KR101878136B1 - Manufacturing method of composite pigments using microwave - Google Patents

Abstract

The present invention relates to a method for producing a composite pigment using microwave. According to the present invention, the production method includes a process of treating microwave under specific treatment condition on the composite pigment which has specific moisture content and is in a cake state, during a process of adsorbing an organic pigment on a surface of a plate-like pigment, thereby remarkably improving color expression.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a composite pigment using microwave,

The present invention relates to a method for producing a composite pigment using microwaves.

In general, color pigments used in color cosmetics use various organic color pigments.

Organic color pigments generally used can be divided into natural pigments and synthetic pigments, but they prefer synthetic tar pigments rather than natural ones in terms of stable supply and economic efficiency.

The tar pigments, which are organic pigments that express general colors, use azo pigments (yellow, red), thioindigo (blue) and triphenylmethane (blue) in various industrial fields as well as the cosmetics industry.

However, most commonly used tar pigments are pigments in which the coloring dyes are laced with calcium, aluminum, barium, zirconium, or the like with a polyvalent metal salt through ionic bonding in order to reduce the solubility of the solvent.

These organic pigments have strong cohesion through laking, and because of coagulation between particles due to metal coagulants in the productized state, it is necessary to homogenize them through a strong dispersion process so that consumers can express desired feeling and color development .

Also, when applied to a powder type makeup or an oil-based dispersion type make-up formulation, even if a pulverizer is mixed with a Henschel mixer for 2 to 3 times, color dispersion is not properly performed, It has a disadvantage of inhibiting one color.

The present inventors have found that the color expressing ability is remarkably improved by microwave treatment of a composite pigment having a specific water content in a cake state in a process of adsorbing organic pigments on the surface of a platelet-shaped pigment, and completed the present invention .

Published patent application No. 10-2012-0049589

An object of the present invention is to provide a method for producing a composite pigment using microwaves.

Another object of the present invention is to provide a composite pigment produced by the above production method.

It is still another object of the present invention to provide a cosmetic composition comprising the composite pigment.

In order to achieve the above object,

The present invention relates to a method for preparing a pigment dispersion, comprising the steps of (1) preparing a plate-like pigment dispersion solution by mixing a plate-like pigment and distilled water and adjusting the pH to 5-6;

Preparing a mixed solution of an organic pigment, sodium hydroxide, aluminum salt hydrate and distilled water (step 2);

The mixed solution prepared in Step 2 was added to the plate-like pigment dispersion solution prepared in Step 1, stirred, washed with distilled water, filtered, and stirred at 50-90 ° C to prepare a cake containing 30-50 wt% (Step 3); And

Treating the moisture-containing cake prepared in the step 3 with a microwave of 750 to 950 W power for 1 to 10 minutes (step 4);

And a method for producing the composite pigment.

The present invention also provides a composite pigment produced by the above-mentioned production method.

Further, the present invention provides a cosmetic composition comprising the composite pigment.

The production method according to the present invention has the effect of remarkably improving the color expressing power by treating the composite pigment in a cake state having a specific moisture content with a microwave of a specific processing condition in the step of adsorbing the organic pigment on the surface of the platy pigment.

Fig. 1 shows the result of evaluation of color expressive power according to the moisture content of the cake of Examples 1-1 to 1-5 and Comparative Example 1. Fig.
Fig. 2 is a result of evaluating the color expressive power according to the moisture content of the cake of Examples 2-1 to 2-5 and Comparative Example 2. Fig.
Fig. 3 shows the result of evaluating color expressive power according to the microwave power of Examples 1-6 to 1-9.
FIG. 4 is a result of evaluating color expressive power according to the microwave power of Examples 2-6 to 2-9.
Fig. 5 shows results of evaluation of color expressive power according to microwave processing times of Examples 1-10 to 1-13. Fig.
FIG. 6 shows results of evaluating the color expressive power according to the microwave processing time in Examples 2-10 to 2-13. FIG.
FIG. 7 shows the result of evaluation of the hidden expressive color expressive force.

