following formula: [Wherein, A represents an alkali metal. R: represents a linear or branched alkyl group or alkenyl group having 8 to 32 carbon atoms. (B) agent: the following compounds (b-1), (b-2), (b-
One or more compounds selected from the group consisting of 3), (b-4) and (b-5): Compound (b-1): Phosphate represented by general formula (2): [Rf (CH ₂ ) _m O (AO) _n ] _y PO (OM) _3-y (2) [wherein, Rf is a linear or branched perfluoroalkyl group having 6 to 21 carbon atoms or the perfluoroalkyl group. Represents a group in which one of the fluorine atoms has been replaced with a hydrogen atom. A: The same or different and represents an alkylene group having 2 to 3 carbon atoms. M: represents a hydrogen atom, an alkali metal, an ammonium group or a substituted ammonium group. m: Indicates the number of 0 to 12. n: Indicates a number from 0 to 10. y: Indicates the number of 1 to 3. Compound (b-2): an epoxy compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom; (B-3): a silane compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom; 4): a titanium compound having a linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom; compound (b-5): A linear or branched perfluoroalkyl group having 6 or more carbon atoms or a group in which one of the fluorine atoms of the perfluoroalkyl group is substituted with a hydrogen atom A polysiloxane compound having the formula: 2. A cosmetic containing the water- and oil-repellent powder according to claim 1.