JP5081422B2 - White composite powder and cosmetics containing the same - Google Patents

Description

  The present invention relates to a method for producing a novel white composite powder having no pearly luster in which titanium dioxide particles are fixed on the surface of α-alumina plate-like particles, and a cosmetic containing the novel white composite powder.

  Conventionally, titanium dioxide has been used in various industrial fields as a white pigment because of its high refractive index. Titanium dioxide has different hiding properties and whiteness depending on its particle size and crystal form. So-called pigment-grade titanium oxide having an average particle size of about 250 nm has particularly high hiding properties, and so-called fine particle oxidation of about 10 to 40 nm. Titanium has a high UV protection effect. These pigment grade titanium dioxide and fine particle titanium oxide generally have an angle dependency that the reflectance in the regular reflection direction is higher than other angles, and the intensity of the reflected light varies depending on the viewing angle (light receiving angle). . That is, when titanium dioxide is dispersed in a resin to form a coating film, there is a drawback that it is difficult to control the texture of the coating film because it has a high gloss when viewed from the front and it is difficult to feel the gloss in an oblique direction. Therefore, it is desired to develop a white pigment capable of exhibiting a beautiful white color regardless of the viewing angle while maintaining an appropriate concealing property and having little angle dependency on the intensity of reflected light. In general, since pigment grade titanium oxide has high cohesive strength, it is necessary to apply various surface treatments and dispersion techniques. Therefore, development of a white pigment having low cohesive strength is desired.

In addition to being used alone, titanium dioxide particles are also used by adhering to the surfaces of the base particles. For example, a mica titanium pigment obtained by coating mica with titanium dioxide particles has been known for a long time (Patent Document 1). This mica titanium pigment has a characteristic that it is smooth due to the shape of the substrate being smooth, and has a pearly luster due to the optical properties of the substrate and the coating layer. It is used in many industrial fields including cosmetics. However, the titanium dioxide composite powder represented by titanium mica also has a large angle dependency as described above. For example, if a large amount of titanium mica is contained in the foundation, unnatural luster and shine will be felt.

On the other hand, there is proposed a mica titanium pigment having no pearly luster and a makeup cosmetic containing the pearly luster for eliminating the messiness and naturalness (Patent Document 2). From the viewpoint of physical properties and shape, the above-described decrease in angle dependency cannot be expected. Further, alumina titanium having interference color such as pearly luster formed by using plate-like particles made of α-alumina as matrix particles covering titanium dioxide and uniformly covering a titania layer having a thickness of 10 to 500 nm. A pigment has been proposed (Patent Document 3), but this also has a problem that the angle dependency is large.
Japanese Patent Publication No. 43-25644 Japanese Patent No. 2559037 Japanese Patent No. 3633710

  The present invention is a white composite powder that maintains a moderate concealing property possessed by titanium dioxide, has a small angle dependency on the intensity of reflected light, can exhibit a beautiful white color regardless of the viewing angle, and has a low cohesive force. The purpose is to provide a body.

  As a result of intensive studies, the present inventors fixed a specific amount of titanium dioxide on the surface of α-alumina plate-like particles having a specific particle diameter, thickness and aspect ratio so as not to have pearl luster. Thus, it is found that a composite powder having an appropriate hiding property and a beautiful white color can be obtained regardless of the viewing angle, and that this composite powder has high lubricity and low cohesion. The present invention has been completed.

That is, the present invention is based on α-alumina plate-like particles having an average particle diameter of 0.5 to 20 μm, an average thickness of 0.03 to 0.35 μm, and an aspect ratio (average particle diameter / average thickness) of 15 to 50. And titanium dioxide particles having an average particle diameter of 0.001 to 0.5 μm are fixed so as to be scattered on the surface of the mother body to form irregularities on the surface, or layered on the surface of the mother body and it is fixed so that the surface of the layer to form irregularities, and the amount sticking of the titanium dioxide particles is 30 to 50 wt% (white composite powder to) white color composite powders you being a It is. Further, the present invention is a cosmetic in which the white color composite powder this.

