JP2003342127A - Composite powder, cosmetic containing the same and method for producing composite powder - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain composite powder that when blended in a cosmetic, ameliorates skin unevenness and color deficiency, realizes natural finish, a cosmetic containing the same and to provide a method for producing the composite powder. <P>SOLUTION: The composite powder comprises laminar substrate powder and, sticking in a protruding form on a surface of the substrate powder, barium sulfate particles. The cosmetic contains the composite powder. The method for producing the composite powder is provided. <P>COPYRIGHT: (C)2004,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a composite powder, a cosmetic composition containing the composite powder, and a method for producing the composite powder, and more particularly to correction of skin irregularities, color defects and improvement of natural finish.

[0002]

2. Description of the Related Art Conventionally, as a method for correcting physical irregularities on the skin such as pores and fine lines on the bare skin, the blurring effect of diffuse reflection of spherical powder has been used. Especially recently, in order to obtain such effects, talc, mica, alumina,
A composite powder in which minute spherical resin powder is uniformly compounded on the surface of flaky powder such as barium sulfate, or a titanium oxide layer and a silica layer are provided on the surface of spherical silica particles to increase the refractive index of light. Composite powders with improved diffusivity and enhanced blurring effect are also being developed.

On the other hand, as a method for correcting a color defect such as dullness or stains on the bare skin, freckles, redness, and dark circles around the eyes, a strong concealing property with a refractive index of 2.69 and Titanium oxide pigments that have tinting strength have been used. Also, as a method of correcting such a color defect,
It is also known that correction based on the spectral characteristics of powder is effective. However, with the blurring effect of diffuse reflection of spherical powder, it is possible to correct irregularities on the skin such as pores and fine wrinkles, and although it is somewhat satisfactory from the viewpoint of uniform finish of the makeup skin, there is a problem with the skin's color defects. It does not give sufficient correction.

On the other hand, by using a titanium oxide pigment, it is possible to hide the color defects of the skin and make them invisible, but the texture is matte and has a high refractive index. Due to the strong light-scattering property, the finish of the foundation became pale and never gave a natural finish. In addition, the transparency was not felt, and the impression was different from the actual bare skin. In order to solve this problem, a powder was developed in which titanium oxide was doped with iron oxide and colored yellow-orange to aim at a finish that was naturally adapted to the skin (for example, Patent Document 1).
However, although it contributed to the effect of making the finish look natural, it was not a sufficient solution to the problem.

Furthermore, in order to obtain a finish close to that of actual bare skin, powder development focusing on the structure of skin tissue has been carried out, but there is a limit to imitating complicated skin tissue,
At present, not only a natural finish cannot be obtained, but also because the hiding property is low, it is not possible to completely cover color defects such as dull skin and uneven color, and a sufficient effect cannot be expected.

[0006]

[Patent Document 1] Japanese Patent Laid-Open No. 7-3181

[0007]

It is known that the correction based on the spectral characteristic of powder is the most effective natural correction method for correcting the color defect of the skin. Such correction by titanium is made in makeup cosmetics. However, since mica titanium has a strong surface reflection, it gives a flicker-like appearance to the makeup skin, and irregularities on the skin such as pores and fine wrinkles are also noticeable, making it very difficult to obtain a natural and beautiful finish. The present invention has been made in view of the above-mentioned prior art, and its object is to compound a cosmetic powder containing a composite powder that corrects skin irregularities and color defects to give a natural finish while being incorporated into a cosmetic composition. , And a method for producing a composite powder.

[0008]

Means for Solving the Problems As a result of intensive investigations by the present inventors in view of the above problems, as a result, it was found that a composite powder containing a certain amount of protruding barium sulfate particles adhered to the surface of flaky substrate particles should be blended in a cosmetic composition. Found that the unevenness of the skin is corrected and a natural finish can be obtained.Furthermore, using interferometric mica titanium as the flaky substrate particles, a composite powder with a certain amount of protruding barium sulfate particles attached to its surface was applied. It has been found that, by blending it with a colorant, it is possible to correct unevenness of the skin and color defects of the skin, and to obtain a transparent and natural finish that is close to the optical characteristics of bare skin, and completed the present invention. It was

That is, the composite powder of the present invention is characterized in that it contains flaky substrate powder and barium sulfate particles adhered to the surface of the substrate powder in the form of protrusions. Further, in the powder, the barium sulfate particles are in the form of flakes, and adhere to the surface of the substrate powder with the peripheral edge of the flakes as a contact point, and to adhere to the surface of the substrate powder at an angle. Is preferred. In the powder, it is preferable that the substrate powder develops an interference color. In the above powder, titanium mica is exemplified as the substrate powder that exhibits the interference color.

Further, in the powder, the barium sulfate particles are thin pieces having a substantially rectangular shape, and adhere to the surface of the substrate powder with a peripheral edge portion of the thin pieces as a contact, and form an angle with respect to the surface of the substrate powder. It is preferred that they are attached to have. Further, in the powder, it is preferable that barium sulfate particles having a substantially uniform particle diameter are attached to the surface of the substrate powder so that the particle intervals are substantially uniform. In the powder, it is preferable that the barium sulfate particle attachment rate is 15 to 100 mass% with respect to the substrate. Further, in the above powder, it is preferable that the coverage of barium sulfate particles is 10 to 70% of the surface area of the substrate powder. In addition, the cosmetic of the present invention is characterized by blending the composite powder.

Further, in the method for producing a composite powder of the present invention, seed particles are allowed to coexist in a slurry solution of flaky substrate powder, and a barium ion solution and a sulfate ion solution are added to the solution to react with each other, whereby It is characterized in that barium sulfate is crystal-grown using the particles as nuclei, and the generated barium sulfate particles are attached to the surface of the substrate powder. In addition, in the method for producing powder, it is preferable that the amount of seed particles added is 0.1 to 15% by mass with respect to the substrate powder.
In addition, in the method for producing powder, it is preferable to carry out the reaction in a state where the pH of the slurry solution is always adjusted to 7-9. In the method for producing the powder, one or two water-soluble organic substances are added to the slurry solution.
It is preferable to carry out the reaction in the coexistence of at least one species.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION Preferred embodiments of the present invention will be described below. The powder obtained by the production method of the present invention is a composite powder having a flaky powder as a substrate and a certain amount of protruding barium sulfate particles attached to the surface thereof. When this powder is blended in a cosmetic, the unevenness of the skin is uniformly corrected by the light diffusivity of the barium sulfate particles attached in the form of protrusions on the surface of the flaky powder, and a natural and beautiful finish is obtained.

