JPH08239310A - Flaky powder, its production, and cosmetic formulated therewith - Google Patents

Abstract

PURPOSE: To obtain metal oxide flaky powder suitable for formulation as a colorant in cosmetics, safe to human body, excellent in light resistance, bleed resistance, heat resistance, etc., containing an organic pigment with high opacifying power. CONSTITUTION: The objective metal oxide flaky powder contains 0.5-40wt.% of an organic pigment (esp. pref. Red #226, Red #202, Red #203, Red #204). The metal oxide is pref. selected from silica, titania, alumina and zirconia. The flaky powder is obtained by the following process: a solution comprising water, an organic solvent, organic pigment and hydrolyzable organometallic compound subject to polycondensation is applied on a smooth-surfaced substrate, and the resultant film is peeled off and then heated at 80-250 deg.C for 5min to 24h. For the flaky powder, the organic pigment lies included and immobilized by the inorganic oxide; therefore, the organic pigment is seldom leached or eliminated from the flakes. The other objective cosmetic formulated with the flaky powder is excellent in perspiration resistance, etc.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flake powder, particularly a pigment-containing flake powder suitable for being incorporated into cosmetics as a coloring agent, a method for producing the same, and the flake powder. Regarding cosmetics.

[0002]

2. Description of the Related Art Conventionally, tar-based synthetic pigments and natural pigments have been used as colorants for cosmetics. When these colorants were directly added to and mixed with the cosmetic base, the dispersion was sometimes incomplete, and color unevenness and color spots were sometimes observed, which was not preferable. Furthermore, when the amount of pigment added increases, the pigment adheres strongly to the skin, nails, etc., causing color separation with other inorganic pigments (for example, Benji) that are also compounded at the time of prescription, which hinders the make-up effect. was there. Also,
It was heavy to use and had the drawback of being difficult to stretch. Therefore, there is a limit to the amount of the pigment compounded, and it has been difficult to obtain a highly saturated cosmetic product.

It has also been carried out to improve the dispersibility of the dye by admixing the dye with an inorganic pigment such as talc or mica to adhere the dye to the surface of the inorganic pigment. However, in this case, there is a drawback that the vividness of the pigment is lowered, and the pigment is easily detached from the inorganic pigment due to the shearing force in the manufacturing process of the cosmetic, for example, the crushing, so that color separation occurs.

On the other hand, it has also been proposed to blend a coloring pigment obtained by dyeing regenerated fibroin fine powder with an acid dye into a cosmetic (for example, JP-A-61-37715). Although some improvement in light resistance and bleeding resistance is recognized by this method, it is not sufficient, and the dyeing efficiency is poor, it is difficult to dye at high concentration depending on the dye, and the dye is detached when using the combined cosmetic. There was a problem such as sometimes.

In addition, the tar-based synthetic pigments that have been frequently used in cosmetics have been the legal pigments that are licensed for use as cosmetics since they pose a problem of carcinogenicity, allergenicity and other harmful effects on the human body. There is a tendency to decrease year by year, and the development of more safe dyes is desired. As a method for reducing allergenicity, a method of purifying a raw material, washing a dye with an organic solvent or the like (for example, JP-A-57-192468, JP-A-59-74164) or a method in which an aqueous solution is treated with activated carbon and then laked (for example, Japanese Patent Publication No. 4-51588) is disclosed. Although the dyes treated by these methods have improved safety, there are problems that the number of manufacturing steps increases and the cost becomes high, and that complete purification and impurity removal are extremely troublesome. It was

Natural dyes are one of the safer dyes, but they have problems in that they are inferior in light resistance, bleeding resistance, heat resistance and the like, and the hue varies greatly depending on pH.

