JPH09194329A - Powder cosmetic - Google Patents

Abstract

PROBLEM TO BE SOLVED: To prepare a powder cosmetic good in touch feeling when applied, excellent in skin protectiveness against ultraviolet radiation, containing modified zinc oxide-based fine powder. SOLUTION: This powder cosmetic contains 0.5-95wt.% of modified zinc oxide fine powder prepared by coating mixed powder composed of fine zinc oxide particles 0.001-0.1μm in average primary particle diameter and flaky powder 8-12 in whiteness with an acylated amino acid. The flaky powder is pref. of barium sulfate which is excellent in feeling when used and high in fine zinc oxide particle dispersion effect, its use being 2.5-50 pts.wt. based on 100 pts.wt. of the fine zinc oxide particles. The mixed powder is prepared by dry mixing using e.g. a juicier-mixer. For the coating, 0.5-50 pts.wt. of the acylated amino acid such as N-lauroyl-L-lysine is used based on 100 pts.wt. of the mixed powder, and the coating operation is of wet type. This powder cosmetic can be prepared into e.g. powder foundation, face powder, eyeshadow, pressed powder, cheek color.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention is characterized by containing a modified fine particle zinc oxide-based powder obtained by coating a mixed powder comprising fine particle zinc oxide and a specific flaky powder with an acylated amino acid. And powder cosmetics. More specifically, the present invention relates to a powder cosmetic having a good feeling in use and a high UV protection effect, which is characterized by containing surface-treated fine zinc oxide powder having excellent transparency and dispersibility and having an UV protection effect.

[0002]

2. Description of the Related Art In recent years,
The elucidation of the effects of A-region ultraviolet rays (UVA) on the skin has progressed, and B
Not only in the range of ultraviolet rays (UVB) but also in correspondence with UVA is regarded as one of the important issues in cosmetics, and cosmetics having a high UVA protective effect have been strongly desired.

Conventionally, since inorganic powders such as titanium oxide and zinc oxide have a UV shielding ability to absorb and scatter UV rays, they have been blended in powder cosmetics as UV protective agents. However, the generally used inorganic powder has a particle size of about 0.2 to about 1 μm, a large refractive index, and absorbs and scatters ultraviolet rays, and at the same time, strongly scatters visible light as well. It has a problem that the natural transparency is significantly impaired.

Therefore, recently, attention has been paid to a method of improving the transparency by making an inorganic powder into fine particles, and a UVA-compliant ultrafine inorganic powder characterized by shape and size (particle diameter, particle size distribution), particularly fine particle oxidation. Titanium and zinc oxide fine particles are being actively developed. However, fine particle titanium oxide compatible with UVA has a strong whiteness and a weak hiding power, so that when it is blended in a large amount in powder cosmetics, there is a problem that whitening occurs, and the blending amount is limited. . On the contrary,
Since fine zinc oxide has less whiteness, it is possible to increase the blending amount in powder cosmetics, and when the whiteness is kept constant, a higher UV protection effect can be obtained compared to fine titanium oxide. Are known.

However, not only fine particle titanium oxide and fine particle zinc oxide but fine particle inorganic powder is a general phenomenon irrespective of its shape. It also has a problem that it cannot be fully exhibited because it is easy and it is difficult to be uniformly dispersed in the powder cosmetic.

[0006]

As a result of intensive studies in view of the above points, the present inventors have found that the fine zinc oxide particles have a whiteness of 8 to 8
By coating a mixed powder consisting of flaky powder in the range of 12 with an acylated amino acid, the resulting modified fine particle zinc oxide-based powder has a high UV protection effect and maintains the friction of fine particle zinc oxide. It was found that the unpleasant feeling of use such as feeling and poor elongation is improved. Furthermore, since the modified fine particle zinc oxide powder has little whiteness and has a natural transparency, it can be incorporated in a large amount in powder cosmetics. Excellent,
Moreover, it is possible to obtain a powder cosmetic having a good feeling in use.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The particulate zinc oxide used in the present invention has an average primary particle diameter in the range of 0.001 to 0.1 μm. Within this range, a high UV protection effect is obtained, and at the same time, the effect of improving the dispersibility by the flaky powder having a whiteness in the range of 8 to 12 is remarkably recognized. When the average primary particle diameter of the fine particle zinc oxide is less than 0.001 μm,
The obtained powder cosmetic has a bad feeling in use, the industrial production of the raw material is difficult, and the average primary particle size is 0.
If it exceeds 1 μm, the cosmetic film becomes whitish, so the average primary particle diameter of the fine particle zinc oxide is 0.001 to 0.1 μm.
Must be within the range. Examples of the method of measuring the average primary particle diameter include a method of using the particle diameter obtained from scanning type or transmission type electron microscope observation.

