JP2860673B2 - Manufacturing method of pigmented flaky pigment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention is excellent in lightness, chroma, gloss and smoothness, and is also excellent in stability such as water resistance, solvent resistance, weather resistance and safety. And a method for producing a dye-containing flaky pigment.

[Problems to be solved by conventional technology and invention]

Conventionally, as pigments with excellent gloss and smoothness, mica coated with titanium oxide, sericite, talc, kaolinite,
Alternatively, a so-called pearl luster pigment such as barium sulfate has been known. These are flaky inorganic powders whose surfaces are coated with titanium oxide having a high refractive index. Interference colors of red, blue, green, gold and silver can be obtained depending on the thickness of the coating layer. However, unlike the interference color, the appearance color is almost white,
Although the pearl luster is excellent, a clear appearance color cannot be obtained.

Therefore, various appearance colors can be obtained by mixing these pearl luster pigments with general colored inorganic pigments and organic pigments. However, since these pearly luster pigments are flaky and have a particle size considerably larger than those of general pigments, merely mixing them causes some problems as pigments. That is, it is difficult to uniformly mix the particles of the pearl gloss pigment and the general pigment due to differences in the size, specific gravity, shape, and surface properties of the particles.

Therefore, for the purpose of coloring the pearl luster pigment, a composite of a general inorganic pigment and a flaky pearl pigment or a general organic pigment and a flaky pearl pigment has been used. As a method of compounding the inorganic pigment and the flaky pigment, iron oxide, nickel oxide, cobalt oxide, copper oxide,
It was known to coat chromium oxide and navy blue. However, such a method of coating an inorganic pigment has unsolved problems such as a limited hue, lack of sharpness, and a dark color cannot be obtained.

On the other hand, a composite pigment of an organic pigment and a flaky pigment is superior in the color clarity and variety of inorganic pigments as compared with the inorganic pigment, and as already seen in JP-A-51-17910, mica A method in which the surface is coated with aluminum hydroxide by a wet treatment using aluminum chloride or the like, an organic dye is added and colored to obtain a pigment, or as disclosed in JP-A-52-148632, It has been known that a gel solution can be produced by adding mica, further adding an organic dye, and coloring. But like this,
In the method in which the flaky pigment is coated with an organic dye after a simple surface treatment, the coated substance is easily peeled off, and the organic dye has a structure in which the organic dye is exposed on the surface. However, the drawback that stability such as water resistance, solvent resistance, weather resistance and heat resistance is inferior remains.

Accordingly, it is an object of the present invention to provide a pigment having a wide variety of colors, clear colors, and excellent stability.

[Means for solving the problem]

In view of the above situation, the present inventors have conducted intensive studies, and as a result, after adsorbing basic aluminum on the titanium oxide-coated flaky inorganic powder, the present invention was carried out in a vacuum atmosphere or an inert gas atmosphere.
The pigment obtained by baking at 200 to 500 ° C., adsorbing the dye, and further hydrothermally treating the alumina is excellent not only in color clarity but also in stability such as water resistance, solvent resistance, and weather resistance. The present invention was also found to be excellent in safety and to complete the present invention.

That is, after adsorbing basic aluminum to the flaky inorganic powder coated with titanium oxide, the present invention is fired at 200 to 500 ° C. in a vacuum atmosphere or an inert gas atmosphere,
An object of the present invention is to provide a method for producing a dye-containing flaky pigment, which comprises adsorbing an organic dye to the obtained powder and then subjecting the powder to hydrothermal treatment.

In the present invention, the flaky shape means a general flaky shape such as a plate shape, a disk shape, a leaf shape, a ribbon shape and the like, and is not particularly limited to a scale shape. Examples of the flaky inorganic powder include mica, sericite, talc,
Examples include clay minerals such as kaolinite and flakes such as barium sulfate and boron nitride. These particles preferably have a particle size of 0.5 to 50 μm.

The titanium oxide-coated flaky inorganic powder used as a raw material of the dye-containing flaky pigment according to the present invention can be prepared by a known method. For example, the above-mentioned mica, talc, flaky inorganic powder such as sericite is suspended in a strongly acidic solution of titanyl sulfate,
Then, the mixture is rapidly heated to 90 to 100 ° C. and kept for 2 to 3 hours to deposit a titanium oxide-containing layer on the flaky inorganic powder. Next, this is filtered, dried and further kept at 950 ° C. for 1 hour to obtain a titanium oxide-coated flaky inorganic powder having a pearl-like interference color.