The present inventors previously applied for a method for producing a flake body containing an acid dye (Japanese Patent Application No. 6-1).
98113). In this method, a solution containing an organic metal compound capable of being hydrolyzed and dehydrated and condensed, for example, a metal alkoxide such as silicon tetramethoxide, and an acid dye is applied on a substrate having a smooth surface, and then the solution is peeled off. A flake body containing an organic dye is obtained.
Although the flakes have an excellent color tone, they are too transparent, and their coloring properties, coloring properties and hiding properties are not sufficient, and they are insufficient to meet various needs for cosmetics. $

SUMMARY OF THE INVENTION In view of the above-mentioned prior art, the present invention is safe for human body, does not cause skin irritation, and is non-allergenic, light resistance, bleed resistance, heat resistance, water resistance, sweat resistance,
It is intended to provide a cosmetic containing a colored flake powder which is excellent in adhesiveness, spreadability, dispersibility, touch to the skin, color tone, and particularly excellent in colorability and hiding power.

[0008]

[Means for Solving the Problem] In order to solve this problem,
The present inventors added an organic pigment to a solution containing an organometallic compound capable of hydrolysis and polycondensation, water, and an organic solvent,
Dispersing, coating this on a substrate, preferably a substrate having a smooth surface, drying and peeling from the substrate, and then heat-treating, easily and efficiently, containing an organic pigment, excellent It was found that a colored flake powder having characteristics could be produced, and the present invention was completed. That is, the present invention is a metal oxide flake powder containing 0.5 to 40% by weight of an organic pigment.

The metal oxide flake powder of the present invention is manufactured as follows. An organic pigment is dispersed in a solution containing an organic metal compound capable of hydrolysis and polycondensation, water, and an organic solvent, and this is applied onto a substrate, preferably a substrate having a smooth surface, and dried to obtain a substrate. If the colored flaky powder is produced, the colored flaky powder can be produced easily and efficiently by peeling it from the substrate and then heat treating it.

As described above, by adding and dispersing the organic pigment, a colored flake powder having a darker color and hiding power than that obtained by adding a dye can be obtained.

The hydrolyzable and polycondensable organometallic compound used in the present invention is preferably a metal alkoxide having an alkoxyl group. Specifically, silicon,
Methoxide such as titanium, aluminum, zirconium,
Ethoxide, propoxide, butoxide and the like are used alone or as a mixture. The composition of the obtained flake powder is a metal oxide such as pure silica, silicate type, titanate type, aluminate type, zirconate type amorphous. The above metal ethoxide is more preferably used from the viewpoint of safety and security in using the obtained colored flake powder. This is because even if the organic residue remaining in the obtained colored flake powder is subjected to some decomposition promotion, if the decomposition product is ethanol, there is no problem in using cosmetics.

The organic pigment in the colored flake powder is preferably selected from the group of organic pigments (commonly known as legal dyes) according to the Ordinance No. 30 of the Ministry of Health and Welfare on August 31, 1941 for cosmetic use. , Red No. 202, Red 203
No., Red No. 204, Red No. 205, Red No. 206, Red No. 207, Red No. 208, Red No. 219, Red No. 220
No., Red 221, Red 226, Red 228, Day 203, Day 204, Yellow 205,
Blue No. 204, Red No. 404, Red No. 405, Daidai No. 401, Yellow No. 401, Blue No. 404, etc. are exemplified. Among these organic pigments, in consideration of versatility, it is preferable to use Red 226, Red 202, Red 203, and Red 204. In fact, colored flake powders produced using these organic pigments have different color tones. And the color development is better. In the present invention, one kind or a mixture of two or more kinds of the above organic pigments is used.

These organic pigments are added to a solution containing an organometallic compound capable of being hydrolyzed and polycondensed, water, and an organic solvent, and a uniform solution is obtained through a dispersion process. As described below, the organic pigment has an organic pigment content of 0.
It is contained in the solution so as to be 5 to 40% by weight.

The preferred blending ratio of the above-mentioned organic pigment, a solution containing an organic metal compound capable of hydrolysis and polycondensation, water, and an organic solvent is as follows based on the organic pigment. Organic pigment 1 part by weight Organometallic compound capable of hydrolysis and polycondensation 5 to 35 parts by weight Water 10 to 75 parts by weight Organic solvent 1 to 50 parts by weight

The organic pigment may be dispersed by a known technique, and examples thereof include the use of a homogenizer, a disperser, a sand grinder mill, a ball mill, a roller mill, a high speed impeller mill, a pebble mill, an attritor, a colloid mill and the like. To be done. However, depending on the type of organic pigment, these dispersers are not always necessary, and there are cases in which a dispersed state that is practically acceptable will be obtained by simply stirring.