Further, since barium sulfate particles are attached in the form of protrusions on the surface of the substrate powder, the contact point between the powder and the skin is reduced and the feeling of use is lightened. Since it is plate-shaped, it has an excellent fit and spreads smoothly and evenly on the skin, so that it is also possible to obtain a favorable effect in terms of feeling in use. As the shape of the above-mentioned "protruding" barium sulfate particles, various shapes can be obtained depending on the substrate powder used and the manufacturing conditions.
For example, as shown in FIG. 1, it is obtained as a thin piece, which is attached to the surface of the substrate powder by using the peripheral portion of the thin piece as a contact point and attached so as to form an angle with the surface of the substrate powder. .

Examples of the flaky powder used as the substrate of such composite powder include mica, talc, sericite, kaolin, titanium oxide, silica, alumina, iron oxide, boron nitride, synthetic mica, synthetic talc, and hydroxyapatite. , Barium sulfate, etc. are exemplified, and there is no particular limitation as long as the weight average particle diameter (spherical conversion) is 1 to 150 μm. In addition, the adhesion rate of barium sulfate is 1 with respect to the substrate.
It is preferably 5 to 100% by mass. Further, the coverage of barium sulfate particles is 10 to the surface area of the substrate powder.
It is preferably 70%.

Further, a composite powder obtained by adhering a certain amount of protruding barium sulfate particles on the surface thereof by the method of the present invention using a flaky powder exhibiting an interference color such as mica titanium as a substrate, By blending in cosmetics, especially makeup cosmetics, the unevenness of skin and color defects are made uniform by the spectral characteristics due to the interference color of flaky powder and the light diffusivity of barium sulphate particles adhering to the surface in a protruding shape. Can be corrected to. In addition, since the barium sulfate particles are attached to the protrusions to improve the diffuse reflection characteristics of the powder, the strong surface reflection light peculiar to titanium mica is reduced, and the barium sulfate refractive index (1.64) is Refractive index of (1.5
Since it is relatively close to 6), a transparent and natural and beautiful finish is possible.

That is, the interference light of the layered structure powder that exhibits an interference color such as mica titanium has blue, yellow, green, red, purple, etc., and by selecting a preferable interference color corresponding to the skin, the color tone of the skin can be improved. While compensating for these shortcomings, a natural and beautiful finish is possible without producing the flicker feeling peculiar to titanium mica. For example, dull skin and dark circles around the eyes have a color deficiency in the yellow to red light absorbed by melanin and congestion, so correcting the reflected interference light from red to orange to make the skin healthy. The result is a bright and transparent finish.

In addition, the reddish natural skin lightened by the reflected interference light of green, which is insufficiently absorbed by the hemoglobin pigment in the blood, is added to the reddish skin such as sensitive skin, atopic skin, and acne skin, which has recently increased. It can be corrected to the finish. In addition, in the case of skin with a lot of color unevenness such as spots and freckles, a beautiful makeup skin in which the skin is naturally made uniform can be obtained by correcting the yellow reflected interference light absorbed by the dark melanin pigment. Examples of the flaky powder used as the substrate of the layered structure powder that expresses the interference color include titanium mica, low-order titanium oxide-coated mica, iron oxide-coated mica titanium, and the like.
There is no particular limitation as long as it has a weight average particle diameter (spherical equivalent) of 1 to 150 μm.

The deposition rate of barium sulfate deposited on the surface of the substrate is 15 to 10 with respect to the substrate exhibiting interference color.
It is preferably 0% by mass. If the deposition rate of barium sulfate is 15% by mass or less, the surface reflection of the flaky substrate powder cannot be suppressed, and flicker characteristics are observed, which is not preferable. On the other hand, when the adhesion rate exceeds 100% by mass, the powder becomes rough and the feeling of use becomes extremely poor, and the interference color of the flaky powder is excessively concealed to correct the color of the makeup skin. The cosmetic effect will be extremely deteriorated. The adhesion rate of barium sulfate is more preferably 4
It is 0 to 70 mass%.

The coverage of barium sulfate attached to the surface of the substrate is preferably 10 to 70% of the surface area of the substrate powder. If the coverage of barium sulfate exceeds 70%, the interference color of the flaky powder may be excessively hidden and the color correction of makeup skin may be hindered, which is not preferable. If the coverage is less than 10%, the coated particles may be too small to exhibit the diffusion property, and the surface reflection of the flaky substrate powder may not be suppressed, resulting in flicker characteristics. .

FIG. 1 is an SEM photograph of the surface of the composite powder obtained by the manufacturing method of the present invention using titanium mica as the substrate.
Shown in. As described above, the surface structure is a structure in which barium sulfate particles, which are thin flakes having a substantially square shape, are attached to the surface of the substrate powder with the peripheral portion as a contact point, and are attached so as to have an angle with respect to the surface of the substrate powder. That is, the particles adhere to the surface of the substrate powder so that the particle intervals are substantially uniform. Such an attachment structure was peculiar to the case where titanium mica was used as the substrate.

The production method of the present invention is characterized in that seed particles are used in the production of the powder in order to obtain a flaky powder to which projection-like particles are adhered. That is, for example, by allowing fine particles such as metal oxides to coexist as seed particles during the reaction by mixing the barium ion solution and the sulfate ion solution,
This serves as a nucleus for crystal growth of barium sulfate, and a structure in which particles formed by crystal growth of barium sulfate from seed particles adhere to the substrate powder is obtained. Hereinafter, a method for producing the composite powder according to the present invention will be described.

