JPH0971417A - Flaky powder and cosmetic compounded therewith - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a high-quality flaky powder and cosmetic having high ultraviolet-shielding performance and high transparency to visible rays, free from non-homogeneity, giving excellent feeling in use and causing little elution of alkali. SOLUTION: This flaky powder is composed of a titanium oxide-coated metal oxide produced by coating the surface of flaky powder of a metal oxide having an average thickness of 0.1-1μm and an aspect ratio of 5-150 and composed mainly of amorphous silica with a titanium oxide layer having a thickness of 5-400nm.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a flake-like powder having a high ultraviolet ray-shielding ability, a high transparency to visible light, no unevenness, an excellent feeling in use, and almost no alkali elution, and a mixture thereof Regarding cosmetics

[0002]

2. Description of the Related Art Titanium oxide contained in cosmetics includes pigment-grade titanium oxide having a large primary particle size (200 to 300 nm) and fine particle titanium oxide having a small primary particle size (10 to 50 nm). The former has a large hiding power, and when applied to the skin, it becomes a so-called thick makeup state and gives an unnatural finish, and since the adhesion to the skin is large, the smooth feel and spreadability (spreading) are insufficient. Tended to be.

The latter has a problem that it is difficult to uniformly disperse it in the medium, and even if it is once dispersed, it agglomerates over time, causing lumps and unevenness. In particular, when a large amount of cosmetics is blended, the above problems become remarkable, and further, since the adhesive force to the skin is large, there is a problem that the smooth feel and the extensibility (spreading) are insufficient.

In order to solve the above problems, the average particle size of 0.
5-20 μm on the surface of mica of 5-100 μm
An ultraviolet-shielding pigment has been proposed which is coated with fine particle titanium dioxide in a coating amount of wt% and a coating thickness that does not substantially exhibit a pearlescent feeling, a bright feeling and a hiding power (Japanese Patent Publication No. 5-87545). When this UV-shielding pigment is used as a cosmetic, it gives a smooth and smooth feel and spreadability (spreading), but the transparency is insufficient, it may be colored, and the thickness can be made uniform. There is a cost, it has a cleavage property, but the cleavage may not occur completely on the surface and the thickness may change stepwise in one piece of mica,
There was a new problem in that alkali might be eluted from the mica and adversely affect the skin.

On the other hand, the inventors of the present invention applied a solution containing an organometallic compound onto a substrate, preferably a substrate having a smooth surface, dried and peeled from the substrate, and then heat-treated. A characteristic glass flake and a method for producing the same are proposed. (For example, JP-A-3-285838 and JP-A-4-37622). The various glass flakes produced according to this method have excellent surface smoothness, a uniform thickness, smooth sliding and good spreadability. Further, a pearlescent pigment in which the surface of these flaky glass is coated with titania or zirconia or a mixture thereof has been proposed.
(JP-A-6-116507). Since the base material of this pigment is synthetic glass containing 80% or more of silica, it has high transparency, is colorless, has a uniform thickness, and has high surface smoothness.
Highly safe without alkali elution. However, depending on the thickness and aspect ratio of the base material, there is a problem in that there is no smooth feel and the spread is poor.

[0006]

In view of the above-mentioned prior art, the present invention has a high ultraviolet-shielding ability which has never been produced before, has high transparency to visible light, and is used without any unevenness. The present invention provides a flaky powder having excellent feeling and almost no alkali elution, and a high-quality cosmetic material containing the same.

[0007]

[Means for Solving the Problem] In order to solve this problem,
The present inventors have studied the flake-shaped metal oxide coated with a titanium oxide layer on the thickness and particle size of the flake-shaped metal oxide as a base material, and the feeling of use as a cosmetic. As a result, the flake metal oxide has a thickness of 0.1 μm or more and 1 μm or less and an aspect ratio of 5 to 5.
When it was 150, it was found that when used as a cosmetic, there was no unevenness and a smooth feel and spreadability (spreading) were obtained, and the present invention was reached.

That is, the present invention has an average thickness of 0.1 to 1.
On the surface of the metal oxide flake powder mainly composed of amorphous silica having an aspect ratio of 5 to 100,
A titanium oxide-coated metal oxide flake powder coated with a titanium oxide layer having a thickness of 400 nm, and a cosmetic containing the powder.

The metal oxide flake powder used in the present invention can be prepared by the method already proposed by the present inventors (for example,
It can be prepared from a liquid containing a hydrolyzable / polycondensable organometallic compound according to JP-A-3-285838 and JP-A-4-37622).

