JP2012121835A - Lipophilically surface treated powder having excellent smooth feeling and detergency - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a lipophilically surface treated powder having excellent smooth feeling and detergency.SOLUTION: The lipophilically surface treated powder is prepared by surface treating an inorganic powder of fine particles of titanium oxide or fine particles of zinc oxide having a primary particle diameter of 5 nm to 150 nm with N-acylamino acid or its salt as a surface treating agent. The surface treating agent of the amount of 0.5 to 30.0 pts.wt. is used for 100 pts.wt. of the inorganic powder. N-acylamino acid is acylamino acid with amino acid selected from 12-20C saturated fatty acid, aspartic acid and glutamic acid. The salt is a salt of a metal selected from Fe, Zn, Ca, Mg, Al, Zr and Ti. The process of surface treatment is performed in the state of under water or the water containing state at a surface treatment temperature of at least 60°C and less than the boiling point of water. A cosmetic material having smooth feeling, detergency, cosmetic effect and cosmetic retainability can be obtained by incorporating the powder.

Description

  The present invention relates to a lipophilic surface-treated fine particle powder excellent in smooth use feeling and detergency, and a method for producing the same, or by using the surface-treated fine particle powder in a dispersed state and using it The present invention relates to a cosmetic that is excellent in feel and cleanability, and that is excellent in makeup effect and makeup persistence.

  Some cosmetics contain organic ultraviolet absorbers and metal oxides such as fine particle titanium oxide and fine particle zinc oxide in order to prevent the harmful effects of sunlight on the skin.

  Sunlight reaching the ground surface is in the wavelength range of 280 nm to 3000 nm, and includes ultraviolet rays, visible rays, and infrared rays. UVA 320nm ~ 380nm, which causes darkening and aging promotion to the skin, erythema of the skin, UVB 290nm ~ 320nm, which causes immediate pigmentation / retarded pigmentation and carcinogenic skin, and ozone layer It is known that there is UVC 200-290 nm that does not reach the ground. Therefore, it is necessary to remove UVA and UVB which adversely affect the skin among the ultraviolet rays.

  Metal oxide powders such as fine particle titanium oxide and fine particle zinc oxide blended in cosmetics are ideally about the optimum particle size for visible light scattering, considering the relationship between particle size and wavelength affecting light scattering. It is preferable to set the optimal particle size of 5 to 100 nm for ultraviolet light scattering far from 200 nm, and to show transparency in the visible region, but to block ultraviolet rays. On the other hand, the smaller the primary particle size of the powder, the stronger the feeling of tightness and the worse the feel of use, and the stronger the cohesion between the particles, the greater the dispersive power required to loosen the aggregated secondary particles. It becomes.

  In addition, since the surface of the metal oxide such as fine particle titanium oxide or fine particle zinc oxide is hydrophilic, there is a problem that when it is used as it is, it has poor adhesion to the skin, and it flows down due to sweat or the like. In order to impart hydrophobicity to the surface, the particle surface is used after being subjected to lipophilic treatment with a surface treatment agent. However, the surface treatment agent covering the surface of the particles greatly affects the feeling of use at the time of applying the cosmetic, cleanability, adhesion to the skin, makeup effect and makeup sustainability. The fine particle powder subjected to lipophilic surface treatment to improve the makeup effect and makeup persistence has a strong feeling of oil and a sticky feeling and tends to deteriorate the cleanability.

In addition, the aggregation state of the lipophilic particles is greatly affected by the type and amount of the surface treatment agent and the treatment method, and when the aggregate particles are large and the aggregate particles are hardly bonded, the UV protection effect It is not easy to loosen the agglomerated particles to a particle size that exhibits the above. The finely divided titanium oxide and finely divided zinc oxide powder subjected to the conventional lipophilic surface treatment cannot be said to sufficiently satisfy these performances.

  Conventionally, many are known as a lipophilic surface treatment agent. For example, silicone oil (for example, methylpolysiloxane, methylhydrogenpolysiloxane, or alkylsilane having an alkyl moiety having 10 or less carbon atoms) is used as the surface treatment agent. Is dissolved in a solvent, added to the powder, dried, and then baked by heating (Patent Document 1). Using a media grinder in an organic solvent such as octyltriethoxysilane. Surface treatment with an organosilicon compound such as octyltriethoxysilane while being dispersed (Patent Document 2), treatment of an inorganic powder used in makeup cosmetics in water using an acylamino acid or a salt thereof as a surface treatment agent Method (Patent Document 3), A layer as a surface treatment agent for improving the dispersibility of powder And a method of coating the surface treatment agent of the B layer by a jet method (Patent Document 4), a method using an acrylic derivative or an acrylamide derivative as a constituent monomer, and a polymer polymerized by living radical polymerization as a surface treatment agent ( Various surface treatment methods such as Patent Document 5) have been proposed.