  The white composite powder of the present invention has an appropriate concealing property and has little angle dependence on the intensity of reflected light, that is, exhibits a beautiful white color without shine and unnatural gloss regardless of the viewing angle. . Furthermore, it is a white composite powder having excellent lubricity and low cohesion. In addition, cosmetics containing this white composite powder have little so-called whitening caused by camera flash or strong sunlight, and exhibit a beautiful white color regardless of the viewing angle. Moreover, the cosmetic compounded with the white composite powder can form a highly uniform decorative film.

Hereinafter, the present invention will be described in detail.
The white composite powder of the present invention uses plate-like particles made of α-alumina as a base. The α-alumina plate-like particles have an average particle diameter of 0.5 to 20 μm, an average thickness of 0.03 to 0.35 μm, and an aspect ratio (average particle diameter / average thickness) of 15 to 50. Preferred are α-alumina plate-like particles having an average particle diameter of 1.5 to 2.5 μm, an average thickness of 0.05 to 0.10 μm and an aspect ratio of 15 to 35. In the present specification, the average particle diameter or the average thickness of the particles is measured by measuring the major axis, minor axis, and thickness of an arbitrary ten particles by observing the particle group with a scanning electron microscope. The particle diameter was 10 arithmetic averages (major axis + minor axis) / 2, and the thickness was 10 arithmetic averages.

  In the white composite powder of the present invention, when the average particle diameter of the α-alumina plate-like particles used as the base is less than 0.5 μm, the white composite powder is not preferable because of poor lubricity. And when these white composite powder is mix | blended with cosmetics, the smoothness at the time of use may be lacking. Further, when the average particle diameter of the α-alumina plate-like particles exceeds 20 μm, the reflectance in the regular reflection direction increases, that is, the angle dependency of the intensity of the reflected light increases, resulting in unnatural gloss and gloss. Not only is it unfavorable because it becomes strong, but it is not preferred when it is rough and blended into cosmetics.

Further, when the average thickness of the α-alumina plate-like particles is less than 0.03 μm, the strength of the matrix is lowered. Therefore, when the white composite powder of the present invention is blended in the cosmetic, the particles are caused by mechanical force or the like. May occur and the uniformity of the particles may be impaired. For this reason, the uniformity of the decorative film may be impaired or rough, which is not preferable. Furthermore, since the light scattering property is reduced, the reflectance in the specular reflection direction is increased, and there is a case where the angle dependency such that the whiteness varies depending on the angle when viewed as a decorative film is not preferable. Moreover, when average thickness exceeds 0.35 micrometer, the smoothness of the coating film at the time of setting it as a coating film with poor lubricity is lost.

In addition, when the aspect ratio exceeds 50, the strength of the base material is reduced, and thus when the white composite powder of the present invention is blended in various industries, the particles are broken by mechanical force and the uniformity of the particles. Since the film is damaged, the uniformity of the film when it is used as a coating film may be impaired or rough. Further, the hiding power is lowered and the reflectance in the regular reflection direction is increased, and the pigment intended by the present invention cannot be obtained. When the aspect ratio is less than 15, the hiding power becomes too high, the appropriate hiding power is lost, and the smoothness of the coating film is lost when the coating film has poor lubricity.

  The α-alumina plate-like particles used in the present invention can be produced by a known alumina production method. Typical production methods include ammonium alum pyrolysis method, organometallic hydrolysis method, ethylene chlorohydrin method, medium spark discharge method of aluminum, ammonium aluminum carbonate (AACH) pyrolysis method, improved buyer method, There is a gas phase oxidation method or the like, and the Bayer method is the most common method for industrially producing in large quantities. In the present invention, α-alumina plate-like particles within the above-mentioned average particle diameter, average thickness, and aspect ratio are used. Generally, the alumina particles obtained by the various production methods described above are fine particles, It tends to be indefinite. In consideration of the control of the particle diameter of alumina, the control of the thickness for increasing the aspect ratio, the purity of alumina, the smoothness of the alumina surface, etc., the production method described in Japanese Patent No. 3759208, that is, aluminum hydroxide or alumina A crystallization inhibitor containing at least phosphate ions is added to the hydrate, and the heating rate is within a range of 5 to 0.3 ° C./min, a temperature of 350 ° C. or higher, and a pressure of 50 to 200 atm. A method of synthesizing and producing alumina particles having a single crystal of α-alumina and a hexagonal plate-like crystal structure is preferable.