That is, a liquid containing an organometallic compound capable of being hydrolyzed and polycondensed is applied onto a substrate, preferably a substrate having a smooth surface, and dried to remove the gel film from the substrate. Then, the flaky metal oxide is produced by sintering.

As the organic metal compound capable of being hydrolyzed and polycondensed as a raw material used in the present invention, a metal alkoxide having an alkoxyl group is preferable. Specifically, methoxides such as silicon, titanium, aluminum and zirconium, ethoxides, propoxides, butoxides and the like are used alone or as a mixture. The composition of the obtained flake powder is 70-100% by weight of at least 70% by weight of amorphous silica, alumina, titania,
0-30 in total of at least one selected from zirconia
It is a metal oxide consisting of wt% and has a softening point (temperature at which the viscosity coefficient is 4.5 × 10 at the 7th power POISE) of 1100 ° C. or higher, so it withstands the temperature at which titanium oxide is coated and heat treated. be able to.

In the present invention, the metal oxide flake powder has an average thickness of 0.1 to 1 μm and an aspect ratio of 5 to 150. A titanium oxide coating of flake-shaped metal oxide satisfying this condition has no unevenness, smooth feel and spreadability (spreading) when used as a cosmetic. Preferably, the average thickness is 0.3 to 0.9 μm,
Aspect ratio 10 to 100, average particle size 5 to 90 μm
The titanium oxide-coated metal oxide flake powder has better smooth feel and spreadability (spreading). More preferably, the average thickness is 0.4 to 0.8 μm, the aspect ratio is 20 to 80, the average particle size is 15 to 50 μm, and the titanium oxide-coated metal oxide flake powder has a smooth feel and spreadability ( Nobi) is very good.

As a method for coating the metal oxide flaky powder with titanium oxide, a known method is used. For example, a method of hydrolyzing sulfuric acid-titanium oxysulfate at a boiling temperature (for example, JP-B-43-25644) and a hydrolysis method of titanium tetrachloride (for example, JP-B-49-3824) are generally known.

After coating the titanium oxide precursor by these methods, it is heat-treated at 700 to 1000 ° C. to form a stable and high-density titanium oxide coating layer.

The coating thickness of the titanium oxide layer in the present invention is 5 to 400 nm. When the thickness is less than 5 nm, a sufficient ultraviolet ray shielding effect is not recognized, which is not preferable. On the other hand, even if the thickness is more than 400 nm, the physical properties such as the ultraviolet shielding effect and the interference color do not particularly change, and the titanium oxide is wasted. Preferably, the titanium oxide layer has a thickness of 2
It is 0 to 160 nm.

When the thickness of the titanium oxide layer is smaller than 40 nm, the titanium oxide-coated metal oxide flake powder is
It is a highly transparent white color. Titanium oxide layer thickness is 40-6
When the thickness is 0 nm, the titanium oxide-coated flake metal oxide becomes highly transparent silvery color, and when the thickness of the titanium oxide layer is sequentially increased to 160 nm, coloring having yellow, red, magenta, blue, and green transparency ( Interference color) is recognized. When the thickness of the titanium oxide layer is further increased, it becomes golden, red,
The same colors of magenta, blue and green are recognized. Therefore, 1
When the thickness of the titanium oxide layer is up to 60 nm, a transparent coloring is generally observed.

These colors are slightly different from those of commercially available titanium oxide-coated mica, and a more transparent feeling is recognized. The reason is that the metal oxide flake powder as the base material has high transparency, has high surface smoothness, and is amorphous (glass). To be

[0018] These transparency and coloring can enhance the designability when used as a cosmetic, and are preferably used.

The cosmetic containing the titanium oxide-coated metal oxide flake powder of the present invention has a high transparency to visible light, is less likely to cause color unevenness, and is a stable product with good color development. Further, it has a high UV shielding efficiency, and a high UV shielding is possible with a small amount of compounding. Further, since the titanium oxide-coated metal oxide flake powder does not aggregate with each other and exhibits good slipperiness, the product has good extensibility (spreading) and excellent feel in use. Furthermore, since the amount of impurities in the metal oxide flake powder can be suppressed to a low level, there is almost no alkali elution as observed in mica, and the product is a high quality product that is safe for the skin.