A surfactant or a dispersant may be added when the above organic pigment is dispersed. The surfactant or dispersant used is not particularly limited, but the colored flake powder is
Considering the fact that they are used as cosmetics, it is preferable to use the substances listed in the standards for cosmetic raw materials. Examples thereof include stearic acid soaps, various metal soaps, polyoxyethylene alkyl ethers, polyoxyethylene fatty acid esters, sorbitan fatty acid esters, dialkylsulfosuccinates, stearic acid, glycerin, and various oils and fats.

Dispersion of the above organic pigment is preferably carried out in a mixed solvent of an organic metal compound capable of hydrolysis and polycondensation, water and an organic solvent, since the process is simple, but before this final dispersion process, The organic pigment may be dispersed in a suitable solvent.

The organic solvent added to the solution containing the organometallic compound may be basically any solvent as long as it substantially dissolves the organometallic compound, but alcohols such as methanol, ethanol, propanol and butanol are preferred.
Ethanol is more preferably used from the viewpoint of safety and security in use of the obtained colored flake powder. However, if the alcohol generated by the hydrolysis reaction of the organometallic compound is sufficient, the solvent need not be used. From the viewpoint of improving the dispersibility of the organic pigment, various organic solvents such as acetone, xylene and butyl acetate may be added to such an extent that the homogeneity of the finally obtained solution is not impaired. However, at this time, it is necessary to dry sufficiently so that these solvents do not remain in the obtained colored flake powder.

In order to accelerate the hydrolysis of the organometallic compound, it is preferable to add an acid such as hydrochloric acid, nitric acid or sulfuric acid. The amount of the acid added is not particularly limited, but a molar ratio of 0.001 to 2 with respect to the organometallic compound is preferable. The amount of added acid is
If the molar ratio is less than 0.001, the promotion of hydrolysis of the organometallic compound is not sufficient, and if the molar ratio is more than 2, the effect of promoting hydrolysis is no longer improved and the acid becomes excessive, which is not preferable. .

In addition, an organic thickener or the like may be added to change the characteristics of the solution. However, if the amount of addition is large, the yield of the dry peeling process may decrease, so the amount of addition should be limited to 10% by weight or less.

Fine particles of metal oxides such as titanium oxide, cerium oxide and zinc oxide may be added to the solution containing the organometallic compound for the purpose of imparting an ultraviolet shielding effect. The addition of the metal oxide fine particles is not particularly limited, but 1) a method in which the metal oxide powder is dispersed at the same time as the organic pigment and 2) a metal oxide powder is previously dispersed in a solvent such as water or alcohol, Examples include a method of adding and dispersing separately from the pigment. More preferably, a metal hydroxide colloid having water or alcohol as a dispersion medium, a hydrous metal oxide colloid, a metal oxide colloid, etc. is added, because the dispersion stability of fine particles such as metal oxide is high, It is good because the process is simplified.

The substrate used in the present invention is made of a material such as metal, glass or plastic and has a smooth surface. A solution containing the above organometallic compound is applied to such a substrate to form a thin film of 0.2 to 50 μm. When this film dries, it contracts, but the substrate does not contract, so cracks occur in the film, and the film becomes flakes. In order for the substrate and the film to be separated from each other, it is preferable that there is little interaction such as strong bonding between the substrate and the film.

As a technique for forming a film on the surface of the substrate, a known technique may be used. For example, a method of dipping the substrate in a liquid containing the above-mentioned organometallic compound and then pulling it up (dip coating method), or Drop the above liquid on,
A method of rotating the substrate at a high speed (spin coating method), a method of spraying the liquid on the substrate (spray coating method), a method of attaching the liquid to a rotating roll and bringing the liquid into contact with the substrate (roll coating method), A method in which the liquid is pushed out from a slit-shaped nozzle and applied on the substrate (die coating method), a method in which the liquid is naturally dropped from the slit and applied on the substrate (curtain coating method), and the like are used. In the present invention, since the organic pigment particles dispersed in the liquid are effectively and uniformly contained in the coating film, the spray coating method, the roll coating method, the die coating method, and the curtain coating method are preferably used among the above methods. To be

There is no particular limitation on the method of heat treatment. The heat treatment temperature and time are preferably conditions under which removal of the solvent and acid is ensured and decomposition of the organic pigment does not occur, and heating is usually performed at 80 to 250 ° C. for 5 minutes to 24 hours. Heat treatment may be performed under reduced pressure for the purpose of suppressing the decomposition of the organic pigment.