  In the white composite powder of the present invention, titanium dioxide is fixed to the surface of the base α-alumina plate-like particles. The amount of titanium dioxide to be fixed is 30 to 50% by mass of the white composite powder. When the fixing amount is less than 30% by mass, the hiding power is insufficient and the object of the present invention cannot be achieved. When the amount of fixing exceeds 50% by mass, it is difficult to fix uniformly due to the relationship with the surface area of the matrix. In addition, when titanium dioxide is fixed to the surface of the α-alumina plate-like particles by precipitation, if the fixed amount exceeds 50% by mass, excess titanium dioxide precipitates as crystals or as a multilayer on the composite powder surface. In many cases, crystals of titanium dioxide are fixed. In such a case, although it has hiding power and optical characteristics, it has defects such as lack of uniformity when it is used as a decorative coating film, causing roughness, and further increasing cohesion.

In the present invention, as will be described later , titanium dioxide is fixed to the surface of the base α-alumina plate-like particles so as not to have pearl luster. According to the present invention, specific plate-like particles called α-alumina plate-like particles having an average particle diameter of 0.5 to 20 μm, an average thickness of 0.03 to 0.35 μm, and an aspect ratio of 15 to 50 are used as a mother powder. By fixing the above-mentioned specific amount of titanium dioxide on the surface without causing pearly luster, a white composite powder with excellent concealment, no angle dependency of reflected light, and low cohesion is obtained. It is done.

The white composite powder of the present invention has a hiding power, the white composite powder is uniformly dispersed in a lacquer at a concentration of 10% by mass, and the dispersion is applied to a white plate and a blackboard with a 50 μm doctor blade and dried. When each Y value (value indicating the light brightness of the CIE standard color system) was measured with a color difference meter, the ratio of Y value (on the blackboard) / Y value (on the white plate) was 0.00. What is 5-0.8 white composite powder is preferable.

Further, the white composite powder of the present invention is applied to the adhesive surface of the translucent adhesive tape with a brush with respect to the angle dependency of the reflected light, and the background of the blackboard is D65 light source with an incident angle of 45 °. And a white composite whose spectral reflectance when measured with a variable angle spectrophotometer is 70% or more of the spectral reflectance in regular reflection at any angle within the range of the light receiving angle of -75 ° to 75 °. What is a powder is preferable.

The white composite powder of the present invention does not have pearl luster. That is, the composite powder obtained by fixing the titanium dioxide on the surface of the α- alumina plate-like particles is not Na has a pearlescent. Pearl luster refers to the property of reflecting light in a certain direction and emitting various colors like a rainbow. Whether or not the white composite powder has a pearly luster can be easily determined visually. And it can achieve in order not to have a pearl luster by making the surface of the white composite powder after fixing titanium dioxide form an unevenness | corrugation. For example, the titanium dioxide particles may be fixed so as to be scattered on the surface of the matrix α-alumina plate-like particles to form irregularities, or the titanium dioxide particles are layered and the surface of the layer is irregular. It may be fixed so that The size of the titanium dioxide particles are flat Hitoshitsubu径0.001 to 0.5 [mu] m. In order to fix the titanium dioxide particles to the surface of the matrix α-alumina plate-like particles in a concavo-convex manner, a known method can be used. For example, there are a method performed by hydrolysis of titanyl sulfate or titanium tetrachloride, a method performed by direct oxidation of titanium tetrachloride, and a method performed by hydrolysis of titanium alkoxide.

  There are roughly two methods for producing a white composite powder having no pearl luster by a method of hydrolysis of titanyl sulfate. The first method is a method in which a titania layer to be fixed is roughly adhered as large grains, specifically, a method in which a titanyl sulfate solution having a relatively high concentration is rapidly heated and rapidly hydrolyzed. The second method is a method in which the titania layer to be fixed is closely attached as small particles, specifically, a method in which a titanyl sulfate solution having a relatively low concentration is gradually heated and hydrolyzed under mild conditions. It is done. In any method, the solid product obtained is separated and fired at a baking temperature of 600 to 900 ° C. The smoothness of the surface of the white composite powder is different between the first method and the second method, and the method of hydrolyzing under the mild conditions described in the second method above provides the surface smoothness. Is more preferable.