In the cosmetics used in the present invention, in addition to the above-mentioned titanium oxide-coated metal oxide flake powder, pigments which are usually used may be used in combination, if necessary. For example, titanium oxide, zinc oxide, zirconium oxide, yellow iron oxide, black iron oxide, red iron oxide, ultramarine blue, dark blue, chromium oxide, inorganic pigments such as chromium hydroxide, mica titanium, pearlescent pigments such as bismuth oxychloride, tar. Pigments, natural pigments, powders of silica beads, plastic beads such as nylon and acrylic, talc, kaolin, mica, sericite, other mica, magnesium carbonate, calcium carbonate, aluminum silicate, magnesium silicate, clay, etc. It is illustrated.

The amount of the titanium oxide-coated metal oxide flake powder to be blended varies depending on the kind of the intended cosmetic, but is used in the range of 1 to 80% by weight based on the solid component such as pigment. The range of 2 to 50% by weight is particularly preferable. If the content is less than this, the ultraviolet ray shielding effect is not significantly exhibited, and there are drawbacks such as poor color development. Conversely, even if more metal oxide flake powder is added than the upper limit,
The ultraviolet ray shielding effect does not increase, other pigment components decrease, and it becomes difficult to adjust the color tone and improve the adhesion to the skin.

In order to improve the dispersibility of the titanium oxide-coated metal oxide flake-like powder used in the present invention in cosmetics and to improve the feel, a titanium oxide-coated metal oxide flake-like powder is prepared. There is no problem in modifying by applying a surface treatment. For example, methyl hydrogen polysiloxane, reactive alkyl polysiloxane, metal soap, hydrogenated lecithin, acyl amino acid, acylated collagen aluminum, magnesium, calcium,
When surface treatment is performed with a so-called hydrophobizing agent such as a metal salt selected from titanium, zinc, zirconium, and iron, the surface of the glass flake changes from hydrophilic to hydrophobic, so an oil agent added when preparing cosmetics. It will become a familiar cosmetic product with a good texture.

[0023]

BEST MODE FOR CARRYING OUT THE INVENTION Examples will be shown below. Example-1 Silicon tetramethoxide, ethanol, and water,
They were mixed at a volume ratio of 1: 2: 1 and stirred at 50 ° C. for 15 hours. On a stainless steel plate having a surface of 20 cm × 20 cm and a thickness of 1 mm, the above-prepared liquid was formed into a film by a dip coating method at a pulling rate of 30 cm / min, dried in an oven at 150 ° C. for 1 minute, and then removed from the stainless plate. The peeled silica gel film was collected with a nylon brush. Collect the collected flaky silica gel at 1000 ° C for 2
Heat treatment was performed for an hour to obtain flake-shaped silica glass.

When the flaky silica glass was observed with a scanning electron microscope, the surface was very smooth and the thickness was about 0.6 μm.

The above flaky silica glass was crushed by a jet mill and classified to have an average particle size of about 30 μm. At this time, the aspect ratio of the classified flake silica glass is about 5
0.

15 g of this classified flake silica glass was dispersed in 100 ml of water and kept at 80.degree. here,
100 g of an aqueous titanium oxysulfate solution corresponding to 4 g of titanium dioxide and 50 g of 50% sulfuric acid were slowly added. After heating and boiling this for about one and a half hours, the slurry is filtered,
It was washed with water to remove sulfuric acid, and dried at 120 ° C. for 2 hours.

The resulting titanium oxide precursor-coated flake silica glass was heat-treated at 1000 ° C. for 1 hour to obtain a highly transparent white powder (titanium oxide-coated flake silica glass). When observed with a scanning electron microscope, the thickness of the titania layer was about 25 nm. The thickness, average particle size, and aspect ratio of the titanium oxide-coated flake silica glass were about 0.6 μm, about 30 μm, and about 50, respectively, which were the same as those of the classified flake silica glass before coating with titanium oxide. It was

This titanium oxide-coated flake silica glass is dispersed in a vinyl resin (having a refractive index of about 1.5 after curing) in an amount of about 10% by weight, and a film having a thickness of about 0.15 mm is obtained by a spectrophotometer. The transmittance was measured with a wavelength of 6
Visible light transmittance of 00 to 800 nm is 8 over the entire area.
It was confirmed that it is 0% or more, and the ultraviolet ray transmittance at a wavelength of 300 to 350 nm is 0 to 5%, that it has high transparency to visible light and that it effectively blocks ultraviolet rays.

To 5 g of the above-mentioned flake silica glass coated with titanium oxide, 50 g of freshly boiled and cooled water was added, and after stirring well for 3 minutes, the pH of the filtered solution was measured and found to be 6.5, which is almost medium. It was confirmed to be sex.