  However, organic silicon compounds such as silicone oil and octyltriethoxysilane, which are surface treatment agents such as Patent Document 1 and Patent Document 2, have a strong oil feeling and high water repellency. The detergency is poor. Further, the fine particle powder is granulated at the time of the surface treatment to form a hard agglomeration and is not easily dispersed. Further, even when N-acylamino acid or a salt thereof is used as a surface treatment agent, as in Patent Document 3, a pigment having a small specific surface area such as a pigment for makeup cosmetics is considered without considering the treatment method. Is not a problem, but when processing pigments with a large specific surface area, such as fine particle titanium oxide and fine particle zinc oxide, the amount of treatment increases because the pigment surface is oleophilic. No consideration is given to the fact that the feel is heavy and the cohesive force between the pigment particles becomes very strong and difficult to disperse. Moreover, in patent document 4, since the feeling of use at the time of application | coating has a strong oil feeling and water repellency is high, detergency becomes bad. In patent document 5, although it is excellent in detergency, the feeling of use at the time of application | coating has a strong oil feeling, and it cannot be said that the adhesiveness to skin is enough. These conventional methods lack the measures for the smooth use feeling at the time of application, cleanability, adhesion to the skin, cosmetic effect and makeup sustainability by the surface treatment agent of the fine particle powder.

JP-A-8-104606 JP 2000-264824 A JP 1-50202 JP2002-80748 JP2007-210903A

  The present invention relates to a lipophilic surface-treated fine particle powder excellent in smooth use feeling and cleanability, and a method for producing the same, and further by making the surface-treated fine particle powder dispersed and blended. It aims at providing the cosmetics excellent in a usability | use_condition, the outstanding washing | cleaning property, the makeup | decoration effect, and makeup persistence.

In the present invention, an inorganic powder of fine particle titanium oxide or fine particle zinc oxide having a primary particle diameter of 5 nm to 150 nm is used as a surface treatment agent with N-acylamino acid or a salt thereof, and 100 parts by weight of the inorganic powder. 0.5 to 30.0 parts by weight of a lipophilic surface-treated fine particle powder having a surface-treated ultraviolet shielding effect, wherein the N-acylamino acid has 12 to 20 carbon atoms, saturated fatty acid and aspartic acid, An acylamino acid compound with an amino acid selected from glutamic acid, and the salt is a metal salt selected from the group consisting of Fe, Zn, Ca, Mg, Al, Zr, Ti, and in the surface treatment step, the surface treatment temperature is A lipophilic surface treatment with a superior feel and cleanliness, characterized by being surface treated in water or in a water-containing state at a temperature of 60 ° C or higher and lower than the boiling point of water. It relates to a particle powder.
Examples of preferred embodiments of the oleophilic surface-treated fine particle powder excellent in smooth use feeling and cleanability according to the present invention include the following. Any combination thereof is a preferred embodiment of the lipophilic surface-treated fine particle powder of the present invention as long as there is no particular contradiction.
(1) Surface treatment is performed with 1 to 12.0 parts by weight of N-acylamino acid or a salt thereof with respect to 100 parts by weight of the inorganic powder.
(2) In the surface treatment step, the surface treatment temperature is 60 ° C. or higher and 95 ° C. or lower in water or water.
(3) In the surface treatment step, an acid or a group consisting of Fe, Zn, Ca, Mg, Al, Zr, Ti with respect to an aqueous solution in which the N-acylamino acid or a salt thereof previously heated to 60 ° C. or more is dissolved. Surface treatment is performed with the N-acylamino acid or salt thereof, which is a surface treatment agent, by adding and reacting an aqueous solution of a metal water-soluble salt selected from
(4) The addition amount of the acid or the soluble metal salt is 60 to 120% of the equivalent of the carboxyl group contained in the used N-acylamino acid.
Furthermore, the present invention relates to a dispersion containing at least the above-described lipophilic surface-treated fine particle powder having an ultraviolet shielding effect and an oil agent as a dispersion medium.
As a preferred embodiment of the dispersion of the present invention, the dispersion contains at least an oil agent and a surfactant as the surface-treated fine particle powder and a dispersion medium.
Furthermore, the present invention relates to a cosmetic comprising the surface-treated fine particle powder or a dispersion containing the surface-treated fine particle powder.