The flaky powder having a whiteness of 8 to 12 used in the present invention is particularly limited as long as it is a powder having a high transparency, suppressing the aggregation of fine zinc oxide particles and enhancing the dispersibility. Not done. The flaky powder here includes a plate-like powder and a flaky powder, and preferably has a thickness of 0.00
It refers to one in the range of 1 to 0.15. Within this range, the ability to suppress the agglomeration of zinc oxide fine particles and to disperse them uniformly is very high. If the whiteness of the flaky powder is less than 8, it is difficult to obtain raw materials, and if the whiteness exceeds 12, the cosmetic film becomes whitish. Must be in the 12 range. Examples of these flaky powders include barium sulfate, silk powder, talc, sericite, kaolin, mica titanium, calcium carbonate, magnesium carbonate, aluminum silicate, magnesium sulfate, and the like, and surface-treated powders thereof. Or two or more species. Of these, barium sulfate is particularly preferable because it has an excellent feeling in use and has a high effect of dispersing fine particle zinc oxide.

As a whiteness evaluation method in the present invention,
0.24 mg / cm ² powder is applied to black paper, and its brightness is measured by a color difference meter (for example, Minolta colorimetric device DP300).
L ^* value is L1 when the color is measured using, and the brightness of black paper is L
When the value is 2, a method of setting the value of L1-L2 to whiteness can be mentioned. As the whiteness of the flaky powder used in the present invention,
Those in the range of 8 to 12 are necessary for imparting transparency to the modified fine particle zinc oxide-based powder.

The amount of flaky powder having a whiteness of 8 to 12 used in the present invention varies depending on the kind, size and shape of the powder, but is 2.5 to 50 relative to 100 parts by weight of fine particle zinc oxide.
It is preferably in parts by weight. Within this range, the effect of increasing the transparency of the modified fine particle zinc oxide-based powder and the effect of smoothing the feel can be sufficiently exerted while maintaining the high ultraviolet protection effect of the fine particle zinc oxide.

In the present invention, the fine particle zinc oxide has a whiteness of 8
The method for obtaining the mixed powder from the flaky powder in the range of 12 to 12 is, for example, a method of dry-mixing the both using a juicer mixer or the like, or putting both in a suitable solvent such as water or ethanol. A method in which the solvent is removed after thorough stirring, drying, and pulverization can be mentioned.

The acylated amino acids used in the present invention include N-lauroyl-L-lysine and N-lauroyl-D.
-Lysine, N-palmitoyl-L-lysine, N-stearoyl-L-lysine and other lysine derivatives, N-palmitoyl-L-serine, N-stearoyl-L-serine and other serine derivatives and the like. Among these, N-lauroyl-L-lysine is particularly preferable from the viewpoint of the feeling of use of the modified fine particle zinc oxide-based powder produced and the raw material cost.

The amount of the acylated amino acid used in the present invention is 0.5 to 100 parts by weight based on 100 parts by weight of a mixed powder consisting of fine particle zinc oxide and flaky powder having a whiteness in the range of 8 to 12.
50 parts by weight are preferred. Within this range, sufficient smoothness can be imparted to the modified fine particle zinc oxide-based powder without impairing the high UV protection effect.

In the present invention, as a method of coating a mixed powder comprising fine particle zinc oxide and flaky powder having a whiteness in the range of 8 to 12 with an acylated amino acid, the effect of the present invention is obtained. Therefore, the wet coating method is preferable. .
As a wet coating method, for example, when the mixed powder is uniformly dispersed in a suitable solvent, an acylated amino acid dissolved in a suitable solvent is added, and pH control, temperature control, or the like is appropriately performed. Another method is to reprecipitate the acylamino acid on the surface of the mixed powder, followed by filtration, drying and pulverization.