Further, a small amount of the above-mentioned flake silica glass coated with titanium oxide was picked up by hand and a slippery feeling on the skin, spread and the like were examined by a sensory test, and it was found to be extremely smooth and excellent in spread.

Comparative Example-1 An unground flake silica glass (having a thickness of about 0.6 μm) produced by the method described in Example-1 was ground with a jet mill and classified to obtain an average particle size of about 2 μm. At this time, the flake silica glass has an aspect ratio of 3.3.

15 g of the classified flake silica glass was dispersed in 100 ml of water and kept at 80 ° C. here,
100 g of an aqueous titanium oxysulfate solution corresponding to 8 g of titanium dioxide and 50 g of 50% sulfuric acid were slowly added. After heating and boiling this for about one and a half hours, the slurry is filtered,
It was washed with water to remove sulfuric acid, and dried at 120 ° C. for 2 hours.

The obtained titanium oxide precursor-coated flake silica glass was heat-treated at 1000 ° C. for 1 hour to obtain a highly transparent white powder (titanium oxide-coated flake silica glass). When observed with a scanning electron microscope, the thickness of the titania layer was about 25 nm.

This titanium oxide-coated flake silica glass was dispersed in a vinyl resin (having a refractive index of about 1.5 after curing) in an amount of about 10% by weight, and a film having a thickness of about 0.15 mm was obtained by a spectrophotometer. The transmittance was measured with a wavelength of 6
Visible light transmittance of 00 to 800 nm is 5 over the entire area.
It was 0 to 70%, and the ultraviolet ray transmittance at a wavelength of 300 to 350 nm was 0 to 5%. It was confirmed that the transparency to visible light is not so high because the flakes are small, but the ultraviolet rays are effectively shielded.

50 g of freshly boiled and cooled water was added to 5 g of the above-mentioned flake silica glass coated with titanium oxide, and after stirring well for 3 minutes, the pH of the filtered solution was measured and found to be 6.5. It was confirmed to be sex.

Furthermore, when a small amount of the above-mentioned flake silica glass coated with titanium oxide was picked up by hand and a sensory test was conducted for slip on the skin, spread, etc., it was found that the slip was poor, the surface was rough, and the feeling was bad.

Example-2, Comparative Example-2 and Comparative Example-3 A powder foundation was prepared with the following composition.

Component-1 Blending amount (% by weight) -------------------------------------- Example-1 Flake of the present invention produced in 14.1 Talc 74.7 Titanium oxide (primary particle size 200 to 250 nm) 3.8 Fine particle titanium oxide (primary particle size 30 to 50 nm) 1.9 Magnesium stearate 2.9 Rouge 0 .5 Yellow iron oxide 0.8 Black iron oxide 0.1 Silk powder 0.5

Component-2 content (% by weight) ----------------------------------------- Squalane 0.5 Sorbitan sesquioleate 0.1

Component-3 Amount of compounding (% by weight) ------------------------------------- Perfume 0.1

Component-1 was mixed with a Henschel mixer
Stir for 5 minutes. Stirring and mixing were performed while dropping the components uniformly melted at 70 ° C. In addition, the ingredients −
After adding 3, the mixture was stirred and mixed for 1 minute and pulverized with an atomizer to obtain a product-1 (Example-2).

Comparative Example-1 instead of the titanium oxide-coated flake silica glass of the present invention (substrate thickness 0.6 μm, particle size 30 μm, aspect ratio 50) prepared in Example-1 in Component-1. The product-2 (Comparative Example-2) was prepared in exactly the same manner as described above, except that the titanium oxide-coated flake silica glass (thickness of substrate: 0.6 μm, particle size: 2 μm, aspect ratio: 3.3) prepared in 1. Got

Further, Product-3 was prepared in the same manner as described above except that the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1 was not added.
(Comparative example-3) was obtained.

0.24 g of each of product-1, product-2 and product-3 was sampled and evenly applied to 4 cm × 5 cm of the skin in the center of the back of the five test subjects, adjoining, and in Izu in August. After exposure to direct sunlight for 30 minutes to 3 hours between 11:00 am and 2:00 pm, the degree of sunburn was observed.