In the present invention, the alumina adsorbing the organic dye is
An organic dye is supported on adsorptive alumina. Here, the adsorptive alumina refers to alumina and / or alumina hydrate having a high specific surface area and an active site, having a strong adsorptive power and having hydrothermal reactivity, and includes, for example, amorphous,
水-, ρ-, η-Alumina and hydrothermally reactive alumina having activity such as boehmite. N ₂ is used to measure the specific surface area.
BET adsorption method or its simplified method.

Examples of the organic dye include an acid dye, a natural dye, an oil-soluble dye, a vat dye, and the like. Coloring with any dye is possible, and an acid dye and a natural dye are most preferable. As acid dyes, Red No. 2, Red No. 3, Red No. 102, Red No. 1
04, Red 105, Red 106, Yellow 4, Yellow 5, Green 3, Blue 1, Blue 2, Red 227, Red 230,
Red 231, Red 232, Orange 205, Orange 2
07, Yellow 202, Yellow 203, Green 201, Green 204,
Green No. 205, Red No. 202, Blue No. 205, Brown No. 201, Red 41
0, Red 502, Red 503, Red 504, Red 506,
Orange color 402, yellow 402, yellow 403, yellow 406,
Yellow No. 407, Green No. 402, Purple No. 401, Black No. 401, and the like can be used, if necessary. Natural pigments include raccaic acid, carminic acid,
Quinones such as kermesic acid, alizarin, shikonin, alkanine, echinochrome; β-carotene, β-apo-8
-Carotinal, capsanthin, lycopene, bixin,
Carotenoids such as crocin and canthaxanthin; flavonoids such as shisonin, raphanin, enocyanine, safrole yellow, rutin, quercetin, cocoa pigments; flavins such as riboflavin; porphyrins such as chlorophyll; diketones such as curcumin; Examples include betacyanidin dyes, and if necessary, these can be used in combination. Oil-soluble dyes, for example, red 215, red 218, red 223, orange 201, orange 206, yellow 201, yellow 204
No. 2, Green No. 202, Purple No. 201, Red No. 501, Red No. 505, Orange No. 403, Yellow No. 404, Yellow No. 405, Blue No. 403, etc., and they can be mixed and used as required. These dyes are contained in the pigment in a weight ratio of 0.001 to 1 g / g carrier, particularly 0.01 to 1 g / g carrier.
Preferably, 5 to 0.2 g / g carrier is adsorbed.

In the present invention, since the alumina surface is subjected to the hydrothermal treatment, the organic dye adsorbed on the alumina is prevented from leaking.

The dye-containing flaky pigment according to the present invention is, for example, after adsorbing basic aluminum on a flaky inorganic powder coated with titanium oxide, and then in a vacuum atmosphere or an inert gas atmosphere.
It is manufactured by baking at 200 to 500 ° C., adsorbing an organic dye to the obtained powder, and then performing a hydrothermal treatment.

To adsorb basic aluminum on the titanium oxide-coated flaky inorganic powder, for example, stir the titanium oxide-coated flaky inorganic powder in a basic aluminum aqueous solution, and adsorb a basic aluminum salt on the surface thereof by ionic bonding. .
This makes it possible to form a uniform alumina layer. Uniform formation of the alumina layer is particularly effective for preventing delamination, obtaining chroma and smoothness as a pigment.

Examples of the basic aluminum salt to be used include those represented by the following general formula.

Al _n (OH) _m X _o (X represents Cl, Br, I, n, m, and o represent numbers satisfying 3n = m + o) Such a basic aluminum salt has solubility in water. Good, the pH of the aqueous solution is acidic,
Particularly, Al ₂ (OH) ₅ Cl is preferable.

This basic aluminum is adsorbed on the titanium-coated flaky inorganic powder, filtered, dried, and further subjected to a baking treatment to form an adsorbable alumina coating layer.

For the specific surface area of the flaky carrier obtained by calcining process which allowed to sufficiently adsorb the organic dye is preferably at least 30 m ² / g, in particular, but is preferably 100 m ² / g or more, 300 meters ²
/ g is technically difficult. In addition, the carrier on the flake is indispensable to have a solid acid point, and preferably, the suspension pH is 2.0 to 6.0, particularly 3.0 to 5.0 so that the organic dye is adsorbed later. Preferred above.
Here, the suspension pH as an index indicating the strength of the solid acid point
Is the value obtained by measuring the pH of a 5% by weight aqueous suspension at 25 ° C. If the pH of the suspension is too acidic, its use as a pigment is limited. If the pH is too high, it becomes difficult to retain and adsorb the dye, and it is difficult to maintain desirable vividness.