  A method performed by hydrolysis of titanyl sulfate will be specifically described. The matrix α-alumina plate-like particles are dispersed in water, and titanyl sulfate is added to and mixed with this dispersion, and then heated to a boiling point to hydrolyze titanyl sulfate, and then filtered and dried. In this case, the aqueous dispersion concentration of α-alumina plate-like particles is 10 to 50 g / L, the amount of titanyl sulfate added to this dispersion is 100 to 300 g / L, and the temperature rise until boiling is 0.5 to 5 ° C. / Min and the boiling temperature maintenance time is preferably 2 to 4 hours. The product obtained by drying is fired at a baking temperature of 600 to 900 ° C.

  The white composite powder of the present invention can be blended in various compositions such as cosmetics, paints, inks (toners), plastics, fibers, rubbers, etc., and can be used as white pigments or various fillers. . As a preferred embodiment using the white composite powder of the present invention, in addition to the above-mentioned optical characteristics, cosmetics, especially makeup cosmetics that require blending of white pigments due to characteristics such as smoothness and low cohesive force. Is particularly preferred.

  The blending amount of the white composite powder in the cosmetic of the present invention is desirably 0.1% by mass to 30% by mass, and particularly preferably 1% by mass to 10% by mass. When the blending amount is less than the preferred range, effects such as low optical properties and low cohesive strength of the white composite powder are not seen, and when the blending amount exceeds the preferred range, noticeable white is conspicuous, and the finish of the cosmetic is It is not preferable. Depending on the purpose, surface treatment with known substances such as metal oxides, metal hydroxides, fluorine compounds, silicone compounds, metal soaps, waxes, fats and oils, hydrocarbons, resins, silica, alumina, zirconia, Surface modification with various inorganic metals or metal oxides such as iron oxide, and further, it can be used in combination with various dispersants.

  In addition to the essential components described above, the cosmetics of the present invention include components such as hydrocarbon oils, ester oils, vegetable oils, silicone oils, silicone derivatives, etc., inorganic pigments, organic pigments, Powders such as extender pigments and their silicone-treated and fluorine-treated products, surfactants, water, polyhydric alcohols, lower alcohols, water-soluble polymers, aqueous components such as humectants, sugars, UV absorbers, oxidation An inhibitor, an antiseptic, an enzyme, a refreshing agent, a pigment, a fragrance, and the like can be blended within a range that does not hinder the effects of the present invention.

  The oil component will be described in more detail. The oil component is not particularly limited as long as it is an oil agent used in ordinary cosmetics, and it may be of any origin, such as animal oil, vegetable oil, synthetic oil, and properties of solid oil, semi-solid oil, liquid oil, volatile oil, etc. Examples thereof include oils such as hydrocarbons, fats and oils, waxes, hardened oils, ester oils, silicone oils, fluorine oils, and lanolin derivatives. Specifically, paraffin wax, ceresin wax, ozokerite, microcrystalline wax, molasses, montan wax, Fischer Trops wax, polyethylene wax, liquid paraffin, squalane, petrolatum and other hydrocarbons, carnauba wax, beeswax, lanolin wax, candelilla Natural products such as glyceryl tribehenate, jojoba oil, pentaerythritol ester of rosin acid, isopropyl myristate, glyceryl trioctanoate, diglyceryl triisostearate, oils such as olive oil, castor oil, mink oil, lanolin Lanolin derivatives such as fatty acid isopropyl, silicone oil such as dimethylpolysiloxane, silicone wax, methylphenylpolysiloxane, decamethylcyclopenta Rokisan, cyclic silicones such as octamethylcyclotetrasiloxane, perfluoro decane, include fluorine-based oils of perfluoro octane etc., can be used more than these one or two.