The thickness of the colored flake powder thus obtained varies depending on the solution or film forming conditions, but is generally 0.1 to 5 μm, and is preferably 0.3 for cosmetics. ~ 1.0, particularly preferably 0.4 ~
It is 0.9 μm. If it is thicker than 5 μm, the difference in drying speed between the free surface after film formation and the vicinity of the substrate becomes too large, and peeling between films occurs in a direction parallel to the substrate. On the other hand, when the thickness is less than 0.1 μm, the adhesive force between the substrate and the film becomes too large and the film does not peel off from the substrate. The particle diameter of the colored flake powder is 1 to 100 μm, and for blending with cosmetics, it is preferably 3 to 50 μm, and particularly preferably 7 to 40 μm.

The content of the organic pigment in the colored flake powder of the present invention is 0.5% by weight or more and 40% by weight or less, more preferably 3 to 30% by weight. If it is less than 0.5%, the coloring effect by the organic pigment becomes small and the color tone of coloring is not good, which is not preferable. On the other hand, when it is more than 40%, the organic pigment exposed on the surface of the flaky powder becomes noticeable, and the properties such as non-allergenicity, extensibility (spreading), dispersibility, and touch to the skin are deteriorated. , Not preferable.

In the cosmetic containing the organic pigment-containing flake powder of the present invention, the organic pigment is encapsulated and fixed by the inorganic oxide, so that the organic pigment may be eluted or detached from the flakes. It is a stable product with almost no bleed resistance, water resistance, and sweat resistance. Also,
Since the organic pigment does not come into direct contact with the skin, non-allergenicity is improved, and it does not stain the skin, nails, etc., and since it has a flake shape, the organic pigment does not clog sweat glands and pores, It is a safe product with no skin irritation.

Further, since the organic pigment is contained in the inorganic oxide, the stability of the organic pigment is improved,
The product has high light resistance and heat resistance, and has a preferable color tone with vivid color. Further, the organic pigment-containing flake-like powder does not aggregate with each other, its surface is smooth, and exhibits good slipperiness, so that extensibility (spreading),
The product has good dispersibility and adhesion, and is excellent in touch feeling.

In the cosmetics of the present invention, in addition to the above-mentioned organic pigment-containing flake powder, pigments that are usually used may be used in combination, if necessary. For example, titanium oxide, zinc oxide, zirconium oxide, yellow iron oxide,
Inorganic pigments such as black iron oxide, rouge, ultramarine blue, dark blue, chromium oxide and chromium hydroxide, pearlescent pigments such as mica titanium and bismuth oxychloride, powders such as silica beads, plastic beads such as nylon and acrylic, talc , Kaolin, mica, sericite, other mica, magnesium carbonate, calcium carbonate, aluminum silicate, magnesium silicate, clays and the like.

The blending amount of the above-mentioned organic pigment-containing flake powder varies depending on the kind of the intended cosmetic, but it is used in the range of 1 to 80% by weight with respect to the solid component such as pigment, and particularly 2 The range of ˜50% by weight is preferred. If the content is less than this, there is a problem that the feeling of use is not improved, color development is not good, and conversely, the addition of more organic pigment-containing flake powder than the upper limit does not improve the coloring effect, It becomes difficult to adjust the color tone and improve the adhesion to the skin.