In order to obtain such a preferable specific surface area and suspension pH, it is necessary to adjust the firing temperature, time and atmosphere. For this reason, the calcination temperature is a temperature that increases the specific surface area and the solid acid point, that is, 200 to 500 ° C, particularly 300 to 500 ° C.
And baking for 10 minutes to 2 hours is preferable.

Further, those fired in the atmosphere form a γ-alumina layer, and cannot be subjected to hydrothermal treatment later. Therefore, 10tor
r. It is necessary to perform firing in the following vacuum atmosphere or in an atmosphere of an inert gas such as N ₂ or Ar. Those fired in this atmosphere can stabilize the dye by the subsequent hydrothermal treatment.

To adsorb the organic dye on the obtained flaky carrier, preferably 0.001 to 10% by weight of the aforementioned dye is added to the flaky carrier.
(Hereinafter simply referred to as%), particularly preferably 0.01 to 3% solution.

As the dye solution, an aqueous solution is preferable for an acid dye or a natural dye, and an organic solvent solution is preferable for an oil-soluble dye. In some cases, a mixed solution of water and a natural solvent is also used. For vat dyes, an aqueous solution of a reductant is used. If necessary, a surfactant, an inorganic salt or the like may be added to the dye solution in order to improve the dyeing property.

The contact and operation of the flaky carrier with the dye solution can be carried out by a method such as dipping, drop mixing, fluidized bed mixing and the like. The contact / action time is preferably 1 to 60 minutes, and the temperature of the dye solution is preferably 80 ° C. or less. By this contact / action operation, a desired amount of the dye can be adsorbed on the carrier.

The flaky carrier to which the dye has been adsorbed can significantly improve the water resistance, solvent resistance and weather resistance of the adsorbed dye by performing a hydrothermal treatment.

The hydrothermal reaction may be treated with hot water at 70 to 180 ° C.
The use of pressurized steam at ~ 180 ° C makes hydrothermal treatment more satisfactory. However, care must be taken because some pigments change color when the temperature exceeds 150 ° C. The time required for the hydrothermal treatment is shorter as the temperature is higher, and 5 hours depending on the temperature.
Minutes to 2 hours are preferred.

The effect of the hydrothermal treatment can be confirmed by observing the surface with a scanning electron microscope (SEM) and measuring the amount of alumina hydrate (pseudo-boehmite) phase produced by flake X-ray diffraction.

After hydrothermal treatment, the powder is finally washed, filtered,
Dry below. If the filtrate is washed with an organic solvent such as acetone or ethanol in order to accelerate drying of the filtrate and prevent secondary aggregation, a powder having good powder properties can be obtained.

The pigment-containing flaky pigment thus obtained has lightness, chroma,
It is excellent in stability such as gloss, water resistance, solvent resistance, weather resistance and the like, and safety, and a cosmetic containing the same has pearl luster in addition to these properties.

The application of the pigment-containing flaky pigment obtained by the production method of the present invention is not particularly limited, and it can be widely used in cosmetics, paints, plastics, inks, paints, daily goods, decorative articles and the like.

As cosmetics, for example, lipstick, eye shadow, blusher,
Nail enamel, eyeliner, eye pencil, mascara and the like can be mentioned. Such cosmetics of the present invention, depending on the type of cosmetic, the composition, the type of pigment, but generally 0.5
Up to 50%, more preferably 1 to 40% of a dye-containing flaky pigment is blended.

Further, a commonly used cosmetic base can be blended with the cosmetic. For example, in addition to the above pigments, extender pigments such as kaolin and nylon powder; titanium oxide;
Inorganic pigments such as zinc white and iron oxide are used. Further, a powder which has been subjected to a known surface hydrophobic treatment such as a silicon treatment, a metal soap treatment, and an N-acylglutamic acid treatment may be used. Examples of the oil include hydrocarbons such as solid or liquid paraffin, solid paraffin, microcrystalline wax, vaseline, ceresin, ozokerite or montan wax; vegetable oils such as olive, ground wax, carnauba wax, lanolin or whale wax or Animal fats and oils;
Further, fatty acids such as stearic acid, palmitic acid, oleic acid, glycerin monostearate, glycerin distearate, glycerin monooleate, isopropyl myristate, isopropyl stearate or butyl stearate and esters thereof; ethyl; Alcohols such as alcohol, isopropyl alcohol, cetyl alcohol, stearyl alcohol, palmityl alcohol and hexyl decyl alcohol are exemplified. Further, polyhydric alcohols having a moisturizing action such as glycol, glycerin or sorbitol can also be used.