The barium compound used as the raw material of the composite powder is not particularly limited as long as it produces barium ions in a solvent such as water or alcohol. Examples of such barium compound include barium hydroxide, barium chloride, barium sulfide, barium nitrate, and barium acetate. Of these, barium chloride and barium hydroxide are preferable because they are easy to treat by-products. The sulfuric acid compound used as the raw material of the composite powder is not particularly limited as long as it produces a sulfate ion in a solvent such as water or alcohol.

Such sulfuric acid compounds include sulfuric acid, sodium sulfate, sodium hydrogensulfate, ammonium sulfate,
Examples include potassium sulfate and lithium sulfate. Of these, sulfuric acid, sodium sulfate and ammonium sulfate are particularly preferable. When reacting the barium compound and the sulfuric acid compound, a barium ion solution and a sulfuric acid ion solution prepared by dissolving the barium compound and the sulfuric acid compound in water or alcohol, respectively, are prepared in advance. When the barium ion concentration and the sulfate ion concentration during the reaction are dilute, the feel of use of the barium sulfate produced becomes better.

The concentrations of the barium ion solution and the sulfate ion solution are both usually 0.01 mmol / L to 1 mol / L.
Is prepared. Preferably, 1 mmol / L-100 m
The range is mol / L. When the concentration is lower than this range, the efficiency is low as an industrial manufacturing method. On the other hand, if the concentration is higher than this range, the degree of supersaturation is large and the number of nuclei is increased, and a large number of fine particles are generated, resulting in aggregation and the like, which makes it difficult to use for cosmetics.

If the barium ion solution and the sulfate ion solution are mixed with time during the reaction, the reaction will proceed in the reaction solution at a concentration lower than that during preparation. From the viewpoint of crystal growth of barium sulfate particles, it is preferable to carry out the reaction in a state where the pH of the reaction solution is always adjusted to 7-9. Particles of titanium oxide, zinc oxide, alumina, aluminum hydroxide, silica, iron oxide and the like can be used as the seed particles that are allowed to coexist during the reaction. The particle diameter of these particles is 0.02 μm to 2 μm, preferably 0.1 μm to 0.5 μm, and these fine particles serve as nuclei for crystal growth of barium sulfate, and can promote adhesion of barium sulfate to the surface of the substrate powder.

The seed particles are contained in an amount of 0.1 to 0.1 with respect to the substrate powder.
It is added in the range of 15% by mass. If it is less than 0.1% by mass, it may be difficult to control the particle size and adhesion structure of the barium sulfate particles to be produced, and the expected diffuse reflection characteristics may not be obtained. On the other hand, if it exceeds 15% by mass, the crystal growth points become too large, and the morphology control tends to be difficult, and furthermore, the interference color of the flaky powder is concealed excessively, which hinders the color correction of makeup skin. It is not preferable because it may cause The added amount of the seed particles is more preferably 1 to 10 mass% with respect to the substrate powder.

Metal ions can be added for the purpose of controlling the crystal growth of particles. By controlling crystal growth of particles, optical diffuse reflection is enhanced,
Alternatively, an angle-dependent change in glossiness can be imparted. In addition, when metal ions are added when titanium mica is used as a substrate, it is possible to grow crystals in a shape other than the above-mentioned substantially square flaky shape.

Examples of the metal ion include lithium ion, sodium ion, potassium ion, magnesium ion, calcium ion, zinc ion and aluminum ion. These are used alone or in combination of two or more. Each metal ion is provided as an aqueous solution or alcohol solution of a salt compound containing the corresponding metal.

The metal ions are added in the range of 0.01 to 10 equivalents with respect to barium ions. 0.01
When the amount is less than the equivalent, it becomes difficult to control the crystal growth of barium sulfate particles. On the other hand, if it exceeds 10 equivalents, the generated barium sulfate will agglomerate and cannot be evenly adhered to the substrate, resulting in an agglomerated state and a reduced feeling of use.

Examples of the metal salt for giving a metal ion include lithium salts such as lithium hydroxide, lithium chloride, lithium nitrate, lithium carbonate and lithium acetate; sodium hydroxide, sodium chloride, sodium nitrate, sodium carbonate and sodium acetate. Sodium salts such as; potassium salts such as potassium hydroxide, potassium chloride, potassium nitrate, potassium carbonate, potassium acetate; magnesium salts such as magnesium hydroxide, magnesium chloride, magnesium nitrate, magnesium carbonate, magnesium acetate; calcium hydroxide, calcium chloride , Calcium salts such as calcium nitrate, calcium carbonate, calcium acetate; zinc salts such as zinc hydroxide, zinc chloride, zinc nitrate, zinc carbonate, zinc acetate; aluminum hydroxide, aluminum chloride, aluminum nitrate, aluminum carbonate Beam, aluminum salts such as aluminum acetate is used.

In addition to these metal ions, it is also preferable to allow one or more water-soluble organic substances to coexist in the reaction solution for the purpose of controlling the crystal growth of the particles. Examples of such water-soluble organic substances include lower alcohols having 1 to 4 carbon atoms such as methanol, ethanol, n-propyl alcohol, and isopropyl alcohol, polyethylene glycols having a molecular weight of 400 to 20,000,
Examples thereof include polyacrylamides such as poly-N, N-diethylacrylamide and poly-N-isopropylacrylamide.

The barium ion solution and the sulfate ion solution prepared as described above are added to a seed particle and a slurry dispersion of a substrate powder containing metal ions and acids added as necessary, and reacted. The solution after completion of the reaction is filtered, washed with water, pulverized and the like to obtain the composite powder of the present invention.

