JPH06171932A - Fluorine-treated barium sulfate powder and cosmetic containing the same - Google Patents

Abstract

PURPOSE:To enhance the water and oil repellency of BaSO4 powder by subjecting the powder to surface treatment with a fluorine compd. CONSTITUTION:A barium salt soln. having 0.001-0.05mol/l concn. is mixed with a sulfate or sulfuric acid soln. having 0.001-0.05 mol/1 concn. in (1:10)-(5:1) molar ratio so that pH 1.0-5.0 is attained and the resulting mixture is brought into a reaction at 5-100 deg.C to obtain BaSO4 powder having 5-100 ratio of the average diameter of the platy faces to the thickness and 20-150 ratio of the square of the peripheral length of the platy faces to the total area of the platy faces. The objective fluorine-treated BaSO4 powder is obtd. by subjecting 100 pts.wt. of the resulting BaSO4 powder to surface treatment with 0.05-20 pts.wt. fluorine compd. and cosmetics are blended with 0.1-99.9wt.% of the fluorine-treated BaSO4 powder.

Description

Detailed Description of the Invention

[0001]

The present invention relates to a fluorine-treated barium sulfate powder, and the unique feel of barium sulfate is improved. The spread on the skin is good when applied, and the feeling of use is excellent.
In addition, the present invention relates to a cosmetic containing the above-mentioned fluorine-treated barium sulfate powder that is resistant to makeup damage.

[0002]

BACKGROUND OF THE INVENTION Cosmetics containing powder include makeup cosmetics such as foundation, white powder, blusher, eye shadow, eyebrow, body cosmetics such as body powder and baby powder. Is commercially available. These cosmetics are usually
Powder, oil, water, wax and the like are constituent components, and the powder includes inorganic color pigments such as red iron oxide, yellow iron oxide and titanium dioxide; color pigments such as organic pigment color pigments such as aluminum lake, talc, Inorganic pigments such as kaolin, sericite, mica and mica; extender pigments such as organic polyvalent metal salts and organic pigments such as polymer resins are used.

The above cosmetics are required to have a beautiful skin and to impart a feeling of transparency and bareness to the skin to which they have been applied due to the nature of their cosmetic effect. Cosmetic properties such as elongation, smoothness, prevention of collapse due to sweat, and water and oil repellency for preventing darkness due to sebum secreted by the skin and makeup deterioration are also problems.

[0004] In order to meet the above-mentioned demand for beautiful skin, pigments having a high hiding power, that is, pigments having a large refractive index and pigments having a high coloring power, such as titanium dioxide, red iron oxide, iron oxide yellow, and organic pigments have been used. Etc. have been blended as a coloring pigment to enhance the covering power. However, the above-described high hiding power pigments, that is, cosmetics containing a large amount of a high refractive index pigment or a high coloring power pigment, give a thick makeup feeling when applied to the skin, become opaque, and become natural. It has the disadvantage that it loses that feeling.

[0005] On the other hand, in order to give the skin to which the makeup is applied a feeling of transparency and bare skin, it has been customary to mix pigments having a small refractive index such as talc, kaolin, mica and mica as extender pigments into cosmetics. However, the extender pigment has been blended in a large amount in cosmetics because it has a better feeling of use such as elongation and stickiness on the skin than the above-mentioned color pigments. However, when a large amount of the extender pigment is blended, there is a problem in that when applied to the skin, the appearance tends to be shiny and unnatural luster tends to be imparted.

Therefore, the surface of the extender pigment is coated with an inorganic silicic acid compound to form an inorganic silicate compound coated pigment (JP-A-61-228406), and an acrylic resin-coated acrylic resin coated pigment (JP-A-61). -69708
It has been attempted to obtain a transparent feeling, a bare skin feeling, and a natural finish by blending an extender pigment such as Japanese Unexamined Patent Publication (KOKAI) No. 1) with a cosmetic material. However, when a cosmetic containing the above-mentioned clothing extender pigment is applied to the skin, it is possible to give a transparent feeling and a bare skin feeling, but the covering power is insufficient because the pigment itself has a small refractive index. It has drawbacks.

That is, as described above, conventionally used pigments having a high hiding power, that is, a pigment having a large refractive index, a pigment having a high coloring power, an extender pigment, an inorganic silicate compound-coated extender pigment, an acrylic resin-coated extender pigment, etc. In the coated extender of,
It is not possible to satisfy both the provision of transparency and the feeling of bare skin and the coverage of uneven skin color, and it has the drawback that it cannot fully exhibit the original function of cosmetics to finish beautiful skin. .

Therefore, in order to satisfy the above drawbacks at the same time, cosmetics containing barium sulfate have been proposed.
Barium sulfate has a refractive index (1.6) between the refractive index of the coloring pigment (about 2.0) and the refractive index of the extender pigment (about 1.4).
It is a pigment that has 4) and has an appropriate covering power while having a transparent feeling and a bare skin feeling. As a cosmetic material characterized by containing barium sulfate powder, a cosmetic material containing barium sulfate coated with a high refractive index metal oxide (Japanese Patent Publication No. 49-46
No. 908), a cosmetic containing tabular barium sulfate (JP-A-61-129107), a cosmetic containing particulate barium sulfate (JP-A-61-191607), titanium dioxide, zinc white, 25 ° C with a pigment selected from the group consisting of barium sulfate, metallic soap, calcium carbonate, magnesium carbonate, silica and alumina.
Having a viscosity in the range of 100 to 1,000,000 cps in a cosmetic composition (JP-A-61-2100181).
Issue gazette) etc.

However, the barium sulfate powder is characterized by the feel of the body pigments such as talc, kaolin, sericite, mica and mica that are commonly used, that is, it is lightly permeable and spreads well on the skin. Compared with that, the powder itself has a heavy specific gravity and a low bulk specific gravity, which is characteristic of a heavy and moist feel, which makes it possible to improve the cosmetic performance, usability, and feel as a powder cosmetic. Therefore, there is a problem that it has an adverse effect. Further, in the cosmetics containing the conventional barium sulfate powder, since the oil absorption of the barium sulfate powder is small, sweat and sebum secreted from the skin cause the makeup effect to be lost because the makeup effect cannot be maintained. There is a problem.

That is, also in the cosmetics using the conventional barium sulfate powder, the cosmetic performance, usability and feel, particularly lightly permeable, the elongation on the skin is good, and further, sweating, sebum and sebum At present, there is a demand for the development of barium sulfate powder which does not easily collapse and cosmetics containing the powder.

Accordingly, an object of the present invention is to provide a fluorine-treated barium sulfate powder which has a good feel, particularly lightly permeable, good elongation on the skin, a large bulk specific gravity, and excellent water and oil repellency. In addition, it is to provide a cosmetic having an appropriate covering power while having a transparent and bare skin feel, excellent makeup performance, usability, and touch, and extremely excellent water and oil resistance, and which does not easily lose its makeup. .

[0012]

Therefore, the present inventors have
As a result of intensive studies to solve the above problems, the inventors have found that a specific barium sulfate powder can achieve the above object, and have completed the present invention.

That is, the present invention provides a fluorine-treated barium sulfate powder obtained by surface-treating barium sulfate powder with a fluorine compound, and a cosmetic comprising the fluorine-treated barium sulfate powder. It is provided.

The fluorinated barium sulfate powder of the present invention and the cosmetic containing the fluorinated barium sulfate powder will be described in detail below. The fluorine-treated barium sulfate powder of the present invention is obtained by surface-treating barium sulfate with a fluorine compound.

As the barium sulfate powder used in the present invention, any of commercially available barium sulfate powder and synthetically obtained barium sulfate powder can be used. Examples of the commercially available barium sulfate powder include fine particle barium sulfate manufactured by Sakai Chemical Industry, trade name "BF-1", trade name "BF-10", trade name "BF-20", and the like, as well as Sakai Chemical Industry. Examples include plate-shaped barium sulfate and the like. Also,
Examples of the barium sulfate powder obtained by the above synthesis include barium sulfate powder obtained by reacting a barium salt solution with a sulfate or a sulfuric acid solution. In this case, the barium salt that can be used includes those soluble in a solvent such as water or alcohol, such as barium chloride, barium nitrate, barium acetate, barium hydroxide and the like. Examples of sulfates include sulfates soluble in solvents such as water and alcohol, such as sodium sulfate and ammonium sulfate.

As the barium sulfate powder, it is preferable that barium sulfate powder having a plate-like structure has excellent cosmetic properties, usability and feel. The plate-like structure here means that the ratio of the average diameter to the thickness of the plate-like surface is 5 to 100, and the ratio of the square of the perimeter of the plate-like surface to the total area of the plate-like surface is 20 to 150. It is preferable that they are present, and specific examples thereof include a thin plate shape, a thin piece shape, a leaf piece shape, a petal shape, a mica shape, and a foil shape.

Further, in the above reaction, the barium ion concentration of the barium salt solution and the sulfate ion concentration of the sulfate or sulfuric acid solution are each 0.001 to before the reaction.
It is preferably 0.05 mol / liter. If the concentration is less than 0.001 mol / liter, the plate-like structure of the crystal collapses and the columnar structure becomes closer to a columnar shape, resulting in poor usability when used as a cosmetic and a low yield as barium sulfate. Not preferable. Also, 0.05 mol /
If it exceeds liters, the plate-like structure of the crystal collapses to form fine particles, which is unfavorable because the use feeling as a cosmetic material deteriorates. In addition, it is preferable that the molar ratio of the barium salt solution and the sulfate solution at the time of the reaction is 1:10 to 5: 1. The pH during the reaction is
Hydrochloric acid, sulfuric acid, if necessary so as to be 1.0 to 5.0
It is preferable to adjust with nitric acid or the like, and the reaction temperature is usually 5
It is 0 to 100 ° C, preferably 60 to 95 ° C. If the pH and the reaction temperature are out of the above ranges, the plate-like structure of the obtained barium sulfate powder will be broken, and the usability as a cosmetic material will be deteriorated, which is not preferable.

Examples of the fluorine compound used for the surface treatment of the barium sulfate powder include polyfluoroalkyl phosphoric acid represented by the following general formula [Chemical formula 1] (US Pat. No. 3,632,744). In addition to the above, fluoroalkyldi (oxyethyl) amine phosphate (JP-A-62-250074) and a polymer having a fluoroalkyl group (JP-A-55-16720).
No. 9, JP-A-61-55481, JP-A-61.
-48803), fluororesins such as tetrafluoroethylene resin (JP-A-57-38707), fluoroalcohol (JP-A-63-2251, JP-A-63-2351).
No. 2252) Perfluoroepoxy compound, sulfoamide type fluorophosphoric acid, perfluorosulfate, perfluoroalkylsilane (JP-A-1-180070, JP-A-2-218603, JP-A 1-160).
No. 907, JP-A-2-127477), manufactured by Shin-Etsu Silicone Co., Ltd., trade name “LP-1T”, trade name “LP-4T”, trade name “LP-8T”, and other silane coupling agents, Trichlorotrifluoroethane (CFC)
And other fluorine-containing halogenated hydrocarbons (Japanese Patent Laid-Open No. 1-3180)
70), fluoroalkyl-containing polyhydric alcohols,
Fluoroalkyl-containing polyoxyethylene compound (JP-A-1-180810, JP-A-1-180811) Fluoroalkyl-containing sulfamidocarboxylic acid,
Examples thereof include fluorine compounds having a fluorine atom in the molecule such as fluoroalkyl-containing acrylate copolymers (US Pat. No. 3,632,744), but are not limited to these examples.

[0019]

[Chemical 1]

As a method for surface-treating the barium sulfate powder with the fluorine compound, any method such as a dry method and a wet method can be used. The dry method is a simple and effective method, and can be easily performed by stirring and mixing the fluorine compound and the barium sulfate powder with a ball mill or the like. The wet method is, for example,
The fluorine compound is dissolved or dispersed in a medium such as water and / or alcohol, acetone, toluene, hexane, the barium sulfate powder is added thereto, and after stirring treatment, the medium is distilled off or filtered. Then, the barium sulfate powder is coated with a fluorine compound. In this case, the stirring treatment may be carried out under heating, or a reaction aid such as an acid, an alkali or a catalyst may be added if necessary. Further, it is also possible to dissolve or disperse a fluorine compound in a volatile solvent, spray the powder using a flow coater or the like, and coat it.Further, in the case of using a volatile fluorine compound such as CFC, It is also possible to directly contact the vapor of the fluorine compound with the barium sulfate powder for coating.

The ratio of the barium sulfate powder to the fluorine compound used in the surface treatment is preferably 0.05 to 20 parts by weight with respect to 100 parts by weight of the barium sulfate powder. And more preferably 0.5 to 15 parts by weight. If it is less than 0.05 parts by weight, the surface treatment effect is not sufficient, and if it exceeds 20 parts by weight, the treatment effect does not improve so much, which is not preferable from the economical viewpoint.

After the above surface treatment, post-treatments such as baking treatment, heat treatment and aging treatment may be carried out in order to enhance the treatment effect as long as the effect of the present invention is not impaired. Further, as a pretreatment, the powder may be subjected to firing treatment, heat treatment, hydrothermal treatment, depressurization treatment, plasma treatment or the like as required.

In the surface treatment, two or more kinds of the above powders may be mixed and used at the same time. Further, within a range that does not impair the effects of the present invention, silicones other than fluorine compounds, higher fatty acids and their metal salts, higher alcohols,
Amino acids such as esters, waxes, acylglutamic acid, N-mono long-chain acyl basic amino acids and metal salts thereof,
It may be simultaneously or doubly treated with other known coating agents such as hydrogenated lecithin, polyethylene, polyacrylic acid, acylated collagen, alkyl phosphate, triglyceride, diglyceride, silica, alumina, alumina silica and titania. . Further, the fluorine compound is
One type or a combination of two or more types can be used.

The fluorine-treated barium sulfate powder of the present invention obtained by the above surface treatment has an improved unique feel of barium sulfate, has good spreadability on the skin when applied, and is excellent in use feeling. Moreover, it is difficult for the makeup to come off. Therefore, excellent cosmetics can be obtained by using this.

The cosmetic of the present invention is characterized by containing the above-mentioned fluorine-treated barium sulfate powder. The amount of the fluorine-treated barium sulfate powder blended in the cosmetic of the present invention is arbitrarily selected according to the properties of the cosmetic, but is preferably 0.1 to 99 in the total composition of the cosmetic of the present invention. 1.9 wt%, more preferably 5 to 95 wt%.

In the cosmetic of the present invention, in addition to the fluorine compound-treated barium sulfate powder, which is the above-mentioned essential component, it is optionally blended in a usual cosmetic within a range that does not impair the effects of the present invention. Ingredients such as liquid oil, solid fat (wax) or semi-solid fat, various surfactants, various powders, water-soluble polymer, oil-soluble polymer, polymer latex, antioxidant, preservative, drug, dye , A fragrance, a moisturizer, an ultraviolet absorber, a thickener, a pH adjuster, water and the like can be added.

Examples of the above-mentioned liquid oil to be blended as necessary include liquid hydrocarbon oils such as liquid paraffin, squalane, and squalene; cottonseed oil, sesame oil, linseed oil, sunflower oil, soybean oil, safflower oil, castor oil. Vegetable oils such as oil, avocado oil, camellia oil, macadamia nut oil, olive oil, jojoba oil and coconut oil; higher fatty acids such as lauric acid, oleic acid and isostearic acid; higher alcohols such as cetanol, hexadecyl alcohol and oleyl alcohol; 2- Cetyl ethylhexanoate, di-2-ethylhexyl, 2-octyldodecyl myristate, di-2-
Neopentyl glycol ethylhexanoate, tri-2-
Esters such as glycerol ethylhexanoate, 2-octyldodecyl oleate, isopropyl myristate, glycerol triisostearate, diglyceride 2-ethylhexanoate, di-paramethoxycinnamic acid-mono-2-ethylhexanoate glyceryl; dimethyl Silicon oil such as polysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, octamethylcyclotetrasiloxane; perfluorodecalin, perfluoroadamantane, perfluorobutyltetrahydrofuran, perfluorooctane, perfluorononane, perfluoropentane Liquid oils commonly used in cosmetics such as fluorine-based oils such as perfluorodecane, perfluorododecane, and perfluoropolyether are used.

Examples of the above-mentioned solid fat or semi-solid fat blended as necessary include petrolatum, lanolin, paraffin wax, beeswax, carnauba wax, ceresin, microcrystalline wax, candelilla wax, and acrylate ester containing fluoroalkyl. Solid fats or semi-solid fats commonly used in cosmetics such as copolymers are used.

Examples of the above-mentioned surface-active agent to be blended as necessary include polyoxyethylene alkyl ether,
Nonionic surfactants such as polyoxyethylene fatty acid ester, polyoxyethylene sorbitan fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene hydrogenated castor oil, polyoxyethylene sorbitol fatty acid ester, etc. Anionic surfactants represented by fatty acid soaps such as sodium stearate and triethanolamine palmitate; and surfactants commonly used in cosmetics such as cationic surfactants and amphoteric surfactants are used.

Examples of the above water-soluble polymer that is blended as necessary include carboxymethyl cellulose, methyl cellulose, hydroxymethyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, tragacanth gum,
Carrageenan, locust bean gum, dextrin,
Water-soluble polymers commonly used in cosmetics such as dextrin fatty acid ester, carboxyvinyl polymer, xanthan gum, gelatin, sodium alginate, and gum arabic are used.

Examples of the moisturizers to be added as needed include sorbitol, xylitol, glycerin,
Moisturizers commonly used in cosmetics such as maltitol, propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, sodium pyrrolidonecarboxylate, lactic acid, sodium lactate and polyethylene glycol are used.

As the above-mentioned preservatives to be blended as necessary, for example, preservatives commonly used in cosmetics such as paraoxybenzoic acid alkyl ester, sodium benzoate, potassium sorbate and the like are used. As the above-mentioned drug to be blended as needed, for example, drugs commonly used in cosmetics such as vitamins, crude drugs, antiphlogistics and bactericides are used. Examples of the ultraviolet absorber that is blended as required include cosmetics such as para-aminobenzoic acid type ultraviolet absorbers, anthranyl type ultraviolet absorbers, salicylic acid type ultraviolet absorbers, cinnamic acid type ultraviolet absorbers, and benzophenone type ultraviolet absorbers. An ultraviolet absorber commonly used for is used.

Examples of the above-mentioned various powders to be blended as needed include talc, mica, sericite, kaolin, bentonite, vermiculite, hectorite,
Zeolite, aluminum oxide, hydrite, aluminum hydroxide, muscovite, synthetic mica, phlogopite, phlogopite, biotite, lithia mica, magnesium carbonate, calcium carbonate, diatomaceous earth, calcium silicate, magnesium silicate, aluminum silicate, barium silicate, Inorganic powder such as strontium silicate, magnesium aluminum silicate, hydrous silicic acid, silicic acid anhydride, metal tungstate, hydroxyapatite, magnesium oxide, ceramics powder, barium sulfate, boron nitride, barium sulfate treated mica; nylon powder, polymethylmethacrylate powder , Polyethylene powder, polystyrene powder, benzoguanamine powder, silicone resin powder, fluororesin powder, microcrystalline cellulose powder, silk powder,
Organic powders of rice starch, Nε-lauroyl-L-lysine, etc .; fatty acid polyvalent metal salts (eg calcium stearate, zinc stearate, magnesium stearate, magnesium myristate etc.) alkyl phosphate polyvalent metal salts (eg monoalkyl Zinc phosphate, calcium cetyl phosphate, zinc sodium cetyl phosphate, etc.), amidosulfonic acid polyvalent metal salt, acylated amino acid polyvalent metal salt (N-
Surfactant polyvalent metal salt powder such as laluloyl-β-alanine calcium salt; inorganic white pigment such as titanium oxide, zinc oxide, zirconium oxide; inorganic red pigment such as iron oxide (red iron oxide), iron titanate, calamine Pigments: Inorganic yellow pigments such as iron hydroxide, γ-iron oxide and loess; Inorganic black pigments such as black iron oxide, carbon black and low order titanium oxide; Inorganic blue pigments such as mango violet, cobalt violet, ultramarine and navy blue Inorganic green pigments such as chromium oxide, chromium hydroxide, cobalt titanium; titanium oxide coated mica, titanium oxide coated bismuth oxychloride, bismuth oxychloride, titanium oxide coated talc, fish scale foil, colored titanium oxide coated mica, etc. Pearl pigment;
Metal powders such as aluminum powders, stainless powders, and copper powders; powders commonly used in cosmetics such as fine particle titanium oxide, fine particle zinc oxide, flaky zinc oxide, fine particle zirconium oxide, fine particle cerium oxide, and other UV protection powders. To be

Examples of the above-mentioned dyes to be blended as necessary include Red No. 3, Red No. 104, Red No. 106, Red No. 201, Red No. 202, Red No. 203, Red No. 204.
No., Red 205, Red 213, Red 219, Red 220, Red 226, Red 227, Red 228
No., Red 230, Red 401, Red 405, Red 505, Yellow 4, Yellow 5, Yellow 202, Yellow 2
03, Yellow 204, Yellow 205, Yellow 401,
Blue No. 1, Blue No. 2, Blue No. 201, Blue No. 404, Green No. 3, Green No. 201, Green No. 204, Green No. 205,
Orange 201, Orange 203, Orange 204, Orange 20
Tar dyes such as No. 5, Orange 206, Orange 207; β
-Carotene, annatto, crocin, capsanthin, shisonin, hibiscus dye, grapeskin extract, safrole yellow, cocoa dye, riboflavin,
Riboflavin butyrate, carminic acid, laccaic acid, chlorophyll, curcumin, betanin, red yeast rice pigment,
Various powders and pigments commonly used in cosmetics such as natural pigments such as brasilin and caramel are used.

The above-mentioned various powders and dyes can be used as they are, but they are inorganic treatment agents such as silica treatment, alumina treatment, silica-alumina treatment, titania treatment and barium sulfate treatment, or silicone treatment, high-grade treatment. Fatty acid and its metal soap treatment, higher alcohol treatment, ester treatment, wax treatment, acylglutamic acid, amino acid treatment such as N-mono long-chain acyl basic amino acid, hydrogenated lecithin and lecithin treatment, acylated collagen treatment, polyethylene treatment, poly Surface treatment with one or a combination of two or more organic treatment agents such as acrylic acid treatment, alkyl phosphate ester treatment, alkyl phosphate metal salt treatment, and treatment with a treatment agent containing a perfluoroalkyl group in the molecule. The various powders and dyes mentioned above can also be used.

Examples of the cosmetics of the present invention include liquid foundations, cream foundations, oil foundations, powder foundations, powder white powders, solid white powders, blushers, eye shadows, lipsticks, eye liners, and other makeup cosmetics and emulsions and creams. The basic cosmetics, medicated cosmetics such as sunscreens, and external medicines such as anti-inflammatory agents and skin protectants can be mentioned,
The form can be widely applied such as powder, cake, emulsion, oil, gel and the like. The cosmetic of the present invention can be produced by a conventional method except that the above-mentioned fluorine-treated barium sulfate powder is blended.

[0037]

The present invention will be described in more detail with reference to examples, but the present invention is not limited thereto. The blending amounts are all weight%.

[0038]

Example 1 150 g of barium sulfate powder was placed in a round bottom flask (or kneader) and heated to 60 ° C. while mixing. In addition, (C ₆ F ₁₃ CH ₂ CH ₂ O) ₂
13 g of P (O) OH and 1500 g of isopropyl ether
Dissolve and warm (50 ℃) to each, add 60
The mixture was mixed at 4 ° C with stirring for 4 hours. Then, isopropyl ether was distilled off under reduced pressure at 50 to 60 ° C. for surface treatment, and after drying, 157 g of the target fluorinated barium sulfate powder was obtained. The obtained fluorine-treated barium sulfate powder was tested for water repellency, oil repellency, bulk specific gravity, and feel as shown below. The results are shown in [Table 1].

(Water repellency evaluation method) About 0.05 g of the obtained fluorine-treated barium sulfate powder was floated in a 30 ml beaker containing 15 ml of water, and the beaker was shaken to observe the dispersibility of the powder in water. did. The evaluation was based on the following 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 white after 1 minute, but floating powder was also seen. 3: When the beaker was shaken, the water became cloudy after 1 minute, but there were many floating powders. 4: When the beaker was shaken, water did not turn cloudy after 1 minute, and dispersed powder was not recognized. Even if the beaker was shaken for 5 minutes or longer, no powder dispersed in water was observed.

(Evaluation method of oil repellency) About 0.05 g of the obtained fluorine-treated barium sulfate powder was placed on a beaker for 30 ml containing 15 ml of squalane, and the beaker was shaken to disperse the powder in the squalane. I observed. The evaluation was based on the following criteria. 0: Powder immediately dispersed in squalane. 1: When the beaker was shaken, the powder was mostly dispersed in squalane within 30 seconds. 2: When the beaker was shaken, squalane became white and cloudy after 1 minute, but floating powder was also seen. 3: When the beaker was shaken, the squalane became cloudy white after 1 minute, but there were also many floating powders. 4: When the beaker was shaken, the squalane did not turn white after 1 minute and no dispersed powder was observed. Even if the beaker was shaken for 5 minutes or longer, no powder dispersed in squalane was observed.

(Measurement of Bulk Specific Gravity) 10 g of the obtained fluorine-treated barium sulfate powder was weighed into a settling tube, shaken sufficiently, and tapped lightly to measure the volume of the powder at that time.

(Feeling evaluation method) The dry feeling of the fluorine-treated barium sulfate powder obtained by five professional panelists,
The feeling of elongation and the like was evaluated on the basis of the following five grades from 1 to 5, and the average value was shown. The feel of untreated powder of plate-shaped barium sulfate H (manufactured by Sakai Chemical Industry Co., Ltd.) having an average particle size of 5 μ was set to a standard value of 3.0. 1: Feeling such as dry feeling is poor 2: Feeling such as smooth feeling is slightly poor 3: Normal (equivalent to plate-shaped barium sulfate H) 4: Fairly feeling such as smooth feeling stretch 5: Smooth feeling, etc. Feels good

[0043]

Example 2 150 g of barium sulfate powder was placed in a round bottom flask (or kneader) and heated to 60 ° C. while mixing. In addition, (C ₈ F ₁₇ CH ₂ CH ₂ O) ₂
17 g of P (O) OH is added to isopropyl alcohol 1500
What was dissolved and heated (50 ° C) was added to each g, and 6
The mixture was stirred and mixed at 0 ° C. for 4 hours. After that, isopropyl alcohol is distilled off under reduced pressure at 50 to 60 ° C. for surface treatment, and after drying, the target fluorinated barium sulfate powder 161
g was obtained. The same test as in Example 1 was conducted on the obtained fluorine-treated barium sulfate powder. The results are shown in [Table 1].

[0044]

Example 3 150 g of barium sulfate powder and 7.5 g of N-lauroyl lysine were placed in a Henschel mixer and stirred for 10 minutes for surface treatment to obtain 155 g of N-lauroyl lysine treated barium sulfate powder. Next obtained N
155 g of barium sulfate powder treated with lauroyl lysine was placed in a round bottom flask (or a kneader), and ₁₇ g of (C ₈ F ₁₇ CH ₂ CH ₂ O) ₂ P (O) OH was dissolved in 1500 g of isopropyl ether in advance. (50 ° C.) that had been added before, and the mixture was stirred and mixed at 60 ° C. for 4 hours.
After that, isopropyl ether was distilled off under reduced pressure at 50 to 60 ° C. for surface treatment, and after drying, 160 g of the target fluorinated barium sulfate powder was obtained. The same test as in Example 1 was conducted on the obtained fluorine-treated barium sulfate powder. The results are shown in [Table 1].

[0045]

Example 4 50 g of barium sulfate powder is placed in a round bottom flask (or kneader). Ethanol 2 in advance
After dissolving 50 g of calcium chloride in 500 g, N-
A solution in which 2.5 g of lauroyl lysine is dissolved is added and mixed with stirring at room temperature for 2 hours. Next, this was filtered, washed with water to remove calcium chloride, and then dried to obtain 51 g of N-lauroyl lysine-treated barium sulfate powder. Next obtained N
51 g of barium sulphate powder treated with lauroyl lysine was placed in a round bottom flask (or kneader) and charged with (C ₆ F ₁₃
CH ₂ CH ₂ O) ₂ P (O) OH and (C ₈ F ₁₇ CH ₂ CH ₂ O)
2.5 g of a 1: 1 mixture with ₂ P (O) OH was dissolved in 500 g of isopropyl alcohol and heated (50 ° C.), and the mixture was stirred and mixed at 60 ° C. for 4 hours. Then, isopropyl alcohol was distilled off under reduced pressure at 50 to 60 ° C. for surface treatment, and after drying, 52 g of the target fluorinated barium sulfate powder was obtained. The same test as in Example 1 was conducted on the obtained fluorine-treated barium sulfate powder.
The results are shown in [Table 1].

[0046]

Example 5 150 g of barium sulfate powder and 7.5 g of N-lauroyl lysine were placed in a Henschel mixer and stirred for 10 minutes for surface treatment to obtain 156 g of N-lauroyl lysine-treated barium sulfate powder. Next obtained N
-Lauroyl lysine-treated barium sulfate powder 156 g was placed in a round bottom flask (or kneader), and (C ₈ F ₁₇ CH ₂ CH ₂ O) ₂ P (O) ONa (commercial product name: Asahi Guard AG530 Asahi Glass ( Made) 17g
What was dissolved in 1500 g of water and heated (50 ° C.) was added, and the mixture was stirred and mixed at 60 ° C. for 4 hours. Then 50
After filtering at -60 ° C or normal temperature, further washing with water on a funnel, and drying, the target fluorinated barium sulfate powder 158
g was obtained. The same test as in Example 1 was conducted on the obtained fluorine-treated barium sulfate powder. The results are shown in [Table 1].

[0047]

[Comparative Example 1] 150 g of barium sulfate powder and 7.5 g of N-lauroyl lysine were placed in a Henshol mixer to obtain 10 parts.
The mixture was stirred and mixed for 1 minute to carry out a surface treatment to obtain 155 g of a target N-lauroyl lysine treated barium sulfate powder. The obtained N-lauroyl lysine-coated barium sulfate powder was subjected to the same test as in Example 1. The results are shown in [Table 1].
Shown in.

[0048]

Comparative Example 2 50 g of barium sulfate powder (produced by Sakai Chemical Industry Co., Ltd.) is placed in a round bottom flask (or kneader). In advance, 2500 g of ethanol and 50 of calcium chloride
After dissolving g, 2.5 g of N-lauroyl lysine was added and the mixture was stirred and mixed at room temperature for 2 hours. Next, this was filtered, washed with water to remove calcium chloride, and then dried to obtain 51 g of the target N-lauroyl lysine-treated barium sulfate powder. The obtained N-lauroyl lysine-coated barium sulfate powder was subjected to the same test as in Example 1. The results are shown in [Table 1].

[0049]

[Table 1]

As is clear from Table 1, the fluorine-treated barium sulfate powder of the present invention has a repellent property when compared with untreated plate-shaped barium sulfate powder and N-lauroyl lysine-coated barium sulfate powder. It can be seen that the water / oil repellency, feel and bulk specific gravity are excellent.

[0051]

[Examples 6 and 7 and Comparative Examples 3 and 4] Pressed face powders having the formulations shown in [Table 2] were produced according to the following production methods, and the feeling of use and the feeling of finish were evaluated according to the following evaluation methods. The results are shown in [Table 3].

[0052]

[Table 2]

(Production method) Powder components (1) to (6) are mixed and pulverized. Transfer this to a Henschel mixer, oil layer component (7),
(8) was added and mixed uniformly. Ingredient (9) was added to this mixture and mixed, then pulverized again and passed through a sieve. This was press-molded on a gold plate to obtain a product.

(Evaluation method) Evaluation is conducted by an in-house specialized panel 1
About 6 items, the following items 1 to 4 were compared with Comparative Examples 3 and 4 by 6 persons, and Examples 6 and 7 were performed.
Was evaluated, and the average score of the evaluations of 16 panelists was obtained. Item 1: Usability Item 2: Feel of bare skin (transparency) Item 3: Feel of cosmetics Item 4: Difficulty in putting off makeup (Evaluation criteria) 4 points: Particularly excellent 3 points: Excellent 2 points: Normal 1 point: inferior 0 point: extremely inferior

[0055]

[Table 3]

As is clear from Table 3, in comparison with Comparative Examples 3 and 4, when the cosmetics of Examples 6 and 7 of the present invention were applied to the skin, the blended fluorine-treated barium sulfate powder was used. It is an excellent face powder that does not exist in conventional cosmetics, such as a feeling, especially a feeling of lightly flowing and spreading on the skin, excellent in water repellency and oil repellency, making it difficult to lose makeup. understood.

[0057]

Example 8 A powder foundation having the composition shown in [Table 4] was prepared according to the following production method.

[0058]

[Table 4]

(Production Method) Powder components (1) to (7) were mixed and pulverized. Transfer this to a Henschel mixer, oil layer component (8) ~
(10) was added and mixed uniformly. Ingredient (11) was added to this mixture, mixed, and then ground again and passed through a sieve. This was press-molded on a gold plate to obtain a product.

[0060]

Example 9 A powder screen having the composition shown in [Table 5] was prepared according to the following production method.

[0061]

[Table 5]

(Production Method) Powder components (1) to (8) were mixed and pulverized. Transfer this to a Henschel mixer, and further add ingredient (9),
(10) was added and mixed uniformly. This mixture was ground and passed through a sieve to obtain a product.

[0063]

Example 10

A creamy foundation having the composition shown in [Table 6] was prepared according to the following production method.

[0065]

[Table 6]

(Production Method) Powder components (11) to (14) were mixed and pulverized. Separately, prepare a solution in which the aqueous phase components (7) to (10) are mixed,
The pulverized pigment was added and dispersed, and then heated to 75 ° C.
A mixture of the oil phase components (1) to (6) heated and dissolved at 80 ° C. was added to the previously prepared aqueous phase with stirring to emulsify. This was cooled with stirring, the component (15) was added at 50 ° C., and the mixture was cooled with stirring to obtain a product.

[0067]

Example 11 A blusher was prepared with the composition shown in [Table 7] according to the following production method.

[0068]

[Table 7]

(Production method) Powder components (1) to (7) were mixed and pulverized. Transfer this to a Henschel mixer, oil layer component (8) ~
(10) was added and mixed uniformly. The mixture was ground again and passed through a sieve. This was press-molded on a gold plate to obtain a product.

[0070]

[Example 12]

An eye shadow having the composition shown in [Table 8] was prepared according to the following production method.

[0072]

[Table 8]

(Production Method) Powder components (1) to (7) were mixed and pulverized. Transfer this to a Henschel mixer, oil layer component (8) ~
(10) was added and mixed uniformly. The mixture was ground again and passed through a sieve. This was press-molded on a gold plate to obtain a product.

[0074]

Example 13 A lipstick having the composition shown in [Table 9] was prepared according to the following production method.

[0075]

[Table 9]

(Production Method) Powder components (7) to (14) were heated and melted and uniformly mixed. Components (1) to (6) are added to this, and the mixture is kneaded in a roll mill and uniformly dispersed, and then remelted to prepare components (15) to (6).
(17) is added and degassed, then poured into a mold and rapidly cooled to solidify.
Remove the solid from the mold and fill the container. Then, in order to arrange the appearance of the stick, it is passed through a flame and the surface is made uniform.

[0077]

Example 14 An eyeliner having the composition shown in [Table 10] was prepared according to the following production method.

[0078]

[Table 10]

(Production Method) The component (6) was added to a part of the component (5), and the mixture was dispersed and gelled through a colloid mill. on the other hand,
Ingredients (1) to (4) and (10) are mixed, heated and dissolved, components (7) to (9) are added, cooled and kneaded with a roll mill, and heated again to be melted, Bentonite gel and the remaining component (5) were added, and the mixture was cooled with stirring.

[0080]

Example 15 An O / W cream having the composition shown in [Table 11] was prepared according to the following production method.

[0081]

[Table 11]

(Manufacturing method) Components (8), (10), (12) and (13) were mixed by stirring and kept at 80 ° C. The other components were mixed, heated and dissolved to 80 ° C. The above-mentioned water phase part was added to this oil phase part to pre-emulsify and homogenize with a homomixer.
The product was obtained by cooling to 0 ° C.

When all of the cosmetics obtained in Examples 8 to 15 were applied to the skin, they were made to feel by the compounded barium sulfate coated with a fluorine compound, and in particular, they were exposed to light air to give a good spreadability on the skin. It was extremely good, which was not found in conventional cosmetics, such as longevity, excellent water and oil repellency, and difficulty in losing makeup.

[0084]

INDUSTRIAL APPLICABILITY According to the present invention, a fluorine-treated barium sulfate powder which is excellent in touch, particularly lightly dryness, has good elongation on the skin, has a large bulk specific gravity, and is excellent in water and oil repellency. And a transparent and bare skin feeling, while having an appropriate covering power, excellent in cosmetic performance, usability, and touch, and having extremely excellent water and oil resistance, it is possible to provide a cosmetic that does not easily lose its makeup.

Claims (2)

[Claims] 1. A fluorine-treated barium sulfate powder obtained by surface-treating barium sulfate powder with a fluorine compound. 2. A cosmetic comprising the fluorine-treated barium sulfate powder according to claim 1.