The modified fine particle zinc oxide-based powder thus obtained has the finely divided zinc oxide uniformly dispersed around the flaky powder, and the acylated amino acid is uniformly covered with a thin layer. It takes the form of

Examples of powder cosmetics of the present invention include powder foundation, white powder, face powder, eye shadow, pressed powder, cheek color and the like.

In the present invention, the ratio of the modified fine particle zinc oxide powder blended in the powder cosmetic varies depending on the characteristics of the product, but it should be possible to obtain a high UV protection effect and an excellent feeling of use. It is preferable to add 0.5 to 95 parts by weight to 100 parts by weight of the powder cosmetic.

The powder cosmetics of the present invention include, in addition to the modified fine particle zinc oxide powder, powders used in powder cosmetics, colorants, oils, moisturizers, surfactants and sterilizers. Agents, fragrances, solvents, salts, sticky agents, polymers, preservatives and the like can be added at the same time. In particular, regarding the powders, conventionally known inorganic powders, organic powders, pigments, and composite powders thereof and powders subjected to surface treatment such as silicone treatment, fluorine compound treatment, metal soap treatment, and oil treatment. Is mentioned. In some cases, the modified fine particle zinc oxide-based powder of the present invention can be further surface-treated by a conventionally known surface treatment method.

Further, for the purpose of improving the ultraviolet protection effect, known ultraviolet rays such as titanium oxide, iron oxide, aluminum oxide, cerium oxide, calcium oxide, benzophenone derivatives, cinnamic acid derivatives, benzoic acid derivatives, salicylic acid derivatives, etc. It is also possible to use a protective agent together.

[0020]

The present invention will be described in detail below with reference to examples and comparative examples.

Sensory property test method Regarding the powder cosmetics of Examples and Comparative Examples, a professional panelist 1
A sensory test was conducted by 0 people, and three items, that is, smoothness when using the powdery cosmetic, spread on the skin, and whitishness of the cosmetic film were evaluated. Evaluation is the following 5 steps (5; very good,
4; good, 3; normal, 2; bad, 1; very bad), and the average value of 10 persons is shown in Table 2.

Evaluation Method of UV Protection Effect In September 1995 (sunny day, 2 days), powder cosmetics of Examples and Comparative Examples were actually used on the upper arms of 10 professional panelists and immediately blacked out visually. The protective effect of UVA was evaluated based on the presence or absence of aging. Here, when the number of panelists is A and the proportion of panelists who have not been immediately blackened is B, C = B / A × 10
The value of 0 was used to judge the ultraviolet protection effect. That is, C
The larger the value, the better the ultraviolet (UVA) protection effect.

Production Example 1 (Production of Modified Fine Particle Zinc Oxide Powder Used in Example 1) Fine Particle Zinc Oxide (Average Primary Particle Diameter 0.02 μm) 76
g and tabular barium sulfate (major axis 3 to 10 μm, minor axis 1 to 5
μm, thickness 0.1-0.3 μm, whiteness 11.1) 19g
Was mixed well with a juicer mixer to obtain a mixed powder. This was stirred by a stirrer with ultrasonic waves in a mixed solution of 6.9 g of 6N hydrochloric acid and 650 g of purified water.
Dispersed for minutes. To this, N-lauroyl-L-lysine 5
g 8.7 g of 5N sodium hydroxide aqueous solution, purified water 65
What was melt | dissolved in the mixed solution of g was slowly added over 20 minutes, and it reprecipitated on the mixed powder surface. Then p
After confirming the pH of the solution with an H meter, neutralization was completed using 1N hydrochloric acid or a 1N sodium hydroxide aqueous solution, followed by stirring for 15 minutes. The dispersion was filtered under reduced pressure, washed with water several times, and then it was confirmed with a salinometer that sodium chloride was completely removed. The obtained powder was transferred to a metal vat and dried for 12 hours with a blow dryer set at 85 ° C. The dried powder was pulverized using a mixer to obtain 98.2 g (yield 98.2%) of modified fine particle zinc oxide-based powder.