Typical embodiments of the manufacturing method of the present invention are shown below. <Embodiment 1> To a slurry dispersion of titanium mica, a solution in which alumina fine particles used as seed particles are ultrasonically dispersed is added and mixed by stirring, and then the barium ion solution and the sulfate ion solution prepared as described above are simultaneously prepared. Added. At this time, the molar ratio of sulfate ion to barium ion is 1 /
It should be in the range of 2 to 2/1. The reaction temperature is preferably 0 to 90 ° C., more preferably 10 to 6
The temperature is 0 ° C, more preferably 20 to 40 ° C. Further, during the reaction, it is preferable to carry out the reaction in a state where the pH of the slurry dispersion liquid is constantly adjusted to be in the range of 7 to 9.

<Embodiment 2> A solution in which silica fine particles used as seed particles are ultrasonically dispersed is added to a slurry dispersion of titanium mica, and the mixture is stirred and mixed, and then a metal salt compound solution containing a specific metal ion is added. To do. The barium ion solution and the sulfate ion solution prepared as described above are simultaneously added to the adjusted slurry solution. At this time, the molar ratio of the sulfate ion to the barium ion is set in the range of 1/2 to 2/1. The reaction temperature is preferably 0 to 90 ° C, more preferably 10 to 60 ° C, and further preferably 20 to 40 ° C. Further, during the reaction, it is preferable to carry out the reaction in a state where the pH of the slurry dispersion liquid is constantly adjusted to be in the range of 7 to 9.

When the composite powder of the present invention is blended with cosmetics, the type of the blended cosmetics is not particularly limited, but from the viewpoint of optical properties, it can be particularly preferably used for makeup cosmetics. In addition, the blending amount is also not particularly limited, for example, by adding it to a skin care cosmetic such as an emulsion, an effect of uniformly showing unevenness of the skin is seen, and a large amount is added as an extender pigment to a makeup cosmetic such as a powder foundation. By doing so, the unevenness correction effect on the skin can be remarkably seen.

However, when a pigment having an interference color such as mica titanium is used as the substrate, dullness, stains, freckles,
In order to have the effect of correcting skin color defects such as redness and dark circles around the eyes, it is preferable to add 1% by mass or more to the cosmetic. Further, if it is blended in an amount of 15% by mass or more, there is an effect that whiteness is excessively emphasized, the finish becomes powdery, and interference light is excessively emphasized, resulting in an unnatural finish. Further, in consideration of the above-mentioned optical color correction and new texture, 3% by mass or more is more preferable because a makeup effect can be imparted.

Further, with respect to the composite powder of the present invention, to the extent that the effect thereof is not impaired, a treating agent used for ordinary cosmetic pigments, such as silicone, metal soap, lecithin,
It is also possible to use those surface-treated with amino acids, collagen, fluorine compounds and the like. As other powder components in the cosmetic of the present invention, titanium oxide, zinc oxide, red iron oxide, yellow iron oxide, black iron oxide, ultramarine blue, cerium oxide, talc, mica, sericite, kaolin, bentonite, clay, silicic acid, Anhydrous silicic acid, magnesium silicate, zinc stearate, fluorinated phlogopite, synthetic talc, barium sulfate, magnesium sulfate, calcium sulfate, boron nitride, bismuth oxychloride, alumina, zirconium oxide, magnesium oxide, chromium oxide, calamine, Inorganic powder such as magnesium carbonate and composites thereof; silicone powder,
One or more organic powders such as silicone elastic powders, polyurethane powders, cellulose powders, nylon powders, PMMA powders, starches, polyethylene powders and composites thereof can be blended as required.

In the cosmetic of the present invention, oily ingredients such as liquid paraffin, squalane, ester oil, diglyceride, triglyceride, perfluoropolyether, vaseline, lanolin, ceresin, carnauba wax, solid paraffin, fatty acid, polyhydric alcohol are used. , Silicone resin, fluororesin, acrylic resin, vinylpyrrolidone and the like may be added alone or in combination of two or more as required. The cosmetics of the present invention include dyes, pH adjusters, moisturizers, thickeners, surfactants, dispersants, stabilizers, colorants,
Preservatives, antioxidants, ultraviolet absorbers, fragrances and the like can be appropriately added within the range where the object of the present invention is achieved.

The cosmetic of the present invention is manufactured by a conventional method,
Examples of the dosage form include emulsion foundation, powder foundation, oil foundation, eye shadow, cheek color, body powder, perfume powder, baby powder, face powder, emulsion, beauty lotion, lotion, beauty cream, sunscreen lotion and the like. .

[0040]

The present invention will be described in more detail with reference to the following examples. The present invention is not limited to this, and the blending amount of each component in the examples of the cosmetics is represented by mass% with respect to the total amount of the cosmetics.

The composite powder of the present invention was produced under various conditions.
(Examples 1 to 16).Example 1 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Weigh 0 g, add 400 ml of deionized water and stir to mix
did. Separately, the particle size used as seed particles is about 0.5 μm
4 g of alumina particles (8% by mass relative to titanium mica)
After ultrasonically dispersing and adjusting in 100 ml of aqueous solution,
Mica titanium was added to the slurry dispersion. Mica titanium
After adjusting the liquid temperature of the slurry dispersion liquid to 60 ° C., 640 mmo
1 / L-barium chloride aqueous solution 150 ml and 640 mmo
150 ml of 1 / L-sodium sulfate aqueous solution was added separately
did. White barium sulfate is formed and deposited at the same time as the dropping
Then, the reaction was performed for 2 hours.

The reaction solution was cooled to room temperature, and the obtained solid product was allowed to settle, filtered and washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain a red interference white powder of Example 1. An SEM photograph of the powder surface is shown in Fig. 1 (the same figure B is an enlarged image of the same figure A). The barium sulfate deposition rate of the obtained powder was 45% by mass with respect to the titanium mica on the substrate.

[0043]Examples 2-4 In a 1000 ml round bottom separable flask, place the substrate
Interfering Mica Titanium 5 with a particle size of about 12 μm
0 g (Example 2: yellow interference system, Example 3: green interference system,
(Example 4: blue interference system), ion-exchanged water 400 m
1 was added and mixed with stirring. Separately used as seed particles
Alumina particles with a particle size of about 0.5 μm (for titanium mica
1 to 12% by mass) in 100 ml of an aqueous solution.
After adjusting the dispersion, add it to the mica titanium slurry dispersion.
Added The temperature of the mica titanium slurry dispersion is set to 60 ° C.
After that, 640 mmol / L-barium chloride aqueous solution 15
0 ml and 640 mmol / L-sodium sulfate aqueous solution
150 ml was added separately. White sulfuric acid at the same time as dropping
Barium was produced and precipitated, and the reaction was performed for 2 hours.