According to the present invention, an inorganic powder of fine particle titanium oxide or fine particle zinc oxide having a primary particle diameter of 5 nm to 150 nm is used as a surface treatment agent with the N-acylamino acid or a salt thereof, based on 100 parts by weight of the inorganic powder. A lipophilic surface-treated fine particle powder having a surface treatment temperature of 60 ° C. or higher and less than the boiling point of water at 0.5 to 30.0 parts by weight and having been surface-treated in water or in a water-containing state. In addition, by blending the surface-treated fine particle powder into a dispersion, it is possible to provide a cosmetic material that is excellent in smooth use feeling, cleanability, cosmetic effect, and makeup sustainability. it can.

Although the preferable aspect of this invention is described below, the arbitrary combination is also a preferable aspect of this invention as long as there is no contradiction in particular.
(1) Powder The inorganic powder used in the present invention can be used as fine particle titanium oxide or fine particle zinc oxide having an ultraviolet shielding effect, or a composite or mixed system thereof. The fine particle titanium oxide has various particle shapes, for example, a spindle shape, a butterfly shape, a rod shape, a bow tie shape, a saddle shape, an indeterminate shape, etc., which may be any shape, and the crystal structure is a rutile type. , Anatase type, rutile / anatase type, any crystal structure may be used, and in order to suppress surface activity, the particle surface is treated with an inorganic material such as silica, alumina, aluminum hydroxide, zirconia, or the like. What is processed by 2 or more types is preferable. Fine zinc oxide also has various shapes, for example, hexagonal, amorphous, petal, etc., and other shapes may be used, and the surface of the particles may be treated with an inorganic material such as silica, alumina, hydroxide. What was processed by 1 type, such as aluminum, or its 2 types or more may be used. The primary particle diameter is preferably 5 to 150 nm in both fine particle titanium oxide and fine particle zinc oxide when measured with an electron microscope.

(2) Surface treatment agent The N-acylamino acid used in the present invention is an acylamino acid compound of a saturated fatty acid having 12 to 20 carbon atoms and an amino acid selected from aspartic acid and glutamic acid, and the carboxyl group of the amino acid is There are free bodies or insolubilized salts such as Fe, Zn, Ca, Mg, Al, Zr, and Ti.

Specifically, Amisoft HS-11P, Amisoft HAP, Amisoft MK-11, Amisoft CA and the like commercially available from Ajinomoto Co., Perisea, Aminoformer, Amino Surfactant and the like commercially available from Asahi Kasei are listed. .

The amount of the surface treatment agent is 0.5 to 30.0 parts by weight with respect to 100 parts by weight of the inorganic powder, and more preferably 1.0 to 12.0 parts by weight. If the amount of the surface treatment agent is small, the lipophilicity is weak, the makeup persistence may be deteriorated, and the stability of the cosmetic may be deteriorated. If the amount of the treatment agent is large, the feeling of use becomes heavy, and the dispersibility and dispersion stability are also increased. Becomes worse. Depending on the primary particle size and specific surface area of the inorganic powder to be used, treatment with the minimum amount of surface treatment agent that can impart oleophilic properties makes the feel more comfortable to use, higher cleanability, makeup effect, makeup lasting You can get sex.

(3) Surface treatment method In the surface treatment of the present invention, the surface treatment agent may be either chemical adsorption or physical adsorption on the surface of the fine particle powder, and a conventionally used method is used as the surface treatment method. Although not particularly limited, the treatment temperature in the surface treatment step is 60 ° C. or more and less than the boiling point of water, preferably 95 ° C. or less in water or water. For example, an inorganic powder is put into a kneader that can be heated and cooled, heated to 60 ° C. or higher while stirring, and an aqueous solution in which a salt such as N-acylamino acid or Na, K dissolved in advance at 60 ° C. or higher is dissolved, Alternatively, an aqueous solution in which N-acylamino acid or a salt thereof is dissolved at 60 ° C. or higher with alkaline water is added and stirred, and inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, acetic acid, or their Fe, Zn, Ca, Mg, Al, By slowly adding a metal-soluble salt such as Zr and Ti, the surface treatment agent of the present invention forms the acylamino acid free substance, or its Fe, Zn, Ca, Mg, Al, Zr, and Ti salt, and the surface treatment. I do. At this time, if the treatment temperature is low, a large amount of surface treatment agent is required, the feeling of use becomes heavy, and the cleanability becomes poor. The amount of the metal-soluble salt added is preferably 60 to 120% of the carboxyl group equivalent contained in the used N-acylamino acid. If the amount is less than this, there is a possibility that sufficient lipophilicity may not be exhibited. If the amount is too large, these salts remain in the surface-treated fine particle powder and deteriorate the stability of the cosmetic. Need to be cleaned. In the surface treatment step, at least the inorganic acid or the metal-soluble salt thereof is maintained at 60 ° C. or higher and lower than the boiling point of water until the end of addition.