Table 1 shows the results.
The average value of the degree of sunburn of 5 subjects was judged by the following classification. 1; Almost no sunburn 2; Sunburn is known 3; Reddish sunburn 4; Quite red sunburn 5: Severe sunburn, skin peels later

[0046]

[Table 1] Table-1 =================================== Powder of the present invention Comparative powder Comparative Powder (Product-1) (Product-2) (Product-3) (Example-2) (Comparative Example-2) (Comparative Example-3) ------------- 30 minutes later 1 1 1 1 hour later 1 1 3 2 hours later 1 1 4 3 hours later 2 25 ===== =============================

After 30 minutes, almost no difference was visually observed, but after 1 hour, a remarkable difference was observed, and the powder containing the titanium oxide-coated flake silica glass of the present invention ( The sunburn of the skin to which the powder (Product-2, Comparative Example-2) containing the titanium oxide-coated flake silica glass prepared in Product-1, Example-2) and Comparative Example-1 was applied was the above-mentioned titanium oxide. Powder not containing coated flake silica glass (Product-3, Comparative Example-
It was significantly reduced as compared with the case of applying 3).

Table 2 shows the results of a sensory test evaluated by a five-step method of 1 to 5 points, in which 20 female panelists use the above three kinds of products for 10 days and the maximum point is 5. .

[0049]

[Table 2] Table-2 =================================== Powder of the present invention Comparative powder Comparative Powder (Product-1) (Product-2) (Product-3) (Example-2) (Comparative Example-2) (Comparative Example-3) ------------- -------------------------------- Nobite 4.8 1.5 1.8 With 4.5 3.0 3.0 3.8 Transparency 4.7 2.0 3 .4 Glossiness 4.6 2.0 2.6 Color sense 4.2 2.8 3.7 Performance sustainability 4.8 3.1 2.0 ============== ====================

As described above, it was confirmed that the cosmetic of the present invention has good spreadability (adhesiveness), good transparency and glossiness, excellent color development, and is resistant to fading.

Example-3 Silicon tetraethoxide, ethanol, and 0.1
Normal hydrochloric acid is mixed in a volume ratio of 10: 20: 1,
The mixture was stirred at 40 ° C for 2 hours. Next, titanium isopropoxide was added so as to be contained as 10% by weight as an oxide after sintering, and stirring was continued. In addition, 45 of this liquid
Volume% water was added and reacted at 40 ° C. for 20 hours to prepare a coating liquid.

On the stainless steel plate having a surface of 20 cm × 20 cm and a thickness of 1 mm, the coating solution prepared above was formed into a film by a dip coating method at a pulling rate of 45 cm / min and dried in an oven at 150 ° C. for 1 minute. Then, the silica gel film separated from the stainless steel plate was collected with a nylon brush. The collected flaky gel was heat-treated at 1000 ° C. for 2 hours to obtain flaky silica-titania glass.
As a result of the analysis, the content of titania was 9.8% by weight.

When the flaky silica-titania glass was observed with a scanning electron microscope, the surface was very smooth and the thickness was about 0.85 μm.

The above flaky silica-titania glass was crushed and classified by a ball mill to have an average particle size of about 80 μm. At this time, the aspect ratio of the classified flake silica-titania glass is about 94.

15 g of this classified flake silica-titania glass was dispersed in 100 ml of water and kept at 80.degree.
To this, 150 g of an aqueous titanium oxysulfate solution corresponding to 21 g of titanium dioxide and 50 g of 50% sulfuric acid were slowly added. This was heated and boiled for about 1 and a half hours, and then the slurry was filtered, washed with water to remove sulfuric acid, and dried at 120 ° C. for 2 hours.

The obtained titanium oxide precursor-coated flake silica-titania glass was heat-treated at 1000 ° C. for 1 hour to obtain a red powder having high transparency (titanium oxide-coated flake silica-titania glass). When observed with a scanning electron microscope, the thickness of the titania layer was about 90 nm.

This flake silica titania glass coated with titanium oxide was mixed with a vinyl resin (having a refractive index of about 1.
5) was dispersed in about 10% by weight, and the transmittance was measured with a spectrophotometer as a film having a thickness of about 0.15 mm. The visible light transmittance at a wavelength of 600 to 800 nm was 70 to 85% over the entire area. Yes and wavelength 300-350
It was confirmed that the ultraviolet ray transmittance of nm is 0 to 5%, the transparency to visible light is high, and the ultraviolet ray is effectively shielded.

50 g of freshly boiled and cooled water was added to 5 g of the above-mentioned flake silica titania glass coated with titanium oxide, and the mixture was stirred well for 3 minutes, and then the pH of the filtered solution was measured and found to be 6.4. It was confirmed to be neutral.