The reaction solution was cooled to room temperature to precipitate the obtained solid product, which was filtered and washed with water to remove salts.
It was dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain various interference white powders of Examples 2 to 4 (Example 2: yellow interference system, Example 3: green interference system, Example 4: blue interference system).
Got Further, the barium sulfate deposition rate of the obtained powder is
It was 45 mass% with respect to the mica titanium of the substrate.

[0045]Examples 5-7 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Weigh 0 g, add 400 ml of deionized water and stir to mix
did. Separately, the particle size used as seed particles is about 0.5 μm
Alumina particles (1 to 12 mass% with respect to mica titanium)
Was ultrasonically dispersed in 100 ml of an aqueous solution and adjusted.
The mica titanium was added to the slurry dispersion. Mica titanium
After adjusting the liquid temperature of the slurry dispersion liquid of
15% by mass of titanium on the substrate mica titanium
Example 5), 30 mass% (Example 6), 100 mass% (implementation)
Example 7) 150 barium chloride aqueous solution of each concentration so that
ml and 150 ml of sodium sulfate aqueous solution are prepared separately
Was added. White barium sulphate is produced and precipitated simultaneously with dropping
It was taken out and reacted for 2 hours.

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered and washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain red interference white powders of Examples 5 to 7. SEM photographs (Examples 5 and 7) of the powder surface are shown in FIGS.

[0047]Examples 8-10 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Weigh 0 g, add 400 ml of deionized water and stir to mix
did. Separately, the particle size used as seed particles is about 0.5 μm
Alumina particles (1 to 12 mass% with respect to mica titanium)
Was ultrasonically dispersed in 100 ml of an aqueous solution and adjusted.
The mica titanium was added to the slurry dispersion. More metal
964 mmol / L-various salts for coexisting ions
100 ml of metal fluoride aqueous solution (Example 8: magnesium, fruit)
Example 9: Calcium, Example 10: Sodium) added
did. The temperature of the mica titanium slurry dispersion was set to 60 ° C.
After that, 640 mmol / L-barium chloride aqueous solution 150
ml and 640 mmol / L-sodium sulfate aqueous solution 15
0 ml was added separately. White sulfuric acid burr at the same time as dropping
Um was generated / precipitated and reacted for 2 hours.

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered, washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization processing was performed to obtain red interference white powders of Examples 8 to 10. SEM photographs (Examples 8 to 10) of the powder surface are shown in FIGS. The barium sulfate deposition rate of the obtained powder was 45% by mass with respect to the titanium mica on the substrate.

[0049]Examples 11-13 In a 1000 ml round bottom separable flask, place the substrate
Talc having a particle diameter of about 12 μm (Example 11)
50g of mica (Examples 12 and 13) was measured, and ion exchange was performed.
400 ml of exchanged water was added and mixed with stirring. Separately, with seed particles
Alumina particles with a particle size of about 0.5 μm (tal
(1 mass% with respect to mica or mica) in 100 ml of aqueous solution
After ultrasonic dispersion and adjustment with, the mica titanium slurry
Added to the dispersion. Liquid temperature of titanium mica titanium slurry dispersion
To 60 ° C., and then 640 mmol / L-barium chloride
Aqueous solution 150 ml and 640 mmol / L-Natrium sulfate
150 ml aqueous solution of water was added separately. White at the same time as dripping
Colored barium sulphate is formed and deposited, and reacted for 3 hours
It was

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered, washed with water to remove salts, and then dried at 150 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain white powders of Examples 11-13. SEM photographs (Examples 11 to 13) of the powder surface are shown in FIGS.

[0051]Example 14 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Weigh 0 g and add 400 g of 10 mass% ethanol solution
And mixed with stirring. Separately, about the particle size used as seed particles
0.5 μm alumina particles (1 to 1 for mica titanium)
2 mass%) is ultrasonically dispersed in 100 ml of aqueous solution for adjustment.
After that, the mica titanium was added to the slurry dispersion.
After setting the temperature of the mica titanium slurry dispersion to 60 ° C.,
640 mmol / L-150 ml of barium chloride aqueous solution
640 mmol / L-sodium sulfate aqueous solution 150 ml
Was added at the same time. At the same time as dropping, white barium sulfate
After formation / precipitation, reaction was carried out for 2 hours.

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered, washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain a red interference white powder of Example 14. The barium sulfate deposition rate of the obtained powder was 45% by mass with respect to the titanium mica on the substrate.

[0053]Example 15 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Measure 0 g, 400 ml of deionized water, and polyethylene
Water in which 0.5 g of glycol (molecular weight about 400) is dissolved
100 ml of the solution was added and mixed with stirring. Separately, with seed particles
Alumina particles with a particle diameter of about 0.5 μm (mica
1 to 12% by mass of titanium) in 100 ml of aqueous solution
After ultrasonic dispersion in the slurry, the mica titanium slurry was adjusted.
-Added to dispersion. Liquid of mica titanium slurry dispersion
After adjusting the temperature to 60 ° C., 640 mmol / L-barium chloride
150ml aqueous solution and 640mmol / L-Natri sulfate
150 ml of an aqueous solution of um was added at the same time. At the same time as dripping
White barium sulphate was formed and deposited, and reacted for 2 hours.
It was

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered, washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain a red interference white powder of Example 15. The barium sulfate deposition rate of the obtained powder was 45% by mass with respect to the titanium mica on the substrate.