As another surface treatment method, water or alkaline water is heated to 60 ° C. or more in a stirrable tank, and the surface treatment agent N-acylamino acid or a salt thereof is stirred and dissolved therein. Disperse the inorganic powder in it. Dispersion may be a known method and is not particularly limited. For example, the dispersion may be stirring in a tank, but preferably the pigment is dispersed in a liquid such as a disper mixer, a homomixer, an in-line mixer, a media grinder, a three roll, an attritor, a colloid mill, or an ultrasonic disperser. Disperse the pigment using a disperser that can be used to disperse. In this case, the alkaline water or the ratio of water to the pigment is 3 to 10 times the amount of alkaline water or water by weight. This ratio may be adjusted by the ratio so that the viscosity is easy to disperse. Next, after dispersing the pigment, the surface treatment of the present invention is carried out by slowly adding an acid or a 1-30% by weight aqueous solution of a metal-soluble salt such as Mg, Ca, Zn, Zr, Al, Ti while stirring. It forms an acylamino acid free compound, or its Fe, Zn, Ca, Mg, Al, Zr, Ti salt. An acylamino acid free form or a salt thereof is formed, and after surface treatment and aging, it is filtered with a filter press or a centrifugal dehydrator. At this time, in order to remove the water-soluble salt contained in the water-containing pigment cake, it may be washed with water. Next, the water-containing pigment cake is taken out and water is removed with a dryer. After drying, a known method may be employed for pulverization, and the pulverization is performed with an atomizer, a pin mill, a JET mill or the like, although not particularly limited. More preferably, a method of pulverizing to a state where there are no coarse particles with a JET mill is preferable.

(4) Dispersion The dispersion medium used in the oily dispersion of the present invention may be any oil that can be used in cosmetics. Broadly speaking, silicone oils, hydrocarbon oils, ester oils, or mixtures thereof It is an oil. Specifically, silicones such as dimethylpolysiloxane, methylphenylpolysiloxane, decamethylcyclotetrasiloxane, methyltrimethicone, caprylylmethicone, liquid paraffin, liquid isoparaffin, hydrogenated polyisobutene, squalane, squalene, petrolatum, paraffin, Celesin, microcrystalline wax, C18-C12 alkane, C13-C15 alkane, etc., and vegetable hydrocarbons, specifically, VEGELIGHT1214, VEGELIGHT1214LC, VEGELIGHT12, VEGELIGHT14, VEGELIGHT16, VEGELIGHHT16, VEGEGHIGHH Ethyl, isopropyl myristate, octyl palmitate, octa Examples include esters such as cetyl acid, isononyl isononanoate, diisostearyl malate, glyceryl tricaprylate, glyceryl caprylate / capric acid, glyceryl 2-ethylhexanoate, C12-15 alkylbenzoate, and the like. Others include safflower oil, soybean oil, evening primrose oil, grape seed oil, rosehip oil, cucumber nut oil, almond oil, sesame oil, wheat germ oil, corn oil, cottonseed oil, avocado oil, olive oil, camellia oil, persic oil, Castor oil, peanut oil, hazelnut oil, macadamia nut oil, medfoam oil, cocoa butter, shea butter, tree wax, coconut oil, palm oil, palm kernel oil, beef tallow, horse fat, mink oil, milk fat, egg yolk oil, turtle oil Oils and fats such as beeswax, whale wax, lanolin, carnauba wax, candelilla wax, jojoba oil, waxes such as lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, linoleic acid, undecylenic acid, hydroxy Fatty acids such as stearic acid and lanolin fatty acid, perfluoropolyether oil, par Fluorocarbons, fluorine-based oils such as hydrofluoroether, oil-soluble ultraviolet absorbers, and the like.

(5) Surfactant The oil-based dispersion of the present invention is more preferable as the content of the surface-treated fine particle powder is as simple as possible, but the content of the surface-treated fine particle powder is higher and the dispersibility is higher. In order to increase, it is more preferable to include a surfactant having a dispersing effect as the third component. It is preferable to use the surfactant to be used in the cosmetic to be blended. For example, linear, branched or alkyl-modified polyether-modified silicone, glycerin fatty acid ester, sorbitan fatty acid ester, propylene glycol fatty acid ester, POE glycerin fatty acid ester, POE / POP alkyl ether, hardened castor oil fatty acid ester, etc. .