Hereinafter, the present invention will be described in detail.

Manufacturing method

The present invention relates to a method for preparing a pigment dispersion, comprising the steps of (1) preparing a plate-like pigment dispersion solution by mixing a plate-like pigment and distilled water and adjusting the pH to 5-6;

Preparing a mixed solution of an organic pigment, sodium hydroxide, aluminum salt hydrate and distilled water (step 2);

The mixed solution prepared in Step 2 was added to the plate-like pigment dispersion solution prepared in Step 1, stirred, washed with distilled water, filtered, and stirred at 50-90 ° C to prepare a cake containing 30-50 wt% (Step 3); And

Treating the moisture-containing cake prepared in the step 3 with a microwave of 750 to 950 W power for 1 to 10 minutes (step 4);

And a method for producing the composite pigment.

In the manufacturing method according to the present invention, the step 1 is a step of preparing a plate-like pigment dispersion solution by mixing a plate-shaped pigment and distilled water and adjusting the pH to 5-6.

As the plate-like pigment, mica, sericite, and a pearlescent pigment in which titanium dioxide has been surface-treated may be used singly or in combination. In addition, TiO (OH) ₂ is formed by hydrolysis of titanium chloride (TiCl ₄ ) directly on the surface using natural or synthetic mica as a starting material and then converted to TiO ₂ by calcination at a high temperature have. The platelet-shaped pigment may be a mica or sericite, or a particle type containing 20 to 65% by weight of titanium dioxide, having an average particle diameter of 1 to 15 탆 and a thickness of 1 탆 or less, but is not limited thereto .

In the manufacturing method according to the present invention, the step 2 is a step of preparing a mixed solution of an organic pigment, sodium hydroxide, aluminum salt hydrate and distilled water. Specifically, a dispersion solution can be prepared by adding 50 to 150 g of a platelet pigment to 5 to 10 L of distilled water, and the pH of the dispersion solution can be adjusted to 5 to 6.

The organic pigments may be azo pigments (yellow, red), thioindigo (blue), triphenylmethane (blue) and the like. C < / RTI > Red # 40, CI16035), Red No. 104 (D & C Red # 28, CI45410), Red No. 201 (D & C Red # 6, CI15850), Red No. 202 Ca Lake, CI 15850: 1), Red 218 (D & C Red # 27, CI45410), Red 220 (D & C Red # 34 Ca Lake, CI15880: C < / RTI > Red # 22 Al Lake, CI 45380), Blue No. 1 (FD & C Blue # FD & C Yellow # 5 Al Lake, CI 19140), Yellow No. 5 (FD & C Yellow # 6 Al Lake, CI 15985). In one embodiment of the present invention, an organic pigment represented by the following Chemical Formula 1 (Yellow No. 4) and Chemical Formula 2 (Red No. 202) was used.

FD & C Yellow # 5 Al Lake, CI 19140)

Red No. 202 (D & C Red # 7 Ca Lake, CI15850: 1)

In the step 2, AlCl ₃ .6H ₂ O, AlK (SO ₄ ) ₂ .12H ₂ O and the like can be used as the aluminum salt hydrate, and the aluminum salt hydrate can be chemically adsorbed while the organic pigment is hydrolyzed to the surface of the platelike pigment Can play a role. The aluminum salt hydrate may be used in an amount of 1 to 15% by weight in the total weight of the mixed solution of the step 2.

In step 3, the mixed solution prepared in step 2 is added to the plate-like pigment dispersion solution prepared in step 1, stirred, washed with distilled water, filtered, and stirred at 50-90 ° C. To prepare a cake containing 30-50 wt% moisture.

The moisture content of the cake is a factor affecting the subsequent microwave treatment in step 4, and is an important factor in expressing color. Preferably, the moisture content of the cake is 40-45 wt% (see Experimental Example 1).

In the manufacturing method according to the present invention, the step 4 is a step of treating the moisture-containing cake prepared in the step 3 with a 750 to 950 W output microwave for 1 to 10 minutes.