In the modified fine particle zinc oxide-based powder obtained in Production Example 1, almost all of the added N-lauroyl-L-lysine was coated on the surface of the mixed powder by electron microscope and infrared absorption spectrum analysis. I confirmed that. FIG.
The electron microscopic observation results of the modified fine particle zinc oxide-based powder shown in FIG. 2 show that N-lauroyl-L-lysine is a thin layer in a state in which the fine particle zinc oxide is uniformly dispersed around the flaky powder. It was confirmed that it took the form of covering.

Production Example 2 (Production of Modified Fine Particle Zinc Oxide Powder Used in Example 2) 81 g of the same fine particle zinc oxide as used in Production Example 1 and 9 g of plate barium sulfate may be used in a juicer mixer. Stir to mix. 6N hydrochloric acid 13.8g, purified water 6
50 g of the mixed solution was dispersed for 15 minutes by stirrer stirring with ultrasonic waves. In addition to this, N-lauroyl-L-
Lysine 10 g was added to a 5N sodium hydroxide aqueous solution 17.5.
g, 129 g of purified water, dissolved in a mixed solution was slowly added over 25 minutes, and re-precipitated on the surface of the mixed powder. Further, through the same operation as in Production Example 1, 96.3 g (yield 96.3%) of modified fine particle zinc oxide-based powder was obtained.
The obtained powder was confirmed by electron microscope and infrared absorption spectrum analysis that almost all of the added N-lauroyl-L-lysine was coated on the surface of the mixed powder.

Production Example 3 (Production of Modified Fine Particle Titanium Oxide Powder Used in Comparative Example 1) UVA-Compatible Fine Particle Titanium Oxide (Average Primary Particle Diameter
07 g) and 19 g of the plate-shaped barium sulfate used in Production Example 1 were well mixed by stirring using a juicer mixer. This was dispersed in a mixed solution of 6.9 g of 6N hydrochloric acid and 650 g of purified water by stirrer stirring for which ultrasonic waves were used in combination for 15 minutes. Add 5 g of N-lauroyl-L-lysine to this.
What was dissolved in a mixed solution of 8.7 g of an aqueous solution of sodium hydroxide N and 65 g of purified water was slowly added over 20 minutes, and re-precipitated on the surface of the mixed powder. Further, through the same operation as in Production Example 1, the modified fine particle titanium oxide based powder 98.
0 g (yield 98.0%) was obtained. The obtained powder was analyzed by an electron microscope and infrared absorption spectrum analysis.
It was confirmed that almost all of lauroyl-L-lysine was coated on the surface of the mixed powder.

Production Example 4 (Production of Surface-treated Fine Particle Zinc Oxide Used in Comparative Example 2) 90 g of the same fine particle zinc oxide used in Production Example 1 was used.
A mixed solution of 13.8 g of 6N hydrochloric acid and 650 g of purified water was dispersed for 15 minutes by stirrer stirring with ultrasonic waves.
A solution obtained by dissolving 10 g of N-lauroyl-L-lysine in a mixed solution of 17.5 g of a 5N sodium hydroxide aqueous solution and 129 g of purified water was slowly added to this over 25 minutes, and re-precipitated on the surface of the mixed powder. It was After the same operation as in Production Example 1, 99.1 g of surface-treated fine particle zinc oxide
(Yield 99.1%) was obtained. The obtained powder was confirmed by electron microscope and infrared absorption spectrum analysis that almost all of the added N-lauroyl-L-lysine was coated on the surface of the particulate zinc oxide.

Production Example 5 (Production of Modified Zinc Oxide Powder Used in Comparative Example 5) 76 g of zinc oxide (average primary particle size, 0.20 μm) and the same plate-like barium sulfate used in Production Example 1 19 g was well mixed by stirring using a juicer mixer. This is 6
A mixed solution of N hydrochloric acid (6.9 g) and purified water (650 g) was dispersed for 15 minutes by stirrer stirring with ultrasonic waves. To this, 5 g of N-lauroyl-L-lysine dissolved in a mixed solution of 8.7 g of a 5N sodium hydroxide aqueous solution and 65 g of purified water was slowly added over 20 minutes, and re-precipitated on the mixed powder surface. It was Further, through the same operation as in Production Example 1, 98.5 g of modified zinc oxide based powder (yield 98.5) was obtained.
%) Was obtained. The obtained powder was confirmed by electron microscope and infrared absorption spectrum analysis that almost all of the added N-lauroyl-L-lysine was coated on the surface of the mixed powder.