(6) Dispersion method The method for kneading or dispersing the surface-treated fine particle powder according to the present invention in a dispersion medium may be a known method, and is not particularly limited. For example, a kneader, three rolls, an extruder, a disper mixer, a homomixer, an in-line mixer, a media grinder, an attritor, a ball mill, a colloid mill, an ultrasonic disperser, etc. may be used.

(7) Cosmetics There are no particular limitations on the cosmetics with which the lipophilic surface-treated fine particle powder of the present invention is blended. As the cosmetic dosage form, for example, conventionally known dosage forms such as emulsion, cream, solid, paste, gel, powder, multilayer, mousse, and spray can be selected. Specifically, as makeup cosmetics, makeup foundation, powder foundation, liquid foundation, oil foundation, stick foundation, pressed powder, face powder, white powder, lipstick, lipstick overcoat, lip gloss, concealer, blusher, eye shadow, Eyebrow, eyeliner, mascara, water-based nail enamel, oily nail enamel, emulsified nail enamel, enamel top coat, enamel base coat, etc. UV for packs, carmine lotions, liquid facial cleansers, facial cleansing foams, facial cleansing creams, facial cleansing powders, makeup cleansers, body gloss, sunscreens or sun creams For defensive cosmetics and lotions, hair gloss, hair cream, hair shampoo, hair rinse, hair color, hair brushing, etc. for anti-perspirant cosmetics, cream, lotion, powder, spray type deodorant products Can be mentioned.

  In addition, the cosmetic compounded with the lipophilic surface-treated fine particle powder of the present invention is a pigment dispersant, an oil agent, a surfactant, an ultraviolet absorber, and the like, which are usually used in cosmetics and the like within a range not impairing the effects of the invention Preservatives, antioxidants, film forming agents, humectants, thickeners, dyes, preservatives, pigments, fragrances and the like can be appropriately blended.

  Furthermore, the surface-treated inorganic powder thus obtained is widely used not only in cosmetics but also in various fields such as plastic additives, inks, paints, toners (magnetic powders), chemical fibers, packaging materials, and electronic materials. It can also be applied as a powder.

EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.

Example 1
Heat up 10,000 cc of ion exchange water to 80 ° C. and add 60 g of disodium N-stearoyl-L-glutamate. 1 kg of fine particle titanium oxide MT-100SA (manufactured by Teika) is added thereto and stirred. The pigment slurry was dispersed for 3 passes with a media disperser (DYNO-MILL), and then a 1N aqueous hydrochloric acid solution was slowly added to the carboxy group equivalent of 100% while stirring. During this time, the temperature was maintained at 60 ° C. or higher and lower than the boiling point of water. After the addition, the mixture was cooled, dehydrated and filtered, dried in a hot air dryer at 115 ° C. for 18 hours, and then pulverized by a jet mill to obtain a lipophilic surface-treated fine particle powder.

(Example 2)
200 g of fine particle titanium oxide TTO-V-3 (Ishihara Sangyo Co., Ltd.) was added to Trimix (Triaxial vertical kneader manufactured by Inoue Trial Co., Ltd.), and 200 cc of ion-exchanged water was heated to 70 ° C. in advance. -A solution in which 22 g of sodium L-aspartate is dissolved is added and heated to 70 ° C with stirring. Thereafter, a 1N aqueous solution of aluminum sulfate was slowly added until the carboxy group equivalent reached 100%. During this time, the temperature was maintained at 60 ° C. or higher and lower than the boiling point of water. After cooling after the addition, it was dried at 115 ° C. for 18 hours with a hot air dryer, and then pulverized by a pin mill to obtain a lipophilic surface-treated fine particle powder.