Here, the water-containing cake can be subjected to microwave treatment in units of 5-15 g (preferably 7-13 g, more preferably 8-12 g, still more preferably 9-11 g, particularly preferably 10 g) .

Preferably, the microwave power is 800-900 W and the treatment time is 2.5-3.5 min (see Experimental Example 2-3).

Conventional heater heat treatment method (Comparative Example 1-2) has a problem that surface-treated organic pigments are not uniformly dispersed on the surface of the platelike pigments and aggregation causes degradation of color expressing power. However, in the microwave treatment according to the present invention, It is uniformly dispersed on the surface of the pigment and the color expressing power is improved.

Composite pigment

The present invention provides a composite pigment produced by the above process.

The composite pigment prepared by the process of the present invention has an effect of remarkably improving color expressing power (see Experimental Example 1-3).

Cosmetics  Composition

The present invention provides a cosmetic composition comprising the composite pigment.

The cosmetic composition comprising the composite pigment according to the present invention has an effect of remarkably improving the hue of color.

The cosmetic composition may contain at least one selected from the group consisting of silicone, silane, silicone copolymer, amino acid, amino acid derivative, lauroyl lysine, lecithin and lecithin derivatives for improvement of hydrophobicity, hydrophilicity or skin affinity of the composite pigment Component. ≪ / RTI >

Hereinafter, the present invention will be described in more detail with reference to the following examples. However, the following examples are illustrative of the present invention, and the present invention is not limited by the following examples.

< Example 1 > Organic Color Pigment Yellow No. 4 ( 50 wt% Manufacture of surface-treated composite pigments

Yellow No. 4 (FD & C Yellow # 5 Al Lake: Sun Chemical, USA)

Step 1: Plate  Preparation of pigment dispersion solution

7 liters of distilled water and 100 g of flaky mica pigment were added to a beaker and the pH was adjusted to 5 to 6 at room temperature while stirring to prepare a mica dispersion solution.

Step 2: Organic pigment, sodium hydroxide and Aluminum chloride hydrate  Preparation of mixed solution

A solution of 100 g of FD & C Yellow # 5 Al Lake: Sun Chemical (USA) in 5 wt% of sodium hydroxide and 700 g of purified water and 700 g of a 15 wt% aqueous solution of AlCl ₃ .6H ₂ O were prepared.

Step 3: Preparation of moisture-containing cake

The mixed solution prepared in Step 2 was gradually added to the plate-like pigment dispersion solution prepared in Step 1 through a dosing device. After completion of the addition, the mixture was further stirred for 30 minutes. After completion of the reaction, the mixture was washed with distilled water, filtered, and stirred at 50-70 ° C to prepare a cake containing 30-50% moisture.

Step 4: microwave treatment

10 g of the moisture-containing cake prepared in the step 3 was treated with a microwave of 750 to 950 W for 1 to 10 minutes to prepare a dried composite pigment.

Specifically, the moisture content of the cake and microwave treatment conditions (output and time) are shown in Tables 1 to 3 below.

< Example  2> Organic color pigment Red No. 202 ( 15 wt% Manufacture of surface-treated composite pigments

D & C Redw # 7 Ca Lake: Sun Chemical (USA)

Step 1: Plate  Preparation of pigment dispersion solution

7 liters of distilled water and 100 g of flaky mica pigment were added to a beaker and the pH was adjusted to 5 to 6 at room temperature while stirring to prepare a mica dispersion solution.

Step 2: Organic pigment, sodium hydroxide and Aluminum chloride hydrate  Preparation of mixed solution

100 g of a 5% by weight aqueous solution of sodium hydroxide and 1,000 g of purified water, 100 g of a 5% by weight aqueous solution of AlCl ₃ .6H ₂ O and 3 g of a sodium hydroxide solution of 100% by weight of sodium hydroxide (D & C Redw # 100 g of an aqueous solution was prepared.

Step 3: Preparation of moisture-containing cake

The mixed solution prepared in Step 2 was gradually added to the plate-like pigment dispersion solution prepared in Step 1 through a dosing device. After completion of the addition, the mixture was further stirred for 30 minutes. After completion of the reaction, the mixture was washed with distilled water, filtered, and stirred at 50-70 ° C to prepare a cake containing 30-50% moisture.

Step 4: microwave treatment

10 g of the moisture-containing cake prepared in the step 3 was treated with a microwave of 750 to 950 W for 1 to 10 minutes to prepare a dried composite pigment.

Specifically, the moisture content of the cake and microwave treatment conditions (output and time) are shown in Tables 1 to 3 below.

< Comparative Example  1> Preparation of yellow pigment

A yellow pigment was prepared in the same manner as in Example 1, except that the heat treatment was conducted in place of the microwave treatment.

< Comparative Example  2> Preparation of Red Pigment

A yellow pigment was prepared in the same manner as in Example 2, except that the heat treatment was conducted in place of the microwave treatment.

How to evaluate color expressive power

The composite pigments of the above Examples and Comparative Examples were mixed in nitrocellulose at a ratio of 5% by weight and applied to a concealed ratio using a BAR APPLICATOR (100 mm / 100 탆). Using a color difference meter (Minolta CM2500 C) L ^* a ^* b ^* and C (saturation, Chroma) were measured and compared.

The increase in L * means an increase in whiteness, expressed as a value from 0 to 100,

An increase in + value of a * value indicates an increase in red color, an increase in - value means an increase in green color, represented by a value of -100 to +100,

An increase in + value for b * indicates an increase in yellow color, an increase in - value means an increase in blue color, and a value from -100 to +100,

An increase in C (Chroma) value means an increase in saturation, expressed as a value between 0 and 100.

In general, the color expressive power can be interpreted to be superior to the color (or average) color difference values L ^* a ^* b ^* and C (chroma) values appearing in each color.

< Experimental Example  1> Evaluation of Color Expression According to Cake Moisture Content

In order to examine the influence of the moisture content of the cake on the expressive power of color, Examples and Comparative Examples were prepared under the conditions shown in Table 1 below.

cake
Water content (% by weight) Microwave
Output (W) Microwave
Processing time (min) Example 1-1 30



850



3 Examples 1-2 35 Example 1-3 40 Examples 1-4 45 Examples 1-5 50 Example 2-1 30 Example 2-2 35 Example 2-3 40 Examples 2-4 45 Example 2-5 50 Comparative Example 1 40 - - Comparative Example 2 40 - -

Examples 1-1 to 1-5 and Comparative Example 1 are samples of a yellow composite pigment, and the results are shown in FIG.

As shown in FIG. 1, in Examples 1-1 to 1-5, the yellow expressiveness was significantly improved compared to Comparative Example 1. In Examples, Examples 1-3 (moisture content 40% by weight) and Examples 1-4 (moisture content 45% by weight), and the moisture content of the cake was most preferably in the range of 40-45% by weight.

Examples 2-1 to 2-5 and Comparative Example 2 are samples of a red composite pigment, and the results are shown in Fig.

As shown in Fig. 2, in Examples 2-1 to 2-5, the hue of color reproduction was markedly improved compared to Comparative Example 2. In Examples 2-1 to 2-5, Example 2-3 (moisture content 40% by weight) and Example 2-4 (moisture content: 45% by weight) exhibited remarkably excellent red expressing power, and the moisture content of the cake was most preferably in the range of 40-45% by weight.

In Experimental Examples 2 and 3 below, optimal microwave power and processing time were derived based on an optimum moisture content of 40% by weight.

< Experimental Example  2> Evaluation of color expressive power according to microwave output

In order to examine the effect of the microwave output on the color expressing power, Examples and Comparative Examples were prepared under the conditions shown in Table 2 below.

cake
Water content (%) Microwave
Output (W) Microwave
Processing time (min) Examples 1-6


40 750


3 Examples 1-7 800 Examples 1-8 900 Examples 1-9 950 Examples 2-6 750 Examples 2-7 800 Examples 2-8 900 Examples 2-9 950

Examples 1-6 to 1-9 are samples of yellow composite pigments, and the results are shown in Fig.

As shown in Fig. 3, in Examples 1-6 to 1-9, yellow expressions of Examples 1-7 (output 800W) and Example 1-8 (output 900W) were remarkably excellent, and microwave output It was found that the range of 800-900 W was the most preferable.

Examples 2-6 to 2-9 are samples of a red composite pigment, and the results are shown in Fig.

As shown in Fig. 4, in Examples 2-6 to 2-9, the red expressing power of Example 2-7 (output 800W) and Example 2-8 (output 900W) were remarkably excellent, It was found that the range of 800-900 W was the most preferable.

In Experimental Example 3, optimum microwave processing time was derived based on an optimum moisture content of 40% and an optimum microwave output of 850 W.

< Experimental Example  3> Evaluation of color expressive power according to microwave processing time

In order to examine the influence of the microwave treatment time on the color expressive power, Examples and Comparative Examples were prepared under the conditions shown in Table 3 below.

cake
Water content (%) Microwave
Output (W) Microwave
Processing time (min) Example 1-10


40


850 2 Example 1-11 2.5 Examples 1-12 3.5 Examples 1-13 4 Examples 2-10 2 Examples 2-11 2.5 Examples 2-12 3.5 Examples 2-13 4

Examples 1-10 to 1-13 are samples of a yellow composite pigment, and the results are shown in Fig.

As shown in Fig. 5, in Examples 1-10 to 1-13, the yellow expressive power of Example 1-11 (treatment time 2.5 min) and Example 1-12 (treatment time 3.5 min) It was found that the microwave treatment time was most preferably in the range of 2.5-3.5 min.

Examples 2-10 to 2-13 are samples of a red composite pigment, and the results are shown in Fig.

As shown in FIG. 6, in Examples 2-10 to 2-13, the red expressive power of Examples 2-11 (2.5 min treatment time) and 2-12 (3.5 min treatment time) It was found that the microwave treatment time was most preferably in the range of 2.5-3.5 min.

< Experimental Example  4> Hide Yulgyi  Evaluation of Color Expression Through

In order to visually evaluate the yellow expressiveness of Examples 1-3 and Comparative Example 1 and the red expression power of Examples 2-3 and Comparative Example 2, a BAR APPLICATOR (100 mm / 100 탆) was applied to the cover paper, , And the results are shown in FIG.

As shown in FIG. 7, it was found that the yellow expressive power of Example 1-3 was remarkably improved as compared with Comparative Example 1, and the red expressive power of Example 2-3 was remarkably improved as compared with Comparative Example 2.

Claims (8)

Mixing the platelet-shaped pigment and the distilled water and adjusting the pH to 5-6 to prepare a plate-shaped pigment dispersion solution (step 1);
Preparing a mixed solution of an organic pigment, sodium hydroxide, aluminum salt hydrate and distilled water (step 2);
The mixed solution prepared in Step 2 was added to the plate-like pigment dispersion solution prepared in Step 1, stirred, washed with distilled water, filtered, and stirred at 50-90 ° C to prepare a cake containing 40-45 wt% (Step 3); And
Treating the moisture-containing cake prepared in step 3 with a microwave of 800-900 W power for 2.5-3.5 minutes (step 4);
&Lt; / RTI &gt;
The method according to claim 1,
Wherein the plate-like pigment in the step (1) is selected from the group consisting of mica, sericite, and a pearlescent pigment in which titanium dioxide has been surface-treated.
The method according to claim 1,
Wherein the organic pigment is selected from the group consisting of azo pigments, thioindigo and triphenylmethane.
The method of claim 3,
Wherein the organic pigment is a compound represented by the following general formula (1) or (2).
[Chemical Formula 1]

(2)

delete A composite pigment produced by the method of claim 1.
A cosmetic composition comprising the composite pigment of claim 6.
8. The method of claim 7,
Wherein the cosmetic composition further comprises at least one component selected from the group consisting of silicone, silane, silicone copolymer, amino acid, amino acid derivative, lauroyl lysine, lecithin and lecithin derivatives.

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