  As the powder component, any powder can be used as long as it is used in ordinary cosmetics, such as a spherical shape, a plate shape, a needle shape, a haze shape, a fine particle, a particle size such as a pigment grade, It is not particularly limited by the particle structure such as porous or nonporous, and examples thereof include inorganic powders and composite powders. Specifically, titanium dioxide, iron-doped titanium oxide, titanium dioxide oxide sintered body, cerium oxide, talc, mica, synthetic mica, iron-containing synthetic mica, kaolin, sericite, magnesium carbonate, calcium carbonate, aluminum silicate , Magnesium silicate, calcium silicate, zinc oxide, bengara, yellow iron oxide, black iron oxide, black titanium oxide, barium sulfate, ultramarine, conger, mica titanium, iron oxide mica titanium, etc., one or two of these More than seeds can be used. These powders include dimethylpolysiloxane, methylhydropolysiloxane, trimethylsiloxysilicic acid, alkyl-modified silicone, acrylate silicone and other silicone compounds, perfluoropolyether phosphoric acid, perfluoroalkyl phosphoric acid, fluorine-modified silicone. The surface treatment may be performed with a conventionally known compound such as a fluorine compound such as zinc soap, metal soap such as zinc laurate, lecithin, ester oil, and wax.

  The cosmetic of the present invention can be applied to all cosmetics that can be blended with powders such as eye color, eyebrow, foundation, blusher, white powder, base, emulsion, cream, etc. It is a makeup cosmetic that must contain a white pigment such as titanium, and includes eye color, eyebrow, foundation, blusher, white powder, and groundwork.

  The dosage form of the cosmetic of the present invention is not particularly limited as long as the color tone of the white pigment has a cosmetic effect, but is preferably an oily cosmetic, a solid powder cosmetic, particularly a solid powder cosmetic. The form of the cosmetic of the present invention is not particularly limited, and may be any of powder, liquid, paste, emulsion, cream, gel, solid and the like.

Hereinafter, the present invention will be described in more detail with reference to examples.
Example 1.
Using aluminum hydroxide as a starting material, the particle size was adjusted to an average particle size of 1.0 μm by pulverizing with a ball mill or the like in advance. This and water are mixed and a 50 mass% slurry is created. In this slurry, 5.0 × 10 ⁻³ mol of phosphoric acid aqueous solution was added as phosphate ions to aluminum hydroxide. The temperature was maintained at 600 ° C. and 150 atm for 3 hours at a temperature rising rate of 0.5 ° C./min. After cooling the container, the product is purely washed with water, sufficiently filtered, and dried in a dryer at 100 ° C. for 12 hours to obtain an α-alumina plate having an average particle diameter of 2.0 μm, an average thickness of 0.08 μm, and an aspect ratio of 25. Particles were obtained.
Next, the α-alumina plate-like particles were added and dispersed in water with stirring. To this, an aqueous solution of titanyl sulfate was added and mixed at room temperature. After that, heating took about 90 minutes to reach the boiling point, and the boiling point was maintained for another 4 hours. Thereafter, filtration and washing were repeated by a conventional method, and then the obtained cake was dried at 105 ° C. for 5 hours, and further calcined at 850 ° C. for 4 hours to give 40% by mass of titanium dioxide to α-alumina plate-like particles. A fixed white composite powder was obtained (relative to the white composite powder). An electron micrograph of the surface of the white composite powder is shown in FIG.

Example 2,
A white composite powder in which 40% by mass of titanium dioxide was fixed to α-alumina plate-like particles having an average particle diameter of 2.0 μm, an average thickness of 0.04 μm, and an aspect ratio of 50 was prepared in the same manner as in Example 1.
Example 3
A white composite powder in which 30% by mass of titanium dioxide was fixed to α-alumina plate-like particles having an average particle diameter of 5.0 μm, an average thickness of 0.10 μm, and an aspect ratio of 50 was prepared in the same manner as in Example 1.

Comparative Example 1
A white composite powder in which 15% by mass of titanium dioxide was fixed to α-alumina plate-like particles having an average particle diameter of 5.0 μm, an average thickness of 0.07 μm, and an aspect ratio of 71 was prepared in the same manner as in Example 1.
Comparative Example 2
A white composite powder in which 40% by mass of titanium dioxide was fixed to α-alumina plate-like particles having an average particle diameter of 5.0 μm, an average thickness of 0.07 μm, and an aspect ratio of 71 was prepared in the same manner as in Example 1.
Comparative Example 3
60 parts of α-alumina plate-like particles (α-alumina plate-like particles of Example 1) having an average particle diameter of 2.0 μm and an average thickness of 0.08 μm and 40 parts of titanium oxide (average particle diameter of 0.25 μm) are mixed in Wonder Blender. (Osaka Chemical Co., Ltd.) was mixed for 10 seconds. This is a mixed powder that is not complexed.

<Evaluation of concealment>
White composite powder of Examples 1-3 above, white composite powder of Comparative Examples 1-2, mixed powder of Comparative Example 3, mica titanium pigment, pigment grade titanium dioxide, fine particle titanium dioxide and α-alumina plate-like particles The concealability was investigated.
1 g of each sample is dispersed in 9 g of lacquer, uniformly coated with a 50 μm doctor blade on a white plate and a blackboard, and dried to obtain a standard product. Each Y value (indicating the light brightness of the CIE standard color system) Value) was measured with a color difference meter, and the ratio of Y value (on the blackboard) / Y value (on the white plate) was determined to evaluate the concealability. The results are shown in Table 1. Moreover, the hiding power of the specimen was judged visually according to the following judgment criteria. The results are also shown in Table 1.
(Criteria)
A: High hiding power.
○: There is moderate hiding power.
X: The hiding power is low.

As shown in the results of Table 1, the white composite powder of the present invention has an appropriate hiding power different from that of conventional titanium dioxide.

<Evaluation of angle dependence of reflected light>
White composite powder of Examples 1-3 above, white composite powder of Comparative Examples 1-2, mixed powder of Comparative Example 3, mica titanium pigment, pigment grade titanium dioxide, fine particle titanium dioxide and α-alumina plate-like particles The angle dependence of the reflected light was investigated.
Using a brush, apply each sample evenly to the adhesive surface of a translucent adhesive tape (5cm x 5cm 3M No. 1526) to obtain a standard, with a D65 light source and an incident angle of -45 ° against a blackboard background Using a variable angle spectrophotometer (GSP-1B type, manufactured by Murakami Color Engineering Co., Ltd.), the reflectance was measured every 5 °. Table 2 shows the reflectivity of 0 ° and the reflectivity of 45 °. In addition, the spectral reflection characteristics of this sample are shown in FIG. The blank portion in FIG. 2 is a portion that cannot be measured because the light receiving portion and the light source overlap.

From the results shown in Table 2, the white composite powder of the present invention has a 45 ° reflectance, that is, a reflectance in the regular reflection direction is lower than that of conventional titanium dioxide, and is compared with a reflectance of 0 ° (value of 0 ° / 45 °). From the result of), it can be seen that the gloss and gloss do not change greatly depending on the viewing angle. Further, it can be seen from FIG. 2 that gloss and gloss are suppressed because there is a feature that does not have a large peak in the regular reflection direction at a light receiving angle of 45 °.

<Evaluation of powder cohesion>
White composite powder of Example 1, mixed powder of Comparative Example 3, mixed powder (Sample 1) with different mixing ratio of Comparative Example 3, pigment grade titanium dioxide (Sample 2) and plate-like alumina (Sample 3) The cohesive strength of the powder was evaluated using the concealment rate.
2 g of each sample is placed in a round metal pan for cosmetics (diameter 32 mm, depth 3 mm), molded into a solid state with a pressing pressure of 200 Kg / cm ² (2 seconds), and the pressed state is used to measure the concealment rate. Provided. That is, each sample was printed out from this pressed state using a cosmetic brush, and about 0.1 g was uniformly applied to the adhesive surface of a translucent adhesive tape (5 cm × 5 cm 3M No. 1526). On the other hand, each of the above samples was directly subjected to measurement of the powder concealment rate. That is, about 0.1 g of each sample was uniformly applied to the pressure-sensitive adhesive surface of a translucent pressure-sensitive adhesive tape (5 cm × 5 cm 3M No. 1526) in a powder state with a cosmetic brush.

After the uniform coating, the excess powder is removed, and the coated body is covered with the black and white of the concealment test paper on the back side, and color measurement is performed with a spectral color difference meter (SZ-Σ90 made by Nippon Denshoku Industries Co., Ltd.). The difference ΔL between the L value (white scene) and the L value (black scene) was obtained. Translucent adhesive tape only [Delta] L _BL (blank) was a transmittance ratio ΔLSAMPLE / ΔL _BL with tape DerutaLSAMPLE after application of each powder sample. Then, [(1−transmittance) × 100] was defined as the concealment rate. Table 3 shows the measurement result of the concealment ratio of each sample in the pressed state and the measurement result of the concealment ratio in the powder state. A sample having a larger difference between the concealment rate in the powder state and the concealment rate in the pressed state was determined to have a stronger cohesion force of the powder by the press.