In order to improve the dispersibility of the organic pigment-containing flake powder used in the present invention in cosmetics and to improve the touch, the flaky powder is surface-treated and modified. You can do anything. For example, methyl hydrogen polysiloxane, reactive alkyl polysiloxane, metal soap, hydrogenated lecithin, acyl amino acid, acylated collagen metal salt selected from aluminum, magnesium, calcium, titanium, zinc, zirconium, iron, etc. When surface treatment is performed with a so-called hydrophobizing agent, the surface of the flake-shaped glass changes from hydrophilic to hydrophobic, so that it becomes more familiar with the oil agent added when formulating the cosmetic composition, resulting in a cosmetic product with a good feel. .

[0032]

Examples are shown below. Example-1 and Comparative Example-1 320 ml of ethanol, silicon tetraethoxide 14
80 ml, pure water 1200 ml, 0.8N nitric acid 200 ml
Were mixed and stirred at 30 ° C for 5 hours to obtain a uniform liquid (liquid A).
I got On the other hand, separately, Red No. 202 (Resor Rubin B
CA) (44 g) was added to 1000 ml of pure water, and the mixture was vigorously stirred while being irradiated with ultrasonic waves to obtain a red No. 202 dispersion liquid (B liquid). Solution B was added while stirring solution A, and red No. 202 was dispersed using a circulating sand mill. After that, the coating liquid was cured at 50 ° C. for about 20 hours. This liquid was sprayed in a mist form from a nozzle having a diameter of 2 mm, and the liquid was applied to the surface of a stainless steel plate having a thickness of 0.5 mm whose surface was polished and smoothed. This is dried at 150 ° C for about 2 minutes to peel off the applied gel film to form flakes.
It heat-processed at 20 degreeC for 24 hours. When the flakes were observed with a scanning electron microscope, the surface was smooth and the thickness was about 0.6.
μm. When the surface area of this flake was measured by the nitrogen adsorption method, the specific surface area was about 20 m ² / g,
It was a porous body having pores with a diameter of 8 nm or less. The content of Red No. 202 in the flakes was about 10% by weight.

The heat-treated flakes were crushed by a jet mill and classified to obtain a bright red flake powder (powder A) having an average particle diameter of about 14 μm. This flake powder is
They did not aggregate with each other, had slipperiness, and had a unique and excellent tactile sensation. When the elution of the organic pigment with respect to water and oil was observed, almost no elution of the organic pigment was observed.

Red No. 226 (Herringdon Pink CN) 1
35 g, 1000 ml of pure water, 100 ml of ethanol, and 2 g of polyoxyethylene glycerin monostearate (Nonion S-10 manufactured by NOF CORPORATION) were mixed and dispersed using a sand mill to obtain a red dispersion liquid. on the other hand,
Separately, silicon tetraethoxide 1480 ml, 0.1N
The mixture was mixed with 1600 ml of nitric acid, irradiated with ultrasonic waves for 30 minutes, and then cured at 50 ° C. for about 10 hours. This solution was mixed with the red color No. 226 dispersion described above, ultrasonic irradiation was carried out for 5 minutes, and further aged at 50 ° C. for about 2 hours to obtain a coating solution.
Flake formation, heat treatment, and pulverization classification were performed by the above-mentioned method to obtain red flake powder (powder B) having a red No. 226 content of about 25%, a thickness of about 0.7 μm, and an average particle size of about 15 μm.
The flaky powder did not aggregate with each other, had slipperiness, and had a unique and excellent tactile sensation. Also,
When the surface area of this flake powder was measured by the nitrogen adsorption method, the specific surface area was about 20 m ² / g and the diameter was 8 n.
It was a porous body having pores of m or less. When the elution of the organic pigment with respect to water and oil was observed, almost no elution of the organic pigment was observed.

Next, a lipstick was prepared with the following composition. Component-1 Blending amount (% by weight) ---------------------------------- Castor oil 35.0 Myristic acid Octyldodecyl 19.0 Isopropyl myristate 5.4 Lanolin 5.5 Beeswax 2.7 Candelilla wax 6.6 Carnauba wax 0.9 Ceresin 7.2

Component-2 blending amount (% by weight) -------------------------------------------- The above red 202 No.-containing flake powder (Powder A) 7.5 The above red No. 226-containing flake powder (Powder B) 4.6 Titanium dioxide 5.5

Component-3 Blending amount (% by weight) ----------------------------------..-- Perfume 0. 1 ------------------------------------------------

Component-1 was mixed and heated to 85 ° C. and melted. Component-2 was added to this melt, and the mixture was stirred and mixed. Furthermore, component-3 is added, mixed with stirring, poured into a mold, cooled, and molded into a stick shape to obtain a lipstick product-1 (Example-
1) was obtained.

Component-4 Amount of compounding (% by weight) ----------------------------------------- Red No. 202 0.8 Red No. 226 1.0 Mica 10.3 Titanium dioxide 5.5

Lipstick product-2 (Comparative Example-1) was obtained in the same manner as described above except that Component-4 was used instead of Component-2.

The above product is used by 20 panelists for 5 days, and the minimum point is 1 point and the maximum point is 5 points.
The results of the sensory tests evaluated are shown in Table 1.

[0042]

[Table 1] Table 1 =================================== Item The cosmetics of the present invention (lipstick products -1) Comparative Cosmetic (Lipstick Product-2) (Example-1) (Comparative Example-1) --------------- ------------- No. 4.7 3.0 -------------------------------------------- --- Adhesiveness 4.5 3.8 --------------------------------------------- Glossiness 4.3 3. 1 ----------------------------------------- Finishing feeling 3.9 2.2 --- −−−−−−−−−−−−−−−−−−−−−−−−−−−−−− Color Sensitivity 4.6 4.0 −−−−−−−−−−−−− −−−−−−−− ------------------------ Makeup mochi 3.7 3.3 ============================ ========

As described above, it was confirmed that the cosmetic composition of the present invention is excellent in spreadability (extendability) and stickiness (adhesion), has a good glossy feeling, has a good color development, and has a good finished feeling and makeup lasting. It was In addition, red No. 202-containing flake powder (powder A)
And the red 226-containing flake powder (powder B) is
It was observed that the color changed more vividly after being incorporated into the cosmetic. It is considered that this is because the fine pores of the powder A and the powder B are impregnated with an oily component such as castor oil to reduce light scattering due to the fine pores.

Example-2 and Comparative Example-2 Red 226 No. 9.1 g, Red No. 203 (Rake Red C) 0.6 g, Yellow No. 205 (Bentzine Yellow)
5.0 g, glycerin 2 g, 1-butanol 50 ml,
Ethanol 340 ml, pure water 2000 ml, silicon tetraethoxide 1480 ml, 0.8N nitric acid 200 ml
Were mixed using a sand mill and cured at 50 ° C. for about 20 hours to obtain a coating liquid. Flake formation, heat treatment, and pulverization classification were carried out by the method described in Example-1, and the organic pigment content was about 3.5.
%, A thickness of about 0.6 μm, and an average particle size of about 10 μm were obtained as red flake powder (powder C). This flake powder is
They did not aggregate with each other, had slipperiness, and had a unique and excellent tactile sensation. A small amount of the above flake powder,
When elution of the organic pigment was observed by adding it to water and oil, elution of the organic pigment was hardly observed.

Nail enamel was prepared with the following formulation. Component-5 Blending amount (% by weight) -------------------------------------------- Nitrocellulose 15.0 Phthal Acid-based alkyd resin 12.0 Dibutyl phthalate 4.0

Component-6 Blending amount (% by weight) -------------------------------- Butyl acetate 25 0.0 Ethyl acetate 7.0 Toluene 24.0 2-Propanol 6.0 Ethanol 2.0 1-Butanol 2.0

Component-7 Blending amount (% by weight) ------------------------------------ Containing flake powder (powder C) 3.0 ---------------------------------------------

Component-5 and component-6 were mixed and dissolved.
Component-7 was added to this, and the mixture was stirred and mixed to obtain NE product-1 (Example-2).

Ingredient -8 blending amount (% by weight) --------------------------------------- Red No. 226 0.065 Red No. 203 0.004 Yellow No. 205 0.036 Mica 2.895

NE product-2 (Comparative Example-2) was obtained by the same method as described above except that Component-8 was used instead of Component-7.

The above product is used by 20 panelists for 5 days, and the minimum point is 1 point and the maximum point is 5 points.
The results of the sensory tests evaluated are shown in Table 2.

[0052]

[Table 2] Table 2 ==================================== Item The cosmetic of the present invention (NE product -1) Comparative cosmetics (NE product-2) (Example-2) (Comparative example-2) ----------------------------------- ------------ No. 4.8 2.5 --------------------------------------- --- Tsuki 4.3 3.9 ----------------------------------------------- Applicability 4.5 1 .. 4 ---------------------------------------- Glossiness 4.7 3.0 ----- −−−−−−−−−−−−−−−−−−−−−−−−−−−−− Finishing feeling 4.5 1.2 −−−−−−−−−−−−− −−−−−−− −−−−−−−−−−−−−−−− Color Sensitivity 4.5 1.7 −−−−−−−−−−−−−−−−−−−−−−−−−− −−−−−−−−− Uniformity 4.6 1.3 =================================== ==

As described above, the cosmetic composition of the present invention is excellent in spreadability (extendability) and stickiness (adhesion), is easy to apply uniformly, has a good transparency and glossiness, has a good color development, and gives a finished feeling. It was confirmed to be excellent.

Example-3 and Comparative Example-3 Commercially available hydrous titanium oxide colloid TiO (OH) 2 (trade name: Titania sol CS-N, manufactured by Ishihara Sangyo Co., Ltd., content of titanium dioxide equivalent about 30% by weight, particle diameter) 30-60n
m, water dispersion) 120ml, 0.2N nitric acid 1900m
1, 1630 ml of silicon tetraethoxide and 1400 ml of ethanol were mixed and aged at 35 ° C. for about 50 hours. In this liquid, 12 g of Daidai No. 203 (Permanent Orange) and 1 of Red No. 228 (Permanent Red)
2 g were added and mixed, the organic pigment was uniformly dispersed using a sand mill, and further cured at 50 ° C. for 10 hours to obtain a coating liquid. Flaking is performed by the method described in Example-1,
The obtained flakes are treated under reduced pressure (about 1 Pa) at 150 ° C.,
Heat treatment was performed for 24 hours. Further, pulverization and classification were carried out by the method described in Example-1, and the organic pigment content was about 5% by weight (daidai No. 203 content was about 2.5% by weight, red No. 228 content was about 2.5% by weight), Titanium dioxide content of about 9.5
A yellow-orange flake powder (powder D) having a weight% of about 0.7 μm and an average particle size of about 12 μm was obtained. When the flaky powder was examined by an X-ray diffraction method, only anatase type titanium dioxide was detected and the matrix was in an amorphous state. Observation of the flakes with a transmission electron microscope revealed that titanium dioxide fine particles with a diameter of 30 to 60 nm were
It was observed that they were evenly distributed and located in the matrix. The flaky powder did not aggregate with each other, had slipperiness, and had a unique and excellent tactile sensation. When a small amount of the above flake powder was added to water and oil respectively and the elution of the organic pigment was observed, almost no elution of the organic pigment was observed.

A coating in which about 10% by weight of the flakes is mixed and dispersed in a vinyl resin (having a refractive index after curing of about 1.5) is applied on a substrate and dried to form a film having a thickness of about 0.15 mm. When the transmittance was measured with a spectrophotometer, it was confirmed that the ultraviolet ray transmittance at a wavelength of 350 nm or less was 5% or less, and the powder was a colored flake powder that effectively shielded ultraviolet rays.

Next, a powder foundation was prepared with the following composition. Component-9 Blending amount (% by weight) -------------------------------------------- The above organic pigment-containing flakes Powder (Powder D) 3.7 Talc 77.9 Mica 9.0 Titanium dioxide 5.4 Magnesium stearate 2.8 Silk powder 0.5

Ingredient -10 Blending amount (wt%) --------------- Squalane 0. 5 Sorbitan sesquioleate 0.1

Component-11 Blending amount (% by weight) -------------------------..-- Perfume 0. 1 ------------------------------------------------

Component-9 was mixed with a Henschel mixer.
Stir for 5 minutes. Stirring and mixing were performed while dripping the component-10 uniformly melted at 70 ° C. further,
After adding Component-11, the mixture was stirred and mixed for 1 minute and pulverized with an atomizer to obtain a powdered product-1 (Example-3).