Production Example 6 (Production of Modified Fine Particle Zinc Oxide Powder Used in Comparative Example 6) 76 g of the same fine particle zinc oxide as used in Production Example 1 and 19 g of plate-shaped titanium oxide (whiteness 14.2) Was thoroughly mixed with stirring using a juicer mixer. This was added to 6N hydrochloric acid 6.
A mixed solution of 9 g and 650 g of purified water was dispersed for 15 minutes by stirrer stirring with ultrasonic waves. To this, 5 g of N-lauroyl-L-lysine dissolved in a mixed solution of 8.7 g of a 5N sodium hydroxide aqueous solution and 65 g of purified water was slowly added over 20 minutes, and re-precipitated on the mixed powder surface. It was Further, through the same operation as in Production Example 1, 97.8 g (yield 97.8%) of modified fine particle zinc oxide-based powder was obtained. The obtained powder was confirmed by electron microscope and infrared absorption spectrum analysis that almost all of the added N-lauroyl-L-lysine was coated on the surface of the mixed powder.

Production Example 7 (Production of Modified Fine Particle Zinc Oxide Based Powder Used in Comparative Example 8) 76 g of the same fine particle zinc oxide as used in Production Example 1 and substantially spherical barium sulfate (average particle diameter 0.8 μm) 19 g was well mixed by stirring using a juicer mixer. This was dispersed in a mixed solution of 6.9 g of 6N hydrochloric acid and 650 g of purified water by stirrer stirring for which ultrasonic waves were used in combination for 15 minutes. To this, 5 g of N-lauroyl-L-lysine dissolved in a mixed solution of 8.7 g of a 5N sodium hydroxide aqueous solution and 65 g of purified water was slowly added over 20 minutes, and re-precipitated on the mixed powder surface. It was Further, through the same operation as in Production Example 1, 98.1 g of a modified fine particle zinc oxide-based powder (yield 9
8.1%) was obtained. The obtained powder was analyzed by an electron microscope and infrared absorption spectrum analysis, and the added N-lauroyl-
It was confirmed that almost all of L-lysine was coated on the surface of the mixed powder.

Example 1 (Powder Foundation) A powder foundation was prepared according to the formulation shown in Table 1. The modified fine particle zinc oxide-based powder used was that produced in Production Example 1.

[0032]

[Table 1]

After the powders were mixed using a mixer, an oil agent component and a preservative were added and further mixed. After passing the obtained mixed powder through 60 mesh, it was stamped on a metal plate using a mold to obtain a powder foundation of the product.

Example 2 (Powder Foundation) All the steps were carried out except that the modified fine particle zinc oxide based powder (Production Example 2) was used in place of the modified fine particle zinc oxide based powder (Production Example 1) of Example 1. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Comparative Example 1 (Powder Foundation) All were carried out except that modified particulate titanium oxide based powder (Manufacturing Example 3) was used in place of the modified particulate zinc oxide based powder (Manufacturing Example 1) of Example 1. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Comparative Example 2 (Powder Foundation) The same as Example 1 except that the surface-treated fine particle zinc oxide (Production Example 4) was used in place of the modified fine particle zinc oxide-based powder (Production Example 1) of Example 1. A powder foundation was prototyped in the same manner.

Comparative Example 3 (Powder Foundation) Instead of the modified fine particle zinc oxide-based powder of Example 1 (Production Example 1), the same fine particle zinc oxide and tabular barium sulfate as those used in Production Example 1 were used. A powder foundation was produced in the same manner as in Example 1 except that a mixture of mixers at a ratio of 1 (weight ratio) was used.