The white composite powder of Example 1 has much less powder agglomeration by pressing than pigment grade titanium dioxide (Sample 2). Moreover, even if the white composite powder of Example 1 and the mixed powder of Comparative Example 3 in which the ratio of α-alumina plate-like particles and titanium dioxide particles is the same, the mixed powder of Comparative Example 3 is Compared with the white composite powder of Example 1, the cohesive force was high.

As is clear from Tables 1, 2, and 3 and FIG. 2, the white composite powders of Examples 1 to 3 are white composite powders that have a small hiding power and angle dependency of reflected light intensity depending on angles. It was. In particular, the white composite powder of Example 1 is the most preferable example because the angle dependency of reflected light intensity is extremely small. As shown in FIG. 1, in the white composite powder of Example 1 of the present invention, titanium dioxide is fixed on the surface of the base α-alumina plate-like particles, and the surface of the titanium dioxide crystals is precipitated. Is uneven. Moreover, the white composite powders of Examples 1 to 3 were excellent in lubricity and low in cohesion as compared with conventional titanium dioxide. In contrast, the white composite powder of Comparative Example 1 lacked the hiding power although the angle dependency of the reflected light was small. Although Comparative Example 2 has an appropriate hiding power, the reflectance in the regular reflection direction is higher than the 0 ° direction, and the angle dependency of reflected light is large. The comparative example 3 has similar characteristics to the white composite powder of the present invention in hiding power and angle dependency, but in the high lubricity and low cohesive force of the present invention. It was not as good as the white composite powder.

Example 4: Powder foundation (component) (%)
1. The remaining amount of talc Sericite 20
3. Fluorophlogopite 30
4). Titanium dioxide 5
5. Titanium dioxide / iron oxide sintered product 3
6). Zinc oxide 2
7). Plate-like barium sulfate 2
8). (Vinyl dimethicone / methicone silsesquioxane)
Cross polymer * 5 3
9. Nylon powder 2
10. Bengala 0.3
11. Yellow iron oxide 1
12 Black iron oxide 0.2
13. White composite powder described in Example 1 10
14 Squalane 5
15. Methylphenyl polysiloxane * 6 3
16. Paramethoxycinnamic acid-2-ethylhexyl 3
17. Heavy liquid isoparaffin 2
18. Dioctyl succinate 2
* 5 KSP-100 Shin-Etsu Chemical Co., Ltd. * 6 Silicon KF-54 Shin-Etsu Chemical Co., Ltd.

(Manufacturing method)
A: Components 1 to 13 are mixed and dispersed.
B: Components 14 to 18 mixed and dissolved are added to [A] and mixed and dispersed.
C: [B] was press-molded into a metal pan to obtain a solid powder powder foundation.
The powder foundation of Example 4, which is an embodiment of the present invention, is an excellent cosmetic material that forms a clean cosmetic film that does not depend on the viewing angle and a uniform cosmetic film that has little powder aggregation and has a smooth feeling of use. It was.

Example 5: Face powder (component) (%)
1. The remaining amount of talc Sericite 10
3. Fluorophlogopite 50
4). Fluorine phlogopite 10
5. White composite powder of Example 2 1
6). (Diphenyl dimethicone / vinyl diphenyl dimethicone / silsesquioxane) cross polymer 5
7). Silicic anhydride (spherical) 2
8). Red No. 202 0.3
9. Ultramarine 0.2
10. Bengala coated mica titanium 5
11. Titanium oxide coated glass powder 5
12 Preservative appropriate amount13. Tridecyl trimellitate 1
14 Pentaphenyltrimethyltrisiloxane 3
15. (Vinyl Dimethicone / Lauryl Dimethicone)
Cross polymer 0.5
16. Glyceryl tri-2-ethylhexanoate 1

(Manufacturing method)
A: Components 1 to 12 are mixed and dispersed.
B: The components 13 to 16 which are uniformly mixed are added to [A] and mixed and dispersed.
C: [B] was filled in a container to obtain a powdery face powder.
The face powder of Example 5, which is an embodiment of the present invention, is an excellent cosmetic material that forms a clean cosmetic film that does not depend on the viewing angle and a uniform cosmetic film that has less powder aggregation and has a smooth feeling of use. It was.