Component-12 Blending amount (% by weight) -------------------------------------- No. 0.1 Red No. 228 0.1 Talc 80.4 Mica 9.7 Titanium dioxide 5.5 Magnesium stearate 2.9 Silk powder 0.6

Component-12 was stirred using a Henschel mixer for 10 minutes. Stirring and mixing were carried out while dropwise adding Component-10, which was uniformly melted at 70 ° C.
Further, after adding Component-11, the mixture was stirred and mixed for 1 minute and pulverized with an atomizer to obtain a powder product-2 (Comparative Example-3).

These product samples were irradiated with a 300 W xenon lamp from a distance of about 15 cm for 100 hours, and the change in color tone before and after irradiation was measured using a color difference meter (CR-300 manufactured by Minolta Camera Co., Ltd.). As a result, the color difference ΔE was 2.4 for powder product-1 (Example-3) and 12.6 for powder product-2 (Comparative Example-3). Therefore,
The cosmetic of the present invention has excellent light resistance.

The above product was given to 20 (female) panelists for 10 persons.
Table 3 shows the results of the sensory test evaluated by a five-stage method in which the sample was used for a day and the minimum score was 1 and the maximum score was 5.

[0064]

[Table 3] Table 3 ==================================== Item Cosmetics of the present invention (powder products -1) Comparative cosmetics (powdered product-2) (Example-3) (Comparative example-3) ------------------------------------------------------------------------------------------ ------------ No. 4.6 4.6 1.9 --------------------------------------------------------------------------------------------------------------------------------------- --- Tint 4.4 3.4 ------------------------------------ Glossiness 4.5 2 .. 2 ---------------------------------------- Color Sensitivity 4.4 3.9 ----- −−−−−−−−−−−−−−−−−−−−−−−−−−−−−− Makeup Mochi 4.7 2.6 ============ =========== =============

As described above, it was confirmed that the cosmetics of the present invention are excellent in spreadability (extendability) and stickiness (adhesion), have a good glossy feeling, have a good color development, and have a good makeup lasting.

[0066]

The above detailed description and embodiments of the present invention,
As is clear in Comparative Examples, the organic pigment-containing flake powder of the present invention has an organic pigment encapsulated and fixed by an inorganic oxide, so that the organic pigment is eluted from the flakes,
Almost no detachment occurs, and a cosmetic composition containing this is a stable product with excellent bleed resistance, water resistance, and sweat resistance. Also, since the organic pigment does not touch the skin directly,
Since it has improved non-allergenicity, does not stain the skin and nails, and has a flake shape, the organic pigment does not clog the sweat glands and pores, and is a safe product without skin irritation. Further, since the organic pigment is contained in the inorganic oxide, the stability of the organic pigment is improved, the light resistance and heat resistance are high, and a product having a vivid color and a preferable color tone is obtained. Furthermore, since the organic pigment-containing flake powder does not aggregate with each other and its surface is smooth and exhibits good slipperiness, it has good extensibility (spreading), dispersibility, adhesiveness, and touch feeling. It will be an excellent product.

Claims (5)

[Claims] 1. A metal oxide flake powder containing 0.5 to 40% by weight of an organic pigment. 2. The organic pigments are Red No. 226, Red No. 202 described in Ordinance No. 30 of the Ministry of Health and Welfare on August 31, 1941.
The flake powder according to claim 1, which is at least one selected from Red No. 203 and Red No. 204. 3. The metal oxide is silica, titania,
The flake powder according to claim 1 or 2, which is at least one selected from the group consisting of alumina and zirconia. 4. A solution containing a hydrolyzable and polycondensable organometallic compound, an organic pigment, water, and an organic solvent is applied onto a substrate having a smooth surface, and the substrate is peeled off to obtain a layer of 80 to 25.
A method for producing a metal oxide flake powder, which comprises heating at 0 ° C. for 5 minutes to 24 hours. 5. A cosmetic comprising the flaky powder according to any one of claims 1 to 3.