[Action]

The adsorptive alumina coating layer of the flaky carrier obtained by the production method of the present invention is porous in view of its enormous specific surface area and BET adsorption curve, and has acidic active sites in the pores. It is considered that the dye is adsorbed.
In addition, this layer easily expands into a hydrated alumina (pseudo-boehmite) by hydrothermal reaction to cause volume expansion. For this reason, it is presumed that when the flaky carrier having the dye adsorbed in the pores is hydrothermally treated, the pores are blocked due to volume expansion, and the elution of the pigment can be prevented.

〔Example〕

Next, the present invention will be described in more detail with reference to examples, but the present invention is not limited thereto.

Example 1 basic aluminum chloride (Hoechst trade name Rokuron -P, composition formula _{Al 2 (OH) 5 Cl ·} 2~3H 2 O) to 140g water 700g
Dissolves in the mica titanium (MERCK
(50 g of Timiron Super Red) was added with stirring, and the basic aluminum chloride was adsorbed on mica titanium. After suction filtration, the product was dried at 80 ° C. for 10 hours to obtain 55.4 g of powder. This is powder A.

15.1 g of this powder A was calcined at 500 ° C. for 2 hours in a nitrogen atmosphere to obtain 14.0 g of powder. As a result of BET measurement, it was found to have a specific surface area of 150 m ² / g. This is powder B. The pH of the 5% aqueous suspension of Powder B was 4.0.

1.0 g of powder B is suspended in 50 g of water, and
A solution obtained by dissolving 0.08 g (Red No. 104, manufactured by Kishi Kasei) in 40 g of water was added while gradually stirring. This was stirred at 60 ° C. for 20 minutes, and then washed by filtration to obtain a colored powder.
This powder is designated as C.

Powder C was boiled with 100 g of water. Then filtration, washing with water,
After washing with ethanol and drying at 80 ° C., a flaky pigment showing a vivid red color in both powder color and coating color was obtained.

When this pigment was analyzed by X-ray diffraction, it was found that a part of the pigment was pseudo-boehmite. Further, as a result of SEM observation, growth of fine crystals was observed on the particle surface. The dye concentration was calculated based on the results of carbon analysis using a carbon analyzer EMIA-110 manufactured by HORIBA.
Was contained. When the powder color of the flaky pigment was measured with a color difference meter (Nippon Denshoku Co., Ltd., # 80), hue (H) = 7.24R, lightness (V) = 4.86, and saturation (C) = 14.93.
Met.

Example 2 Base aluminum chloride (trade name: Rocron-P, manufactured by Hoechst), composition formula: Al ₂ (OH) ₅ Cl · 2 to 3 (H ₂ O) 140 g was added to water 7
Dissolves in 100 g of mica titanium (M
50 g of Timiron Super Gold (manufactured by ERCK) was added with stirring to adsorb the base aluminum chloride to titanium mica. After suction filtration, the product was dried at 80 ° C. for 10 hours to obtain 55.4 g of powder.

Firing 15.1 g of this powder in a nitrogen atmosphere at 500 ° C. for 2 hours,
14.0 g of powder was obtained. As a result of the BET measurement,
It had a specific surface area of 150 m ² / g. The pH of this powder in a 5% aqueous suspension was 4.0.

1.0 g of this powder was suspended in 50 g of water, and a solution obtained by dissolving 0.08 g of tartrazine (Yellow No. 4, manufactured by Kishi Kasei) in 40 g of water was added thereto with gentle stirring. Then, the mixture was stirred at 60 ° C. for 20 minutes, washed by filtration, and a colored powder was obtained.

This powder was boiled with 100 g of water. Next, the resultant was filtered, washed with water, washed with ethanol, and dried at 80 ° C. to obtain a flaky pigment exhibiting a vivid yellow in both powder color and coating color.

When this pigment was analyzed by X-ray diffraction, it was found that a part of the pigment was pseudo-boehmite. Further, as a result of SEM observation, growth of fine crystals was observed on the particle surface. Also,
This pigment contains 7.4% of pigment, H = 3.13Y, V
= 7.84 and C = 9.40.

Example 3 140 g of basic aluminum chloride (trade name: Rocron-P, manufactured by Hoechst Co., composition formula: Al ₂ (OH) ₅ Cl · _{2 to} 3H ₂ O) was added to 700 g of water.
Titanium mica with a blue interference color (MERCK T
Imiron Super Blue (50 g) was added with stirring to adsorb basic aluminum chloride to mica titanium. After suction filtration, the product was dried at 80 ° C. for 10 hours to obtain 55.4 g of powder.

Firing 15.1 g of this powder in a nitrogen atmosphere at 500 ° C. for 2 hours,
14.0 g of powder was obtained. As a result of the BET measurement,
It had a specific surface area of 150 m ² / g. The pH of this powder in a 5% aqueous suspension was 4.0.

1.0 g of this powder was suspended in 50 g of water, and a solution obtained by dissolving 0.08 g of Brilliant Blue FCF (Blue No. 1, manufactured by Kishi Kasei) in 40 g of water was added thereto while stirring gradually. Then 60
The mixture was stirred at 20 ° C. for 20 minutes, and washed by filtration to obtain a colored powder.

This powder was boiled with 100 g of water. Then, filtration, washing with water, washing with ethanol, and drying at 80 ° C., a flaky pigment showing a clear blue color in both powder color and coating color was obtained. When this pigment was analyzed by X-ray diffraction, it was found that a part of the pigment was pseudo-boehmite. Further, as a result of SEM observation, growth of fine crystals was observed on the particle surface. Further, this pigment contains 7.0% of a coloring matter, H = 3.93B, V = 3.90,
C was 8.31.

Example 4 Powder prepared exactly as powder C obtained in Example 1
1.0 g was placed in an autoclave, and 100 g of water was added thereto. The resulting suspension was heated to 130 ° C. in 30 minutes, kept as it was for 1 hour, and allowed to cool to 70 ° C. in 30 minutes. The treated powder obtained by washing and drying this was a flaky pigment showing a clear red color in both the powder color and the coating color. When this pigment was analyzed by X-ray diffraction, it was found that a part of the pigment was pseudo-boehmite. Further, as a result of SEM observation, growth of fine crystals was observed on the particle surface. This pigment contained 7.4% of a dye, and had H = 7.20R, V = 4.80, and C = 14.98.

Comparative Example 1 A pigment was obtained by the method described in JP-A-51-17910. That is, 60 g of mica titanium as in Example 1 was added to ion-exchanged water 2
And heated to 75 ° C. with stirring. To this was added an aqueous sodium hydroxide solution to adjust the pH value to 8, and further
The AlCl ₃ · 6H ₂ O 8.5g was gradually injected a solution obtained by dissolving in water 350 ml. At the same time, a 7.5% aqueous sodium hydroxide solution was added to maintain the pH at 8 throughout the reaction.
Thereafter, the mixture was further stirred for 1 hour, and the obtained pigment was filtered, washed, and dried at 120 ° C. 5% pH of 7.7
Met. 1.0 g of this powder was suspended in 50 g of water, and a solution prepared by dissolving 0.08 g of Phloxine B (Red No. 104, manufactured by Kishi Kasei) in 40 g of water was added thereto with gentle stirring. Then 60 ° C,
Stir for 20 minutes, wash by filtration, H = 5.3R, V = 6.22, C = 1
A red flaky pigment of 2.38 was obtained. This pigment was not hydrothermally treated.

Comparative Example 2 Powder C was prepared in exactly the same manner as powder C obtained in Example 1. This powder was not subjected to hydrothermal treatment. When this pigment was analyzed by X-ray diffraction, it was found to be χ-alumina, and no pseudo-boehmite was generated. Also,
As a result of SEM observation, the particle surface was smooth. The obtained red powder contains 7.4% of the pigment, H = 7.20R,
V = 4.90, C = 14.90.

Comparative Example 3 Powder prepared in exactly the same manner as Powder A obtained in Example 1
15.0 g was baked in the air at 500 ° C. for 2 hours to obtain 14.0 g of powder. As a result of BET measurement, this product has a specific surface area of 140 m ² / g
Γ-alumina having the following formula: Also, 5% of this powder
The pH in the water suspension was 4.2.

1.0 g of this powder was suspended in 50 g of water, and Phloxine B was added thereto.
A solution obtained by dissolving 0.08 g in 40 g of water was added while gradually stirring. Then, the mixture was stirred at 60 ° C. for 20 minutes, and washed by filtration to obtain a colored powder.

This powder was boiled with 100 g of water. Next, it was filtered, washed with water, washed with ethanol, and dried at 80 ° C. to obtain a colored powder.
The pigment was analyzed by X-ray diffraction and found to be γ-alumina, not pseudoboehmite and not subjected to hydrothermal treatment. This pigment contains 7.0% of a coloring matter,
= 7.20R, V = 4.95, C = 13.80.

Comparative Example 4 Powder prepared exactly in the same manner as powder A obtained in Example 1
15.0 g was calcined at 600 ° C. for 2 hours in a nitrogen atmosphere to obtain 13.6 g of powder. As a result of BET measurement,
γ-alumina having m ² / g. The pH of the powder in a 5% aqueous suspension was 4.9.

1.0 g of this powder was suspended in 50 g of water, and Phloxine B was added thereto.
A solution obtained by dissolving 0.08 g in 40 g of water was added while gradually stirring. Then, the mixture was stirred at 60 ° C. for 20 minutes, and washed by filtration to obtain a colored powder.

This powder was boiled with 100 g of water. Thereafter, the mixture was filtered, washed with water, washed with ethanol, and dried at 80 ° C. to obtain a colored powder.
The pigment was analyzed by X-ray diffraction and found to be γ-alumina, not pseudoboehmite and not subjected to hydrothermal treatment. This pigment contains 5.0% of a pigment,
= 7.00R, V = 5.20, C = 13.00.

Test Example The performance of the invention shown in the example was compared with that of a comparative example.

0.2 g of the flaky pigment obtained in each of the above Examples and Comparative Examples was suspended in water, ethanol, or a 0.3% saline solution.
After shaking at 0 ° C. for 1 hour, the mixture was filtered. The dye concentration in the filtrate was quantified by spectrophotometry (manufactured by Shimadzu, UV-200), and the amount of dye eluted was examined. The results are shown in Table 1 (unit: pp
b).

From the above test examples, it was found that the pigment of the present invention was excellent in water resistance and solvent resistance.

Reference Example 1 Nail enamel: (composition A) (g) nitrocellulose 20.0 alkyd resin 15.0 camphor 3.0 plasticizer (dibutyl phthalate) 6.0 butyl acetate 23.0 ethyl acetate 9.0 isopropanol 7.0 butanol 2.0 toluene 4.8 (composition B) (g) Example 1 Pigment 2.0 Organically Modified Bentonite 1.2 (Production Method) After mixing and dissolving composition A, composition B was added.

The nail enamel described above had both a clear appearance color and pearl luster.

Reference Example 2 Lipstick: (composition) (g) carnauba wax 2 ceresin 7 candelilla wax 5 microstalin wax 5 beeswax 5 lanolin 4 castor oil 40 hexadecyl alcohol 15 sucrose pentastearate 5 pigment of Example 1 12 antioxidant -Appropriate amount of fragrance (Production method) The components excluding the pigment in the above composition were mixed and dissolved by heating at 90 ° C, and then the pigment was added and molded.

The obtained lipstick had both a clear appearance color and a pearly luster, and the appearance color and the application color matched.

Reference Example 3 Powder eye shadow: (Composition) (g) Talc 15 sericite 30 Pigment of Example 1 38 Ultramarine 5 Iron oxide 22 2-Ethylhexanoic acid triglyceride 6 Lanolin 5 Polyethylene wax 4 (Production method) Powder portion of the above composition Was stirred and mixed with a blender, and the oil phase portion heated and uniformly dissolved was sprayed on the mixture to further stir.
Thereafter, compression molding was performed with a pulverized molding machine to produce a solid powder eyeshadow.

The obtained eye shadow had a clear appearance and a natural finish with no glare at the time of application and application.

〔The invention's effect〕

Dye-containing flaky pigment obtained by the production method of the present invention,
Excellent in lightness, saturation, gloss and smoothness, and also excellent in stability such as water resistance, solvent resistance, weather resistance and safety, so that in addition to cosmetics, paints, plastics, inks, paints, sun Brilliant colors and pearl luster can be imparted to household goods, ornaments and the like.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-53-92842 (JP, A) JP-A-56-16559 (JP, A) JP-A-52-148632 (JP, A) JP-A-2- 34669 (JP, A) JP-A-2-16168 (JP, A) JP-A-63-152671 (JP, A) JP-B-59-36663 (JP, B2) (58) Fields investigated (Int. Cl. ⁶ , DB name) C09C 1/00-3/12 A61K 7/02 A61K 7/021

Claims (1)

(57) [Claims] 1. After adsorbing basic aluminum on a flaky inorganic powder coated with titanium oxide, baking at 200 to 500 ° C. in a vacuum atmosphere or an inert gas atmosphere to obtain an organic dye. And then subjecting it to a hydrothermal treatment.