Comparative Example 4 (Powder Foundation) All the steps were carried out except that the same modified zinc oxide powder as used in Production Example 1 was used in place of the modified fine particle zinc oxide powder (Production Example 1) of Example 1. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Comparative Example 5 (Powder Foundation) All the steps were carried out except that a modified zinc oxide based powder (Production Example 5) was used in place of the modified fine particle zinc oxide based powder (Production Example 1) of Example 1. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Comparative Example 6 (Powder Foundation) In place of the modified fine particle zinc oxide powder (Production Example 1) of Example 1, modified fine particle zinc oxide powder (Production Example 6) was used. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Comparative Example 7 (Powder Foundation) Instead of the modified fine particle zinc oxide-based powder of Example 1 (Production Example 1), the same fine particle zinc oxide and tabular barium sulfate as those used in Production Example 1 were used. , N-lauroyl-L-lysine was used in the same manner as in Example 1 except that a dry simple mixture of N: lauroyl-L-lysine at a ratio (weight ratio) of 76:19:15 was used.

Comparative Example 8 (Powder Foundation) In place of the modified fine particle zinc oxide powder (Production Example 1) of Example 1, modified zinc oxide powder (Production Example 7) was used. A trial production of a powder foundation was carried out in the same manner as in Example 1.

Table 2 shows the results of the sensory characteristic tests of Examples 1 and 2 and Comparative Examples 1 to 8 and the evaluation results of the ultraviolet protection effect.

[0044]

[Table 2]

From the results shown in Table 2, in Examples 1 and 2 in which the modified fine particle zinc oxide based powder of the present invention was blended, the modified fine particle titanium oxide based surface-treated with N-lauroyl-L-lysine was used. It can be seen that the whitishness of the cosmetic film is suppressed as compared with Comparative Example 1 in which the above is blended. As in Comparative Example 1, if a large amount of the modified fine particle titanium oxide-based powder is blended in order to obtain the ultraviolet protection effect, the cosmetic film is too whitish to be used as a commercial product. Also, regarding the smoothness at the time of use and the elongation on the skin, fine particle zinc oxide alone was used as N-lauroyl-
In comparison with Comparative Example 2 containing L-lysine treated, Comparative Example 3 containing a simple mixture of fine particle zinc oxide and tabular barium sulfate, and Comparative Example 4 containing conventional fine particle zinc oxide as it is. However, it is also clear that Examples 1 and 2 are significantly superior. Furthermore, even when compared with Comparative Example 7 in which a simple mixture of fine particle zinc oxide, barium sulfate in plate form, and N-lauroyl-L-lysine was blended, in terms of smoothness during use and elongation on the skin, Examples 1 and 2 were significantly superior. Furthermore, as compared with Comparative Example 8 in which modified fine particle zinc oxide-based powder using barium sulfate having a substantially spherical shape rather than flaky shape was blended, smoothness in use, elongation on skin, whitening of cosmetic film were observed. Examples 1 and 2 were significantly superior in terms of softness. The same method as the modified fine particle zinc oxide-based powder used in the present invention except that the flaky powder of Comparative Example 6 having a whiteness value outside the whiteness range of the present invention was used. Comparative Example 6 containing the modified fine particle zinc oxide powder obtained in
However, the whiteness of the makeup film was strong and it was inferior as a product. That is, it is understood that Examples 1 and 2 are excellent in the UV protection effect in the UVA region, and that all of the items evaluated this time have excellent effects in a well-balanced manner.

[0046]

From the above, it is apparent that the present invention provides a powder cosmetic excellent in touch feeling and ultraviolet ray protection effect by using the modified fine particle zinc oxide type powder.

[Brief description of the drawings]

FIG. 1 is an electron microscope observation (20,000) of the modified fine particle zinc oxide based powder (Production Example 1) used in the present invention.
2) is a photograph showing the surface morphology.

Claims (1)

[Claims] 1. The average primary particle diameter is 0.001 to 0.1 μm.
It contains a modified fine particle zinc oxide powder obtained by coating a mixed powder consisting of fine particle zinc oxide in the range of m and a flaky powder having a whiteness in the range of 8 to 12 with an acylated amino acid. Powder cosmetics characterized by: