JP2000264824A - Ultraviolet-screening cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject cosmetic which is excellent in water-resistance, safety, and redispersibility of the pigment with time, producible at low cost, and useful as a sunscreen preparation by including a specific microparticulate metal oxide in a specific amount, water, etc., and substantially no surfactant. SOLUTION: This cosmetic is obtained by including (A) 1-30 wt.% of a microparticulate metal oxide with a mean particle size of 5-50 nm surface- treated with a silane compound containing a 6-20C alkyl group and a reactive group, (B) preferably 1-50 wt.% of a cyclic silicone such as decamethylcyclopentasiloxane and (C) preferably 0.5-50 wt.% of water, and substantially no surfactant. The component A is obtained by, for example, mixing a silane compound such as octyltriethoxysilane with a microparticulate metal oxide such as titanium dioxide in an organic solvent such as n-hexane followed by removing the organic solvent and also doing a heat treatment.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is substantially free of surfactants, has excellent water resistance, has excellent redispersibility of pigment over time, has higher safety, and can be produced at low cost. A possible UV protection cosmetic.

[0002]

2. Description of the Related Art Many sunscreen agents containing titanium oxide or zinc oxide surface-treated with a silicone compound have been developed. In particular, recently, products having a high compounding ratio such that the compounding ratio of these pigment components exceeds 25% have been observed. On the other hand, these pigments are easy to cake in the formulation, and have a problem that they are agglomerated at the time of use or harden at the bottom of the container and do not redisperse.To prevent this, add a surfactant to the product to prevent this. It is common to mix.

[0003]

However, these sunscreen agents have a problem that the water resistance of the preparation itself is lowered by water or sweat. That is, an object of the present invention is to provide an ultraviolet protection cosmetic which is excellent in water resistance, excellent in redispersibility of a pigment over time, safer, and inexpensive to produce.

[0004]

Means for Solving the Problems The present inventors have studied a method of uniformly and inexpensively treating the surface of a powder with a silane compound having an alkyl group and a reactive group instead of a silicone compound. Have been. As a result, it has been found that when fine metal oxide particles surface-treated with a silane compound having an alkyl group and a reactive group are used, caking of the pigment hardly occurs even without the addition of a surfactant, and redispersion is easy. Was. And it discovered that the water resistance of a formulation can be improved by not using a surfactant. Furthermore, it was also found that the safety could be increased because no surfactant was added.

That is, the first aspect of the present invention relates to
0 to 30% by weight of a fine particle metal oxide having an average particle diameter in the range of 5 to 50 nm surface-treated with a silane compound having an alkyl group and a reactive group of 0, a cyclic silicone, and water. The present invention relates to an ultraviolet protection cosmetic, which is substantially free of a surfactant.

According to a second aspect of the present invention, there is provided a fine metal oxide having an average particle diameter of 5 to 50 nm, which is surface-treated with a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group. The present invention relates to an ultraviolet protection cosmetic comprising 30% by weight, a cyclic silicone, and water, containing substantially no surfactant, and having a non-uniform appearance and a multilayer separation type.

A third aspect of the present invention comprises substantially only a water-repellent pigment, of which the surface is treated with a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group. It is characterized in that the cosmetic contains 1 to 30% by weight of a fine particle metal oxide having an average particle diameter in the range of 5 to 50 nm, a cyclic silicone, and water, and contains substantially no surfactant. And a UV protective cosmetic.

A fourth invention relates to the above ultraviolet protection cosmetic, wherein at least one alkyl group of the silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group is an octyl group. .

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION The silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group used in the present invention refers to an alkyl group having 6 to 20 carbon atoms and a reactive atom such as a halogen atom or an alkoxy group. Silane compounds such as an alkylsilane compound having a group and an alkylsilazane compound. Preferred silane compounds include silane compounds represented by the following general formula. RR ¹ nSiX _{3-n wherein} n is an integer of 0 to 2, and R is an alkyl group having 6 to 20 carbon atoms (which may be linear or branched). R ¹ represents an alkyl group having 1 to 6 carbon atoms, and X is selected from a halogen atom and a reactive group such as an alkoxy group. Examples of particularly preferred silane compounds used in the present invention are silane compounds in which at least one alkyl group of a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group is an octyl group, and more preferably. , R is an octyl group, n is 0, and X is an ethoxy group. This silane compound can be easily treated uniformly,
In addition, it is preferable because it is easy to supply and inexpensive in terms of cost, and has excellent characteristics such as redispersibility when blended into a product.

In the present invention, the fine particle metal oxide surface-treated with a silane compound needs to have an average particle size in the range of 5 to 50 nm. If it is less than 5 nm, the activity of the powder is high and the agglomeration is strong, so that the powder often behaves substantially as secondary particles having a particle diameter larger than the applicable range of the present invention. On the other hand, if it exceeds 50 nm, an optical problem may occur such that the preparation tends to be opaque at the time of bathing or the like. As a treatment method with the silane compound, n-hexane, cyclohexane, a silane compound and a fine particle metal oxide are mixed in an organic solvent such as a lower alcohol, and optionally finely pulverized, and then the organic solvent is heated or reduced in pressure. Removed and optionally 100-18
A method in which a silane compound is chemically reacted with a reactive group on the surface of the fine particle metal oxide by, for example, a method of performing heat treatment at 0 ° C.

The fine metal oxide used in the present invention includes titanium dioxide, low titanium oxide, zinc oxide, silicon dioxide (silicic anhydride), aluminum oxide, zirconium oxide, iron oxide, tungsten oxide, cerium oxide and the like. However, titanium dioxide or zinc oxide having an excellent ultraviolet protection effect is most preferable. The crystal forms of these powders are not particularly limited, and any of titanium dioxide, such as rutile, anatase, and amorphous, may be used. Furthermore, regarding the shape of these powders,
Examples include a spherical shape, a rod shape, a spindle shape, a needle shape, and an irregular shape, but any shape can be used as long as the average particle size is within the above range.

In the present invention, a fine particle metal oxide surface-treated with a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group and having an average particle diameter in the range of 5 to 50 nm is used as a UV protective cosmetic. Must be contained in an amount of 1 to 30% by weight based on the total amount of If the amount is less than 1% by weight, it is difficult to secure the redistribution of the pigment under the condition that no surfactant is used, and if it exceeds 30% by weight, the viscosity of the preparation becomes too high and the usability deteriorates. is there.

In the present invention, various powders can be used in addition to the fine metal oxide particles. For example, Red No. 104, Red No. 201, Yellow No. 4, Blue No. 1, Black No. 4
No. 01, etc., yellow No. 4 Al lake, yellow No. 203 B
Lake pigments such as a lake, nylon (registered trademark) powder, silk powder, urethane powder, Teflon (registered trademark) powder, silicone powder, polymethyl methacrylate powder, cellulose powder, silicone elastomer spherical powder, polyethylene powder, polypropylene powder Polymer powders such as yellow iron oxide, red iron oxide, black iron oxide, chromium oxide, carbon black, ultramarine,
Colored pigments such as navy blue, white pigments such as zinc oxide, titanium oxide and cerium oxide, extender pigments such as talc, mica, sericite, kaolin and barium sulfate, pearl pigments such as titanium mica, barium sulfate, calcium carbonate, Metal salts such as magnesium carbonate, aluminum silicate, and magnesium silicate; inorganic powders such as silica and alumina; bentonite, smectite, and boron nitride. The shape of these powders (spherical, rod, needle, plate, irregular, scaly,
There is no particular limitation on the spindle shape. These powders are conventionally known surface treatments, for example, fluorine compound treatment, silicone treatment, silicone resin treatment, pendant treatment, silane coupling agent treatment, titanium coupling agent treatment, oil agent treatment, N-acylated lysine treatment, It may or may not have been surface-treated in advance by polyacrylic acid treatment, metal soap treatment, amino acid treatment, inorganic compound treatment, plasma treatment, mechanochemical treatment, etc. In order to prevent caking, it is preferable that all powders to be blended are basically non-hydrophilic. For hydrophilic powder, it is preferable to perform a water-repellent surface treatment, particularly a surface treatment with a silicone compound, for example,
It is preferable that a surface treatment using methyl hydrogen polysiloxane has been performed. Further, among these powders, silicone elastomer spherical powder, polyethylene powder, polypropylene powder, Teflon (registered trademark) powder, silicone rubber powder, urethane powder, polyalkylsilsesquioxane powder, nylon (registered trademark) powder, Spherical powders (including hollow resin powders) such as silica beads, alumina beads, apatite powder, and allylated acrylic beads are preferably blended because they have an excellent effect of improving the feel of the UV protective cosmetic.

[0014] Speaking of UV protection cosmetics,
In recent years, since a high content of powders is generally used, if the amount of hydrophilic powders increases, the viscosity of the preparations increases, causing a problem that the usability deteriorates. Therefore, it is preferable to produce a product using a water-repellent powder that does not easily give a viscosity.

The ultraviolet protective cosmetic of the present invention is characterized in that it contains a cyclic silicone and water as essential components in addition to the above-mentioned components, but contains substantially no surfactant. Examples of the cyclic silicone include a cyclic silicone containing 4 to 6 silicon atoms, and in particular, decamethylcyclopentasiloxane and octamethylcyclotetrasiloxane are preferable. The compounding amount of the cyclic silicone is preferably 1 to 50% by weight based on the total amount of the ultraviolet protection cosmetic.
Although purified water is used as the water, mineral water, purified deep sea water, and the like can also be used. The amount of water is preferably from 0.5 to 50% by weight based on the total amount of the ultraviolet protection cosmetic. The surfactant referred to in the present invention includes compounds having a hydrophilic group and a water-repellent group in one molecule, which are generally recognized as surfactants. Examples of the surfactant include an anionic surfactant, a cationic surfactant, a nonionic surfactant, and a betaine surfactant.

It is preferred from the viewpoint of the object of the present invention that the ultraviolet protective cosmetic of the present invention has a non-uniform appearance and is of a multilayer separation type. Here, the multi-layer separation type refers to a type that separates into multiple layers such as a two-layer separation type, and specifically, a transparent liquid layer and a powder layer in several days to several days under standing conditions. Or a dispersion state in which a powder dispersion layer is further added to these layers. The ultraviolet protection cosmetic of the present invention does not use a surfactant and essentially requires a volatile cyclic silicone. Therefore, unlike the conventional water-in-oil type cosmetic, the ultraviolet protection cosmetic shows a multi-layered appearance over time. Therefore, it is necessary to use the cosmetic of the present invention after shaking it well before use, and it is preferable to put a medium such as beads or balls for stirring in a container. In the present invention, for the purpose of eliminating the redispersion failure due to the caking of the pigment by blending the fine particle metal oxide treated with the silane compound, even if separation occurs in appearance, there is no problem if caking does not occur. .

In the ultraviolet protective cosmetic of the present invention, in addition to the above-mentioned components, oils, fluorine compounds, resins, adhesives, preservatives, fragrances, ultraviolet absorbers (UV-
A or B may be used), moisturizer,
Components such as salts, solvents, antioxidants, chelating agents, neutralizing agents, pH adjusters, insect repellents, and bioactive components can be used.

Examples of the oil include volatile and non-volatile oils, solvents and resins which are usually used in cosmetics, and may be liquids, pastes or solids at room temperature, but liquids excellent in handling are preferred. Examples of oils include, for example, cetyl alcohol, isostearyl alcohol,
Higher alcohols such as lauryl alcohol, hexadecyl alcohol, octyldodecanol, polyhydric alcohols such as glycerin, sorbitol, ethylene glycol, propylene glycol, and polyethylene glycol, myristyl myristate, hexyl laurate, decyl oleate, isopropyl myristate, dimethyl Hexyldecyl octanoate, glyceryl monostearate, diethyl phthalate, ethylene glycol monostearate,
Esters such as octyl oxystearate, liquid paraffin, hydrocarbons such as petrolatum, squalane, lanolin, reduced lanolin, waxes such as carnauba wax, mink oil,
Fats and oils such as cocoa butter, coconut oil, palm kernel oil, camellia oil, sesame oil, castor oil, and olive oil, and ethylene / α-olefin / oligomer.

Examples of other types of oils include dimethylpolysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, alkyl-modified organopolysiloxane, terminal-modified organopolysiloxane, fluorine-modified organopolysiloxane, Examples include silicone compounds such as amino-modified organopolysiloxane, silicone gel and silicone RTV rubber, and fluorine compounds such as perfluoropolyether, pitch fluoride, fluorocarbon, and fluoroalcohol.

Examples of the solvent include ethanol, light liquid isoparaffin, lower alcohol, ethers, LP
G, fluorocarbon, N-methylpyrrolidone, fluoroalcohol, volatile linear silicone, next-generation chlorofluorocarbon and the like.

Examples of the tackifier and resin include trimethylsiloxysilicic acid, sodium polyacrylate, cellulose ether, calcium alginate, carboxyvinyl polymer, ethylene / acrylic acid copolymer, vinylpyrrolidone-based polymer, vinyl alcohol / vinylpyrrolidone Copolymers, nitrogen-substituted acrylamide polymers, polyacrylamides, cationic polymers such as cationized guar gum, dimethylacrylammonium polymers, acrylic acid methacrylic acrylic copolymers, POE / POP copolymers, polyvinyl alcohol, pullulan, agar , Gelatin, tamarind seed polysaccharide, xanthan gum, carrageenan, high methoxyl pectin, low methoxyl pectin, guar gum, gum arabic, crystalline cellulose, arabinogalactan, Rayagamu, tragacanth, alginic acid, albumin, casein, curdlan, gellan gum, dextran, cellulose, polyethyleneimine, highly polymerized polyethylene glycol, cationized silicone polymer, synthetic latex, and the like.

It is preferable that the ultraviolet protective cosmetic composition of the present invention contains various physiologically active ingredients. The physiologically active ingredient includes a substance that gives some physiological activity to the skin when applied to the skin. For example, whitening ingredients, anti-inflammatory agents, anti-aging agents, slimming agents, tightening agents, antioxidants (radical scavengers), humectants, blood circulation promoters, antibacterial agents, bactericides, desiccants, cooling sensations, warmth Agents, vitamins, amino acids, wound healing promoters, stimulants, analgesics, cell activators, skin coloring agents, enzyme components and the like. Among them, natural plant extract components, seaweed extract components, and crude drug components are particularly preferable. In the present invention, these physiologically active components are
It is preferable to mix one or more species.

Examples of these physiologically active ingredients include Ashitaba extract, Avocado extract, Amacha extract, Altea extract, Arnica extract, Aloe extract,
Apricot extract, apricot nucleus extract, ginkgo extract, fennel extract, turmeric extract, oolong tea extract, age extract, echina pear extract, ougon extract, oakaku extract, ouren extract, barley extract, hypericum extract, edulis extract, Dutch mustard extract, orange extract , Seawater dried product, seaweed extract, hydrolyzed elastin, hydrolyzed wheat powder, hydrolyzed silk,
Chamomile extract, carrot extract, kawagomugi extract, licorice extract, calcade extract, syllium extract, kiwi extract, kina extract, cucumber extract, guanosine, gardenia extract, kumazasa extract, clara extract, walnut extract, grapefruit extract, clematis extract, chlorella extract, mulberry extract , Gentian extract, Black tea extract, Yeast extract, Burdock extract, Rice bran extract, Rice germ oil, Comfrey extract, Collagen, Cowberry extract, Psychic extract, Psychoextract, Saitai extract, Salvia extract, Sabonso extract, Sasa extract, Hawthorn Extract, salamander extract,
Shiitake mushroom extract, Japanese radish extract, radish extract, perilla extract, linden extract, sycamore extract, peonies extract, shobu root extract, white birch extract, horsetail extract, swordfish extract, scotch extract, sardine extract, scotch extract, mint extract , Mallow extract, senkyu extract, assembly extract, soybean extract, syllium extract, thyme extract, tea extract, clove extract, cypress extract, chimpanzee extract, touki extract, calendula extract, tonin extract, spruce extract, dokudami extract, tomato extract, natto extract,
Carrot extract, garlic extract, nobara extract, hibiscus extract, Bakmondou extract, parsley extract,
Honey, Hamamelis extract, Parietaria extract, Chikoshii extract, Bisabolol, Loquat extract, Coltsfoot extract, Fukinotou extract, Bucurio extract, Butcher bloom extract, Grape extract, Propolis, Loofah extract, Safflower extract, Peppermint extract, Bodaiju extract, Button extract, Hop extract Extract, pine extract, horse chestnut extract, watermelon extract, mukuroji extract, melissa extract, peach extract, cornflower extract, eucalyptus extract, yukinoshita extract, yuzu extract,
Yokuinin extract, mugwort extract, lavender extract,
Examples include apple extract, lettuce extract, lemon extract, astragalus extract, rose extract, rosemary extract, Roman chamomile extract, royal jelly extract and the like.

Also, biopolymers such as deoxyribonucleic acid, mucopolysaccharide, sodium hyaluronate, sodium chondroitin sulfate, collagen, elastin, chitin, chitosan, hydrolyzed eggshell membranes, amino acids, sarcosine, N
Amino acid derivatives such as -methyl-L-serine, moisturizing components such as sodium lactate, urea, sodium pyrrolidonecarboxylate, betaine, whey, raffinose, sphingolipids, ceramides, cholesterol, cholesterol derivatives, oily components such as phospholipids, ε- Anti-inflammatory agents such as aminocaproic acid, glycyrrhizic acid, β-glycyrrhetinic acid, lysozyme chloride, guaiazulene, hydrocortisone,
Activities of vitamins A, B ₂ , B ₆ , C, D, E, calcium pantothenate, biotin, nicotinamide, vitamin C esters and other vitamins, allantoin, diisopropylamine dichloroacetic acid, 4-aminomethylcyclohexanecarboxylic acid, etc. Ingredients, antioxidants such as tocopherols, carotenoids, flavonoids, tannins, lignans, saponins, cell activators such as α-hydroxy acids, β-hydroxy acids, blood circulation promoters such as γ-oryzanol, vitamin E derivatives, retinol, retinol Wound healing agents such as derivatives, arbutin, kojic acid, placenta extract, sulfur, ellagic acid, linoleic acid, tranexamic acid, whitening agents such as glutathione, cepharanthin, licorice extract, capsicum tincture, hinokitiol, garlic iodide extract, pyridoxine hydrochloride dl-alpha-tocopherol acetate dl-alpha-tocopherol, nicotinic acid, Niochin acid derivatives, calcium pantothenate, D- pantothenyl alcohol, acetyl pantothenyl ethyl ether, biotin, allantoin, isopropylmethylphenol,
Estradiol, ethinylesteradiol, capronium chloride, benzalkonium chloride, diphenhydramine hydrochloride, tacanal, camphor, salicylic acid, nonylate vanillylamide, nonylate vanillylamide, pyrocton olamine, glyceryl pentadecanoate, l-menthol, mononitroguaiacol, resorcinol, γ-aminobutyric acid and the like.

When these physiologically active ingredients are blended into the ultraviolet protection cosmetic, the amount of blending depends on the effective concentration of the active ingredient, but is generally preferably 0.05 to 20% by weight, more preferably. 0.1 to 15% by weight.
In addition, it is preferable to mix | blend 1 type or 2 or more types of biologically active components in combination.

Examples of the ultraviolet absorber include 2-ethylhexyl paramethoxycinnamate and 2-hydroxy-4
-Methoxybenzophenone, 2-hydroxy-4-methoxybenzophenone-5-sulfuric acid, 2,2'-dihydroxy-4-methoxybenzophenone, p-methoxyhydrocinnamic acid diethanolamine salt, paraaminobenzoic acid (hereinafter abbreviated as PABA), Ethyldihydroxypropyl PABA, glyceryl PABA, homomenthyl salicylate, methyl-O-aminobenzoate, 2-ethylhexyl-2-cyano-3,3-diphenylacrylate, octyldimethyl PABA, octyl methoxycinnamate, octyl salicylate, 2-phenyl- Benzimidazole-5-sulfate, triethanolamine salicylate, 3- (4-methylbenzylidene) camphor, 2,4
-Dihydroxybenzophenine, 2,2 ', 4,4'-
Tetrahydroxybenzophenone, 2,2′-dihydroxy-4,4′-dimethoxybenzophenone, 2-hydroxy-4-N-octoxybenzophenone, 4-isopropyldibenzoylmethane, butylmethoxydibenzoylmethane, 4- (3,4 -Dimethoxyphenylmethylene) -2,5-dioxo-1-imidazolidine 2-ethylhexyl propionate, polymer derivatives thereof, and silane derivatives. Further, among these absorbents, those in which 4-tert-butyl-4′-methoxydibenzoylmethane is preferably sealed in a polymer can also be preferably used.

The ultraviolet protective cosmetics of the present invention include sunscreen agents, suntan agents and cosmetic base materials having an ultraviolet protective effect, foundations having an ultraviolet protective effect, and the like.

[0028]

The present invention will be described below in more detail with reference to Examples and Comparative Examples. In addition, methods for evaluating various properties of the ultraviolet protection cosmetics obtained in Examples and Comparative Examples are described below.

[Evaluation of usability] Ten expert panelists are prepared for each evaluation item (however, there is a case where the panelers are duplicated depending on the item), and the panelists actually use the preparation and evaluate according to the following evaluation criteria. Was performed, and the evaluation result was obtained using the total score of all panelists. Therefore, the higher the score, the higher the usefulness for the evaluation item. (Score:
50 points)

Reference score --------------------------------------- It seems to be highly effective 5 Feel the effect 4 Feel the effect a little 3 Feel the effect a little 2 Don't feel the effect 1

[Evaluation of water resistance]
The water resistance of the preparation was evaluated by the in vitro method. That is, the evaluation was performed by evaluating the durability of the coating film of the preparation under running water. (1) Test method Under the following test conditions, after drying the glass plate coated with the preparation, a certain amount of hot water is applied vertically from above the glass plate,
After a certain period of time, the state of the coating film flowing down (water resistance) is examined. The degree of water resistance depends on the application area of the original formulation.
The ratio of the area of the flow-down portion was examined and evaluated according to the following criteria. (2) Test conditions ・ Sample application amount 4mg / cm ²・ Drying conditions 38 ° C for 1 hour ・ Flowing water temperature 37 ° C ・ Flowing water flow rate about 40ml / sec ・ Water pressure The above water amount is perpendicular to the coating film and height is 20cm.・ Test time: 10 minutes

[0032]

Example 1 A sunscreen was obtained based on the following formulation. As the silane-treated fine metal oxide, 10% by weight surface treatment was performed on silica-alumina-treated fine titanium oxide (average particle diameter: 17 nm) using octyltriethoxysilane as an alkylsilane compound and n-hexane as a solvent. What was heat-treated at 160 ° C. was used. Further, silicone-treated fine zinc oxide treated with 5% by weight of silica-treated fine zinc oxide (average particle diameter: 50 nm) with methyl hydrogen polysiloxane was used in combination.

[0034] Ingredient Compounding amount (% by weight) --------------------------------------- --------------------- Component A Silane-treated fine particle titanium oxide 10 Decamethylcyclopentasiloxane (cyclic silicone) Remainder Octamethylcyclotetrasiloxane (cyclic silicone) 15 Component B Silicone-treated fine-particle zinc oxide 20 Octyl paramethoxycinnamate (UV absorber) 10 Trimethylsiloxysilicic acid (50% by weight deca 4 Methylcyclopentasiloxane solution) High polymerization degree dimethyl silicone gum (20% by weight 0.5 deca) Methylcyclopentasiloxane solution) Organopolysiloxane elastomer spherical powder (solid content 35% by weight and 1% kneaded with decamethylcyclopentasiloxane) Dimethylpolysiloxane (10 cs) 2 Component C Hibiscus extract 1 Roeekisu 0.2 Ethanol 0.5 Preservative qs Purified water 20

The silane-treated fine particle metal oxide of Component A and the cyclic silicone were previously ground using a bead mill to obtain a paste. After the component B was mixed well, it was added to the paste of the component A and further mixed. Then, after adding the mixture of the component C, the mixture was filled in a container together with a stainless steel ball for stirring to obtain a product. This product exhibited a multilayer dispersion type appearance, and phase separation occurred between the transparent liquid layer, the powder dispersion layer, and the powder layer over several days. The obtained product was excellent in UV protection effect.

Comparative Example 1 (Example in which no silane-treated fine metal oxide was blended) In place of alkylsilane of the silane-treated fine metal oxide of Example 1, methyl hydrogen polysiloxane 10 was used.
A product was obtained in the same manner as in Example 1 except that the same silica / alumina-treated fine particle titanium oxide was used except that the titanium oxide was coated at a percentage by weight.

Comparative Example 2 (Example in which a surfactant was blended) Instead of 15% by weight of octamethylcyclotetrasiloxane of Example 1, octamethylcyclotetrasiloxane 1 was used.
A product was obtained in the same manner as in Example 1 except that 2% by weight and 3% by weight of a polyether-modified silicone (KF6017 manufactured by Shin-Etsu Chemical Co., Ltd.), which is a type of surfactant, were used.

Comparative Example 3 (Example in which cyclic silicone is not blended) Instead of the cyclic silicone of Example 1, dimethylpolysiloxane (6 cs) was used, and a high degree of polymerization dimethylsilicone gum and cyclic compound in organopolysiloxane elastomer spherical powder were used. A product was obtained in the same manner as in Example 1 except that the respective components prepared using dimethylpolysiloxane (6 cs) instead of silicone were blended.

Comparative Example 4 (Example in which water was not blended) A product was obtained in the same manner as in Example 1 except that dipropylene glycol was blended in place of the purified water of Example 1.

Comparative Example 5 (Example in which no water-repellent pigment is used) Instead of the silane-treated fine particle titanium oxide and the silicon-treated fine particle zinc oxide of Example 1, the corresponding fine particles of titanium oxide and fine particles which have not been subjected to water-repellent treatment, respectively. A product was obtained in the same manner as in Example 1 except that zinc oxide was used.

The results of the usability evaluation and the water resistance evaluation of the above products are shown below.

Easy dispersion of pigment Good feeling of use -------------------------------------- -------------- Example 1 50 48 Comparative Example 1 24 28 Comparative Example 2 43 42 Comparative Example 3 30 10 Comparative Example 4 10 10 Comparative Example 5 10 40

[0043]

From the above results, it was found that the examples of the present invention exhibited superior performance as compared with the comparative examples. Comparative Example 1 was an example in which the silane-treated fine particle metal oxide was not blended, but it can be seen that the pigment settled out, making it difficult to redisperse. Comparative Example 2 was an example in which a surfactant was blended, and it was found that the blending of the surfactant lowered the water resistance. Comparative Example 3 was an example in which no cyclic silicone was used, but the feel was poor and the water resistance was extremely reduced. Comparative Example 4 was an example in which water was not used, but the performance of each evaluation item was inferior. Comparative Example 5 was an example in which the water-repellent pigment was not used. However, not only was re-dispersion not possible due to caking of the pigment, but also the water resistance was poor. Also,
No skin trouble was observed in the samples of the examples of the present invention.

[0045]

From the above, it can be seen that the present invention provides higher safety and water resistance by substantially not containing a surfactant, and the re-generation of pigment over time by blending a silane compound-treated pigment. It is clear that an ultraviolet protective cosmetic characterized by being excellent in dispersibility and being relatively inexpensive to produce can be obtained.

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[Procedure amendment]

[Submission date] April 26, 1999 (1999.4.2
6)

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0009

[Correction method] Change

[Correction contents]

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION The silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group used in the present invention refers to an alkyl group having 6 to 20 carbon atoms and a reactive atom such as a halogen atom or an alkoxy group. Silane compounds such as an alkylsilane compound having a group and an alkylsilazane compound. Preferred silane compounds include silane compounds represented by the following general formula. RR ¹ _n SiX _{3-n wherein} , in the above general formula, n is an integer of 0 to 2, and R is an alkyl group having 6 to 20 carbon atoms (which may be linear or branched. R ¹ represents an alkyl group having 1 to 6 carbon atoms, and X is selected from a halogen atom and a reactive group such as an alkoxy group. Examples of particularly preferred silane compounds used in the present invention are silane compounds in which at least one alkyl group of a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group is an octyl group, and more preferably. , R is an octyl group, n is 0, and X is an ethoxy group. This silane compound can be easily treated uniformly,
In addition, it is preferable because it is easy to supply and inexpensive in terms of cost, and has excellent characteristics such as redispersibility when blended into a product.

 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Hiroaki Ishii 5-28, Kotobukicho, Odawara-shi, Kanagawa Kanebo Co., Ltd. Cosmetics Research Institute F-term (reference) 4C083 AA112 AB051 AB242 AC102 AC342 AD161 AD162 AD172 BB01 BB23 CC19 DD05 EE01 EE09 EE17 4J002 CP001 DE027 DE046 DE106 DE116 DE136 DE146 DJ016 FB096 FD200 GB00

Claims (4)

[Claims] 1. A particulate metal oxide having an average particle diameter in the range of 5 to 50 nm, which is surface-treated with a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group.
An ultraviolet ray protective cosmetic comprising: a weight percent, a cyclic silicone, and water, and substantially free of a surfactant. 2. Fine metal oxide particles having a mean particle diameter in the range of 5 to 50 nm, which have been surface-treated with a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group.
An ultraviolet ray protective cosmetic comprising: a weight percent, a cyclic silicone, and water, substantially free of a surfactant, and having a non-uniform appearance and a multilayer separation type. 3. An ink containing substantially only a pigment which has been subjected to a water-repellent treatment, among which a silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group has an average particle diameter of 5%. The cosmetic according to claim 1, wherein the cosmetic contains 1 to 30% by weight of the fine particle metal oxide in the range of 50 to 50 nm, the cyclic silicone, and water, and is substantially free of a surfactant. Or the ultraviolet protective cosmetic according to 2. 4. The silane compound having an alkyl group having 6 to 20 carbon atoms and a reactive group, wherein at least one alkyl group is an octyl group. UV protection cosmetics.