Example 6: Oily eye color (component) (%)
1. White composite powder described in Example 3 5
2. Fluorotetrasilicon mica 20
3. Spherical polymethyl methacrylate powder 5
4). Silicic anhydride (spherical) 2
5. Yellow iron oxide 1.5
6). Ultramarine 1.5
7). Black iron oxide 0.2
8). Mica titanium 12
9. Preservative appropriate amount10. 10. remaining amount of glyceryl tri-2-ethylhexanoate Pentaphenyltrimethyltrisiloxane 10
12 Paramethoxycinnamic acid-2-ethylhexyl 3
13. Dimethylpolysiloxane 3
14 Ceresin wax 4
15. Polyethylene wax 5
16. Microcrystalline wax 3

(Manufacturing method)
A: Components 10 to 16 are heated to 85 ° C. and mixed and dissolved.
B: Components 1 to 9 are added to [A] and uniformly dispersed.
C: [B] was heated again to 85 ° C. and filled in a metal pan to obtain an oily eye color.
The oily eye color of Example 6, which is an embodiment of the present invention, is an excellent cosmetic material that forms a clean cosmetic film that does not depend on the viewing angle and a uniform cosmetic film with less powder agglomeration and has a smooth feeling of use. there were.

Electron micrograph of the white composite powder of Example 1 Example of the present invention, comparative example and spectral reflection characteristic graph of titanium dioxide

  In FIG. 1, the horizontal axis represents the angle, and the vertical axis represents the spectral reflectance.

Claims (7)

An α-alumina plate-like particle having an average particle diameter of 0.5 to 20 μm, an average thickness of 0.03 to 0.35 μm, and an aspect ratio (average particle diameter / average thickness) of 15 to 50 is used as a base material, and the average particle diameter is 0. 0.0001 to 0.5 μm of titanium dioxide particles are fixed so as to be scattered on the surface of the base and form irregularities on the surface, or layered on the surface of the base and the surface of the layer is uneven A white composite powder characterized in that the titanium dioxide particles are fixed to form 30 to 50% by mass (relative to the white composite powder). The average particle diameter of the matrix α-alumina plate-like particles is 1.5 to 2.5 µm, the average thickness is 0.05 to 0.10 µm, and the aspect ratio is 15 to 35 . white color composite powder. When the matrix α-alumina plate-like particles are added with a crystal inhibitor containing at least phosphate ions in aluminum hydroxide or alumina hydrate, the rate of temperature rise is within a range of 5 to 0.3 ° C./min. temperature 350 ° C. or higher, and hydrothermal synthesis at a pressure range of 50 to 200 atmospheres, the crystal structure is alumina particles having a hexagonal plate-like shape with α- alumina single crystal according to claim 1 or 2 white color composite powders according . Α-alumina plate-like particles having an average particle diameter of 0.5 to 20 μm, an average thickness of 0.03 to 0.35 μm, and an aspect ratio (average particle diameter / average thickness) of 15 to 50 are dispersed in water. The white solution according to any one of claims 1 to 3, wherein titanyl sulfate is added to and mixed with the dispersion, and then heated until boiling to hydrolyze titanyl sulfate, and then filtered, dried, and calcined. Manufacturing method of color composite powder. The method of manufacturing a white color composite powder according to claim 4, alpha-water dispersion concentration of the alumina plate-like particles is 10 to 50 g / L, amount of titanyl sulfate to the dispersion 100 to 300 g / L The white temperature according to claim 4, wherein the temperature rise rate until boiling is 0.5 to 5 ° C / min, the boiling temperature maintaining time is 2 to 4 hours, and the firing temperature is 600 to 900 ° C. Manufacturing method of color composite powder. Cosmetics containing white color composite powder according to any one of claims 1-3. The cosmetic according to claim 6, wherein the cosmetic is a makeup cosmetic.

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