[0055]Example 16 In a 1000 ml round bottom separable flask, place the substrate
Red interferometric mica titanium 5 with a particle size of about 12 μm
Weigh 0 g, add 400 ml of deionized water and stir to mix
did. Separately, the particle size used as seed particles is about 0.5 μm
Alumina particles (1 to 12 mass% with respect to mica titanium)
Was ultrasonically dispersed in 100 ml of an aqueous solution and adjusted.
After adding to the titanium mica titanium slurry dispersion, dilute hydrochloric acid and
And / or dilute sodium hydroxide solution to adjust the pH to 8-9.
Adjusted to. Adjust the temperature of the mica titanium slurry dispersion to 60
After reaching ℃, dilute hydrochloric acid and / or dilute sodium hydroxide solution
640 mmol while adjusting the pH to 8-9 by adding
/ L-barium chloride aqueous solution 150 ml and 640 mmol
/ L-sodium sulfate aqueous solution 150 ml was added at the same time.
It was White barium sulphate is generated and deposited at the same time as the dropping,
The reaction was carried out for 2 hours.

The reaction solution was cooled to room temperature, the obtained solid product was allowed to settle, filtered, washed with water to remove salts, and then dried at 120 ° C. for 12 hours. After drying, pulverization treatment was performed to obtain a red interference white powder of Example 16. The barium sulfate deposition rate of the obtained powder was 45% by mass with respect to the titanium mica on the substrate.

[0057]Comparative Example 1 As a comparative example, ion-exchange without adding any coexisting seed particles
White powder was produced in the same manner as in Example 1, except that an appropriate amount of water was adjusted.
I got the end. Various cosmetics containing the composite powder of the above examples
Was applied to 20 female panelists,
Pore, fine wrinkles, etc. and color defects (dullness, stains, blemishes, etc.)
Effect of correcting blur, redness, dark circles around the eyes, etc.
Brightness, natural finish, and feel during application (smoothness)
Practical characteristic evaluation based on the following criteria
It was

[0058]Practical characteristic evaluation criteria ◎ Answer of 17 or more is good ○ Answered that 12 to 16 people are good △ Answer that 9 to 11 people are good × Answered by 5 to 8 people ×× 4 people or less answered The cosmetic prescription and evaluation results are shown below.

[0059]

[Table 1]Powder foundation Example 17 Comparative Example 2 Comparative Example 3 Sericite 17 17 17 Synthetic Mica 10 10 10 Talc residual residual residual Red interference system composite powder (Example 1) 8 − − Composite powder (Comparative example 1) -8- Red Interference Mica Titanium-8 Titanium oxide 10 10 10 Red iron oxide 0.8 0.8 0.8 Yellow iron oxide 2 2 2 Black iron oxide 0.1 0.1 0.1 Zinc flower 2 2 2 Silicone elastic powder 2 2 2 Dimethyl polysiloxane 3 3 3 Liquid paraffin 5 5 5 Vaseline 5 5 5 Sorbitan sesquiisostearate 1 1 1 Paraben Suitable amount Suitable amount Suitable amount Antioxidant Proper amount Proper amount Proper amountPerfume Suitable amount Suitable amount Suitable amount Skin unevenness correction effect ○ × × × Skin dullness correction effect ◎ △ ○ Finished transparency ◎ △ △ Natural finish ○ △ ×Feel of use (smoothness) ◎ ○ △

As is clear from Table 1, the foundation of Example 17 containing the composite powder of Example 1 is capable of correcting unevenness of the skin and color defects and imparting a transparent and natural finish. there were. Further, it had a smooth and light feeling in use. On the other hand, with the foundation of Comparative Example 2 in which the composite powder of Comparative Example 1 was blended, unevenness of the skin and color defects were not corrected, and a transparent and natural finish could not be obtained. In addition, in the foundation of Comparative Example 3 in which the interferometric mica titanium was mixed, although the color defect was corrected, the unevenness of the skin was conspicuous, the skin was tingling, and the transparent and natural finish could not be obtained.

[0061]

[Table 2]Powder foundation (summer powder solid foundation that can be used with water) Example 18 Comparative Example 4 Comparative Example 5 Siliconized sericite 18 18 18 Silicone treated mica Residual Residual Residual Silicone treated talc 15 15 15 Silicone treatment 8 --- Yellow interference system composite powder (Example 2) Silicone-treated composite powder-8- (Comparative Example 1) Silicone treatment--8 Yellow interference system mica titanium Silicone treated titanium oxide 8 8 8 Aluminum stearate treatment 6 6 6 Fine particle titanium oxide Silicone-treated red iron oxide 1.2 1.2 1.2 Silicone treated yellow iron oxide 2.5 2.5 2.5 2.5 Silicone treated black iron oxide 0.9 0.9 0.9 Polyurethane powder 2 2 2 Paraben Suitable amount Suitable amount Suitable amount Dimethyl polysiloxane 4 4 4 Methylphenyl polysiloxane 3 3 3 Octyl methoxycinnamate 3 3 3 Polyether modified silicone 2 2 2 Antioxidant Proper amount Proper amount Proper amountPerfume Suitable amount Suitable amount Suitable amount Skin unevenness correction effect ○ × × × Correction effect for skin stains and freckles ◎ △ △ Transparent finish ◎ △ × Natural finish ○ △ ×Feel of use (smoothness) ◎ ○ △

As is clear from Table 2, the foundation of Example 18 containing the composite powder of Example 2 corrects the unevenness of the skin and color defects and gives a transparent and natural finish. there were. Further, it had a smooth and light feeling in use. In contrast,
In the foundation of Comparative Example 4 in which the powder of Comparative Example 1 was blended, the unevenness of the skin was not corrected, and further, the transparency and the natural finish were not sufficient. Also,
In the foundation of Comparative Example 5 in which the interference type mica titanium was blended, the unevenness of the skin was conspicuous and there was a flicker feeling, and a transparent and natural finish could not be obtained.

[0063]

[Table 3]Powder foundation (summer powder solid foundation that can be used with water) Example 19 Comparative Example 6 Comparative Example 7 Silicone treated mica 25 25 25 Siliconized Sericite 17 17 17 Silicone treated talc Residual Residual Residual Silicone treatment 8 --- Blue interference system composite powder (Example 4) Silicone-treated composite powder-8- (Comparative Example 1) Silicone treatment--8 Blue interference mica titanium Silicone treated titanium oxide 10 10 10 Spherical PMMA powder 4 4 4 Paraben Suitable amount Suitable amount Suitable amount Dimethyl polysiloxane 4 4 4 Methylphenyl polysiloxane 1 1 1 Vaseline 3 3 3 Octyl methoxycinnamate 3 3 3 Sorbitan diisostearate 1 1 1 Antioxidant Proper amount Proper amount Proper amountPerfume Suitable amount Suitable amount Suitable amount Effect of correcting unevenness of skin ○ × × Correction effect of skin color ○ △ △ Transparent finish ◎ △ × Natural finish ◎ △ ×Feel of use (smoothness) ○ ○ △

As is clear from Table 3, the foundation of Example 19 in which the composite powder of Example 4 is blended corrects the unevenness of the skin and the color defect and gives a transparent and natural finish. there were. Further, it had a smooth and light feeling in use. In contrast,
The foundation of Comparative Example 6 containing the powder of Comparative Example 1 did not correct the unevenness of the skin, and could not obtain sufficient results in terms of transparency and natural finish. Also,
In the foundation of Comparative Example 7 containing the interference type mica titanium, the unevenness of the skin was conspicuous and there was a flicker feeling, and a transparent and natural finish could not be obtained.

[0065]

[Table 4]Face powder (white powder) Example 20 Example 21 Example 22 Talc residual residual residual Mica 20 20 20 Plate-shaped barium sulfate 5 5 5 Red interference system composite powder (Example 1) 10 − − Red interference system composite powder (Example 5) -10- Red interference system composite powder (Example 7) -10 Fine particle titanium oxide 3 3 3 Spherical silicone powder 3 3 3 Vaseline 1 1 1 Squalane 3 3 3 Ester oil 1 1 1 Paraben Suitable amount Suitable amount Suitable amount Antioxidant Proper amount Proper amount Proper amountPerfume Suitable amount Suitable amount Suitable amount Effect of correcting unevenness of skin ○ △ ◎ Skin dullness correction effect ◎ ◎ △ Finished transparency ◎ ○ △ Natural finish ○ △ ○Feel of use (smoothness) ○ △ ◎

As is clear from Table 4, Examples 1, 5,
The face powders of Examples 20, 21 and 22 in which the composite powder of Example 7 was mixed corrected the irregularities of the skin and the color defects and gave a transparent and natural finish.
Further, it had a smooth and light feeling in use.

[0067]

[Table 5]W / O type emulsion cream foundation Example 23 Comparative Example 8 Comparative Example 9 Ion-exchanged water 43 43 43 Chondroitin sodium sulfate 1 1 1 1,3-butylene glycol 3 3 3 Methylparaben Suitable amount Suitable amount Suitable amount Dimethyl polysiloxane 16 16 16 (20cs) Decamethylcyclopentasiloxane 5 5 5 Silicone resin 1 1 1 Cetyl isooctanoate 1 1 1 Polyoxyalkylene modified 4 4 4 Organopolysiloxane (modification rate 20%) Antioxidant Proper amount Proper amount Proper amount Perfume Suitable amount Suitable amount Suitable amount Spherical silica 5 5 5 Silicone treated titanium oxide 10 10 10 Silicone-treated red interference compound powder 6 --- (Example 15) Silicone treated composite powder-6- (Comparative Example 1) Silicone-treated Red Interference Mica Titanium--6 Silicone-treated red iron oxide 1.4 1.4 1.4 Silicone treated yellow iron oxide 3 3 3Silicone treated black iron oxide 0.1 0.1 0.1 Skin unevenness correction effect ◎ △ △ Skin dullness correction effect ○ △ △ Transparent finish ○ ○ ○ Natural finish ○ ○ △Feel of use (smoothness) ◎ △ ◎

As is apparent from Table 5, the foundation of Example 23 containing the composite powder of Example 15 corrects skin irregularities and color defects and gives a transparent and natural finish. there were. Further, it had a smooth and light feeling in use. On the other hand, in the foundation of Comparative Example 8 in which the composite powder of Comparative Example 1 was blended, the unevenness of the skin and the color defect were not corrected, and the transparent natural finish could not be obtained. Also,
In the foundation of Comparative Example 9 in which the interference-based mica titanium was mixed, the unevenness of the skin was conspicuous, the skin was tingling, and the transparent and natural finish could not be obtained.

[0069]

[Table 6]W / O type emulsion cream foundation (solid type) Example 24 Comparative example 10 Comparative example 11 Ion-exchanged water 40.5 40.5 40.5 Sodium glutamate 1 1 1 1,3-butylene glycol 5 5 5 Methylparaben Suitable amount Suitable amount Suitable amount Dimethyl polysiloxane 4 4 4 (20cs) Decamethylcyclopentasiloxane 16 16 16 Silicone resin 1 1 1 Cetyl isooctanoate 1 1 1 Polyoxyalkylene modified 4 4 4 Organopolysiloxane (modification rate 20%) Antioxidant Proper amount Proper amount Proper amount Perfume Suitable amount Suitable amount Suitable amount Waxes 5 5 5 Silicone treated titanium oxide 8 8 8 Silicone-treated red iron oxide 0.5 0.5 0.5 Silicone treated fine particles titanium oxide 6 6 6 Silicone-treated red interference compound powder 6 --- (Example 16) Silicone-treated composite powder (Comparative Example 1) -6- Silicone-treated Red Interference Mica Titanium--6 Silicone treated black iron oxide 0.1 0.1 0.1Silicone treated yellow iron oxide 1.4 1.4 1.4 1.4 Skin unevenness correction effect ◎ △ △ Skin dullness correction effect ◎ △ ○ Transparent finish ○ ○ △ Natural finish ○ ○ △Feel of use (smoothness) ◎ △ ◎

As is clear from Table 6, the foundation of Example 24 containing the composite powder of Example 16 is intended to correct irregularities on the skin and color defects and to give a transparent and natural finish. there were. Further, it had a smooth and light feeling in use. On the other hand, in the foundation of Comparative Example 10 in which the composite powder of Comparative Example 1 was blended, unevenness of the skin and color defects were not corrected, and a transparent natural finish could not be obtained. In addition, in the foundation of Comparative Example 11 in which the interferometric mica titanium was mixed, although the color defect was corrected,
The unevenness of the skin was conspicuous, there was a tingling sensation, and a transparent and natural finish could not be obtained.

The other prescriptions carried out are shown below.

[Table 7]

[0072]

[Table 8]

[0073]

[Table 9]

[0074]

[Table 10]

[0075]

[Table 11]

Each of the cosmetics shown in Tables 5 to 9 was capable of correcting irregularities on the skin and color defects and imparting a transparent and natural finish. Further, it had a smooth and light feeling in use.

[0077]

As described above, according to the present invention, a composite powder in which projecting barium sulfate particles are adhered to the surface of a flaky substrate powder is obtained. The unevenness is uniformly corrected and a natural and beautiful finish is obtained. Furthermore, in the case of a composite powder obtained by using a flaky powder that expresses an interference color such as titanium mica as the flaky substrate powder, the use of a cosmetic mixture containing the flaky powder uniformly causes unevenness of the skin and color defects. It is corrected to give a transparent and natural and beautiful finish.

[Brief description of drawings]

1 is an SEM photograph of the surface of the composite powder of Example 1. FIG.

2 is an SEM photograph of the surface of the composite powder of Example 5. FIG.

3 is a SEM photograph of the surface of the composite powder of Example 7. FIG.

4 is a SEM photograph of the surface of the composite powder of Example 8. FIG.

5 is an SEM photograph of the surface of the composite powder of Example 9. FIG.

6 is a SEM photograph of the surface of the composite powder of Example 10. FIG.

7 is an SEM photograph of the surface of the composite powder of Example 11. FIG.

8 is a SEM photograph of the surface of the composite powder of Example 12. FIG.

9 is an SEM photograph of the surface of the composite powder of Example 13. FIG.

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁷ Identification code FI theme code (reference) // C01B 33/42 C01B 33/42 (72) Inventor Kyoko Castle City 2-2 Hayabuchi, Tsuzuki Ward, Yokohama City, Kanagawa Prefecture No. 1 Shiseido Research Center (Shin-Yokohama) (72) Inventor Go Miyamoto 2-2-1 Hayabuchi, Tsuzuki-ku, Yokohama, Kanagawa Shiseido Research Center (Shin-Yokohama) (72) Inventor Tetsuya Kanamaru 2-2-1, Hayabuchi, Tsuzuki-ku, Yokohama-shi, Kanagawa Shiseido Research Center (Shin-Yokohama) (72) Inventor Katsuhiko Yagi 2-2-1, Hayabuchi, Tsuzuki-ku, Yokohama-shi, Kanagawa Shiseido Research Co., Ltd. F term in the center (Shin Yokohama) (reference) 4C083 AA112 AA122 AB172 AB212 AB222 AB232 AB242 AB351 AB362 AB431 AB432 AC012 AC022 AC112 AC122 AC242 AC342 AC352 AC372 AC422 AC442 AC482 AC542 AC582 AC852 AD022 AD042 AD072 AD092 AD152 AD162 AD172 AD342 AD392 AD622 AD642 AD662 CC01 CC04 CC12 DD17 DD21 DD32 DD33 EE07 EE12 FF01 FF04 4G073 BA13 BA20 BA75 BA76 BD19 CM31 CN31 CN26 CN31 CN31 CN26 CB4

Claims (13)

[Claims] 1. A composite powder comprising a flaky substrate powder and barium sulfate particles adhering to the surface of the substrate powder in the form of protrusions. 2. The powder according to claim 1, wherein the barium sulfate particles are flaky and adhere to the surface of the substrate powder by using the peripheral edge of the flakes as a contact point, and A composite powder, characterized in that it adheres so as to have an angle. 3. The powder according to claim 1 or 2, wherein
The composite powder, wherein the substrate powder exhibits an interference color. 4. The composite powder according to claim 3, wherein the substrate powder is mica titanium. 5. The powder according to claim 4, wherein the barium sulfate particles are thin pieces having a substantially square shape, and the peripheral edge portions of the thin pieces are attached to the surface of the substrate powder as contact points, and are adhered to the surface of the substrate powder. A composite powder characterized in that it is attached so as to have an angle to it. 6. The powder according to claim 5, wherein barium sulfate particles having a substantially uniform particle size are formed on the surface of the substrate powder.
A composite powder characterized in that the particles are adhered so that the particle intervals are substantially uniform. 7. The composite powder according to claim 1, wherein the deposition rate of barium sulfate particles is 15 to 100 mass% with respect to the substrate. 8. The composite powder according to claim 1, wherein the coverage of barium sulfate particles is 10 to 70% of the surface area of the substrate powder. 9. A cosmetic comprising the composite powder according to claim 1. 10. Seed particles are allowed to coexist in a slurry solution of flaky substrate powder, and a barium ion solution and a sulfate ion solution are added to the solution to react with each other, whereby barium sulfate is crystal-grown with the seed particles as nuclei. A method for producing a composite powder, wherein the produced barium sulfate particles are attached to the surface of the substrate powder. 11. The method for producing a powder according to claim 10, wherein the amount of seed particles added is 0.1 to 15 relative to the substrate powder.
A method for producing a composite powder, characterized in that the content is% by mass. 12. The method for producing a powder according to claim 10 or 11, wherein the reaction is performed in a state where the pH of the slurry solution is always adjusted to 7-9. Production method. 13. The method for producing a powder according to claim 10, wherein the reaction is performed in the state where one or more water-soluble organic substances coexist in the slurry solution. Method for producing composite powder.