(Example 3)
A hydrous titanium oxide obtained by hydrolysis of a titanium tetrachloride aqueous solution is made into a slurry of 100 g / L in terms of titanium oxide, 1.4 kg of a 48% sodium hydroxide aqueous solution is added to 2 L of this slurry, and heated at 95 ° C. for 120 minutes, Filter and wash thoroughly to obtain a cake. Next, the washed cake is slurried with water to 100 g / L in terms of titanium oxide, 760 g of 35% hydrochloric acid aqueous solution is added to 2 L of the slurry, heated to 95 ° C., and aged for 90 minutes. A spindle-shaped fine particle titanium oxide slurry having an average major axis of 0.1 μm and an average minor axis of 0.01 μm was obtained. Next, 8 wt% sodium aluminate aqueous solution as Al2O3 was added to the resulting fine particle titanium oxide slurry, and the pH was set to 7.0 with an aqueous sulfuric acid solution to cover Al hydroxide, and a slurry of fine particle titanium oxide 5% Got. Next, the slurry was filtered and washed sufficiently to obtain a wet cake containing fine particles of titanium oxide solid content of 36%.
Next, 556 g of the obtained water-containing wet cake (solid content 36%) and 3444 g of ion-exchanged water were mixed, dispersed with a homomixer at 9000 rpm for 3 minutes, heated to 80 ° C., and then N-lauroyl-L-asparagine. Add 24 g of sodium acid and stir for 30 minutes. Thereafter, a 1N aqueous solution of aluminum sulfate was slowly added until the carboxy group equivalent reached 100%. During this time, the temperature was maintained at 60 ° C. or higher and lower than the boiling point of water. After cooling after addition, it was dewatered and filtered, dried at 115 ° C. with a hot air dryer for 18 hours, and then pulverized with a pin mill to obtain a lipophilic surface-treated fine particle powder.
Example 4
5000 cc of ion-exchanged water is heated to 90 ° C., and 20 g of potassium N-myristoyl-L-glutamate is added. 1000 g of fine particle zinc oxide MZ-500 is added thereto and stirred. After dispersing with a homomixer for 30 minutes, a 1N aluminum chloride aqueous solution was slowly added until the carboxy group equivalent was 120%. During this time, the temperature was maintained at 60 ° C. or higher and lower than the boiling point of water. After cooling after addition, it was filtered, dried at 115 ° C. for 18 hours with a hot air dryer, and then pulverized with an atomizer to obtain a lipophilic surface-treated fine particle powder.

(Comparative Example 1)
The temperature of Example 1 was carried out at a room temperature of 50 ° C.

(Comparative Example 2)
The 1N hydrochloric acid aqueous solution of Example 1 was carried out at a carboxy group equivalent of 30%.

(Comparative Example 3)
10000 cc of deionized water is heated to 80 ° C., and 350 g of disodium N-stearoyl-L-glutamate is dissolved. 1000 g of fine particle titanium oxide MT-100SA is added thereto and stirred. After dispersing with a homomixer for 30 minutes, 1N hydrochloric acid was slowly added until the carboxy group equivalent was 100%. During this time, the temperature was maintained at 60 ° C. or higher and lower than the boiling point of water. After the addition, the mixture was cooled, dehydrated and filtered, dried in a hot air dryer at 115 ° C. for 18 hours, and then pulverized by a jet mill to obtain a lipophilic surface-treated fine particle powder.

(Comparative Example 4)
Reactive organosilicone (Shin-Etsu Chemical Co., Ltd .: KF-99P) 80 g and reactive organosilicone prepared in advance while stirring and mixing with 2 kg of fine particle titanium oxide MT-100SA (manufactured by Teika) into a Hensyl mixer. (Shin-Etsu Chemical Co., Ltd .: X-24-9171) 120 g of a mixed solution was added and stirred for 30 minutes. The said process was performed at 50 degreeC. Next, after pulverizing with a jet mill, it was dried with a hot air dryer at 110 ° C. for 9 hours to obtain a lipophilic surface-treated fine particle powder.

(Comparative Example 5)
2 kg of fine particle titanium oxide TTO-S-3 (manufactured by Ishihara Sangyo Co., Ltd.) is charged into 5000 ml of a mixture of deionized water / IPA = 50/50, and a reactive organosilicone (Shin-Etsu Chemical Co., Ltd .: X24-9171) as a surface treatment 160 g and 40 g of isopalmitic acid were added and dispersed by circulation for 30 minutes in a sand grinder (DYNO-Mill). The said process was performed at 40 degrees or less. The dispersion was dried under reduced pressure at 100 ° C. for 7 hours in a vacuum dryer, and then pulverized by a pin mill to obtain a lipophilic surface-treated fine particle powder.

(Comparative Example 6)
While adding 2 kg of fine particle zinc oxide (MZ-500 manufactured by Teika Co., Ltd.) to the Hensill mixer and stirring and mixing, 100 g of the surface treatment agent reactive organosilicone (Shin-Etsu Chemical: KF-99P) is added to the Hensyl mixer. The temperature was maintained at 80 ° C. and stirred for 30 minutes. Next, after pulverizing with a jet mill, it was dried with a hot air dryer at 110 ° C. for 9 hours to obtain a lipophilic surface-treated fine particle powder.

(Dispersion production example)
(1) Titanium oxide-based lipophilic surface-treated fine particle titanium oxide 40 parts, cyclopentasiloxane (KF-995, manufactured by Shin-Etsu Chemical Co., Ltd.) and PEG-10 dimethicone (KF-6017, manufactured by Shin-Etsu Chemical Co., Ltd.) 10 parts After stirring and mixing with a disper, the mixture was dispersed for 2 hours using a batch media disperser (RMB-04, manufactured by IMEX Co., Ltd.) to obtain a dispersion of each lipophilic surface-treated fine particle powder.
(2) Zinc oxide-based lipophilic surface-treated fine particle zinc oxide powder 50 parts, cyclopentasiloxane (KF-995, manufactured by Shin-Etsu Chemical Co., Ltd.) and PEG-10 dimethicone (KF-6017, manufactured by Shin-Etsu Chemical Co., Ltd.) After 5 parts were stirred and mixed with a disper, the mixture was dispersed for 3 hours using a batch media disperser (RMB-04, manufactured by IMEX) to obtain a dispersion of each lipophilic surface-treated fine particle powder.

(Test and evaluation method)
The surface-treated fine particle powders and dispersions produced in the examples and comparative examples were evaluated below. The test method is shown below.

(1) Lipophilicity evaluation of lipophilic surface-treated fine particle powder 80 g of ion-exchanged water is put into a 100 cc beaker, about 1 g of the surface-treated fine particle powder is added, and stirred 50 times with a spatula to visually check the degree of turbidity of water. judge. This was repeated three times, and expressed as the state after 50 times stirring / the state after 100 times stirring / the state after 150 times stirring according to the following evaluation criteria.
(Evaluation criteria)
5: All the powder floats on the surface of the water, no turbidity 4: The powder floats on the surface of the water, but the water is slightly cloudy 3: The powder floats on the surface of the water, but the water is slightly cloudy 2: Some powder floats on the surface of the water, but most migrates into the water 1: All powder enters the water

(2) Dispersibility evaluation for oil agent usable in cosmetics The prepared dispersion was applied to a TAC transparent film with a bar coater # 3, dried at room temperature for 3 hours, and then applied to a spectrophotometer (Shimadzu Corporation UV-3150). 560 nm transmittance was measured.

(3) Evaluation of feeling of use The dispersion produced for 10 panelists was applied to the arm, and the feeling of use at that time was evaluated.
(Evaluation criteria)
Ask the panelists to answer either (A) the feeling of smoothness or (B) the feeling of stickiness is strong. (A) If the answer is +1, (B) In this case, the total number of 10 persons was set as a score of -1.

Lipophilicity: In a process where the temperature during the surface treatment of the present invention is 60 ° C. or more and less than the boiling point of water, lipophilicity could be imparted with a small amount of treatment agent.
Dispersibility: Dispersibility is good when the amount of the N-acylamino acid or salt thereof is within the range of the present invention, but the dispersibility becomes worse when the amount of treatment increases.
Usability: The product of the present invention was very smooth and good, but the comparative product using a large amount of treatment and other treatment agents had a sticky feeling.
From the above results, it can be expected that by blending the product of the present invention into a cosmetic, it is possible to provide a cosmetic that is excellent in a smooth use feeling and a cosmetic effect and imparts an ultraviolet shielding effect with improved makeup sustainability.

Production Example 1: Production of two-layer type W / O sunscreen An emulsion (two-layer type W / O sunscreen) having the composition shown in Table 2 was produced. As for evaluation, the in-vitro SPF shown below was measured for the ultraviolet shielding effect, and the usability and detergency evaluation test was conducted by having 10 panelists apply the prepared emulsion to their arms, and the usability was evaluated. Further, after 5 hours of application, the product was washed with soap and evaluated for detergency.
(In-VitroSPF)
The produced emulsion was applied to a TAC transparent film with a bar coater # 3, dried at room temperature for 3 hours, and then measured with an SPF analyzer (SPF-290 manufactured by Optometric Co.) for in-vitro SPF value.
(Usage evaluation criteria)
◎: 8 or more responded that they had a smooth feeling
○: Reply when 5 to 7 people have a smooth feeling △: Reply when 2 to 4 people have a smooth feeling ×: Reply that 2 or less people have a smooth feeling (evaluation criteria for detergency)
◎: Reply is excellent in cleanability ○: Reply is excellent in cleanability ×: Reply is poor in cleanability

(Manufacturing method)
The oil phase components of components (1) to (12) are mixed, components (13) to (16) are heated and dissolved at 70 ° C. to homogenize, and this is added to the previously produced oil phase component. The mixture was emulsified with a mixer and cooled to 35 ° C. to obtain an emulsion.

As can be seen from these results, it can be seen that the product of the present invention has a smooth use feeling, that is, has no stickiness, has a very good coating feel, and is excellent in cleanability after use.

Production Example 2: Production of emulsion type foundation A W / O type liquid foundation having the composition shown in Table 3 was produced by the following method.

Manufacturing method:
The above components (7) to (11) were previously mixed and pulverized. The mixture of components (7) to (11) previously pulverized was added to an oil phase in which components (1) to (6) were uniformly dissolved and mixed at 70 ° C., and the mixture was uniformly dispersed with a homodisper. An aqueous phase in which components (12) to (16) are uniformly mixed and dissolved at 70 ° C. is gradually added to the oil phase, uniformly dispersed with a homomixer, cooled, and component (17) is added to prepare emulsified particles to prepare a liquid foundation. Manufactured.

The cosmetic compounded with the lipophilic surface-treated fine particle powder of the present invention was excellent in a smooth use feeling, cleanability, cosmetic effect, and makeup sustainability as compared with the conventional one.

Production Example 3 Production of UV Cut Powder Foundation A powder foundation having the composition shown in Table 10 was produced by the following method.

(Manufacturing method)
The above components (1) to (6) were mixed and pulverized through a pulverizer. This was transferred to a high-speed blender, and components (7) to (11) were mixed by heating and uniformed, and further mixed to make uniform. This was passed through a pulverizer and sieved to make the particle size uniform, and then compression molded with an aluminum dish at a surface press pressure of 3 MPa to produce a UV cut powder foundation.

The in-vitro SPF value of the cosmetic containing the lipophilic surface-treated fine particle powder of the present invention was 18, and the conventional product was 13. In addition, the cosmetic containing the lipophilic surface-treated fine particle powder of the present invention was excellent in a smooth use feeling, cleanability, makeup effect, and makeup sustainability.

Claims (8)

  An inorganic powder of fine particle titanium oxide or fine particle zinc oxide having a primary particle diameter of 5 nm to 150 nm is used as a surface treatment agent with N-acylamino acid or a salt thereof, and 0.5 to 30 with respect to 100 parts by weight of the inorganic powder. 0.0 part by weight of a lipophilic surface-treated fine particle powder having a surface-treated smooth feel and cleanability, wherein the N-acylamino acid has 12 to 20 carbon atoms, saturated fatty acid and aspartic acid , An acylamino acid compound with an amino acid selected from glutamic acid, and the salt is a metal salt selected from the group consisting of Fe, Zn, Ca, Mg, Al, Zr, Ti, surface treatment temperature in the surface treatment step The surface treatment is carried out in water or in a water-containing state at a temperature of 60 ° C. or higher and lower than the boiling point of water. Particle powder.   The lipophilic surface treatment according to claim 1, wherein the inorganic powder is subjected to a surface treatment with 1.0 to 12.0 parts by weight of N-acylamino acid or a salt thereof with respect to 100 parts by weight of the inorganic powder. Fine particle powder. 3. The lipophilic surface-treated fine particle powder according to claim 1, wherein the surface treatment step is performed in a water or water-containing state at a surface treatment temperature of 60 ° C. to 95 ° C. 3. In the surface treatment step, an acid or a group consisting of Fe, Zn, Ca, Mg, Al, Zr, Ti with respect to an aqueous solution in which the N-acylamino acid or its Na or K salt is previously heated to 60 ° C. or higher is dissolved. A surface treatment is carried out with the N-acylamino acid or a salt thereof as a surface treatment agent by adding and reacting an aqueous solution of a water-soluble salt of a metal selected from the above. The lipophilic surface-treated fine particle powder according to any one of the above. The lipophilic surface-treated fine particles according to claim 4, wherein the addition amount of the acid or the soluble metal salt is 60 to 120% of the equivalent of the carboxyl group contained in the used N-acylamino acid. powder. A dispersion containing at least the lipophilic surface-treated fine particle powder according to claim 1 and an oil agent as a dispersion medium. A dispersion comprising at least the surface-treated fine particle powder according to any one of claims 1 to 5 and an oil agent and a surfactant as a dispersion medium. A cosmetic comprising the surface-treated fine particle powder according to any one of claims 1 to 7 or a dispersion containing the surface-treated fine particle powder.