Furthermore, a small amount of the above-mentioned flake-form silica glass coated with titanium oxide was picked up by hand, and a sensory test was conducted to examine slippage, spread, etc. on the skin. As a result, it was found to be quite smooth and spread well.

Comparative Example-4 An unpulverized flaky silica-titania glass (thickness: about 0.85 μm) produced by the method described in Example-3 was pulverized and classified by a ball mill to have an average particle diameter of about 200 μm.
At this time, the flake silica glass has an aspect ratio of about 2
35.

This classified flaky silica-titania glass was coated with a titanium oxide layer having a thickness of about 90 nm by the same method as in Example-3. The transparency and ultraviolet shielding ability of this titanium oxide-coated flake silica-titania glass were almost the same as those of the titanium oxide-coated flake silica-titania glass described in Example-3.

Further, 50 g of freshly boiled and cooled water was added to 5 g of the above-mentioned flake silica-titania glass coated with titanium oxide.
After adding 3g and stirring well for 3 minutes, the pH of the filtered solution
Was measured and it was confirmed to be almost neutral.

However, when a small amount of the above-mentioned flake silica-titania glass coated with titanium oxide was picked up by hand and a sensory test was conducted for slip on the skin, spread, etc., a feeling of being caught on the skin was felt, and slipperiness was poor. It didn't feel very good.

Comparative Example-5 Using the liquid prepared by the method described in Example-3, the pulling rate of the stainless steel substrate was set to 60c which was higher than that in Example-3.
A flake silica-titania glass was produced by the method described in Example-3 at m / min. When the thickness was measured with a scanning electron microscope, it was about 1.5 μm.

The flaky silica-titania glass was crushed by a ball mill and classified to have an average particle size of about 80 μm. The aspect ratio of the classified flake silica-titania glass is about 53.

This classified flaky silica-titania glass was coated with a titanium oxide layer having a thickness of about 90 nm by the same method as in Example-3. The transparency and ultraviolet shielding ability of this titanium oxide-coated flake silica-titania glass were almost the same as those of the titanium oxide-coated flake silica-titania glass described in Example-3.

Further, to 5 g of the above-mentioned flake silica-titania glass coated with titanium oxide, 50 parts of newly boiled and cooled water was added.
After adding 3g and stirring well for 3 minutes, the pH of the filtered solution
Was measured and it was confirmed to be almost neutral.

However, when a small amount of the above-mentioned flake silica-titania glass coated with titanium oxide was picked up by hand and a sensory test was conducted for slip on the skin, spread, etc., it felt rugged, spreads poorly, and feels too much. Was not good.

Example-4, Comparative Example-6 and Comparative Example-7 A powder foundation was prepared by the following procedure.

Instead of the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1 in Example-2, the titanium oxide-coated flake silica titania glass prepared in Example-3 is used. (Substrate thickness 0.
A product-4 (Example-4) was obtained in exactly the same manner as in Example-2 except that 85 μm, a particle size of 80 μm and an aspect ratio of 94) were added.

Further, instead of the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1, the titanium oxide-coated flake silica titania glass prepared in Comparative Example-4 (of the substrate) Thickness 0.85 μm, particle size 200 μm, aspect ratio 235)
Product-5 (Comparative Example-6) was obtained in exactly the same manner as in Example-2.

Further, instead of the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1, the titanium oxide-coated flake silica titania glass prepared in Comparative Example-5 (of the substrate) Product-6 (Comparative Example-7) was obtained in exactly the same manner as in Example-2, except that the thickness was 1.5 μm, the particle size was 80 μm, and the aspect ratio was 53).

Table 3 shows the results of a sensory test evaluated by a 5-step method of 1 to 5 points, in which 20 female panelists use the above three kinds of products for 10 days and the maximum score is 5. .

[0074]

[Table 3] Table 3 =================================== Powder of the present invention Comparative powder Comparative Powder (Product-4) (Product-5) (Product-6) (Example-4) (Comparative Example-6) (Comparative Example-7) ---------- -------------------------------- Nobite 4.6 3.2 2.8 With 4.5 2.8 3.8 Transparency 4.7 4.7 4.24 2.2 Glossiness 4.6 4.0 3.8 Color perception 4.1 3.8 3.7 Performance sustainability 4.7 4.0 4.0 4.0 ============== ====================

As described above, it was confirmed that the cosmetic of the present invention has good spreadability (adhesion), good transparency and glossiness, excellent color development, and is resistant to fading.

Example-5 15 g of flake silica glass (thickness 0.6 μm, particle size 30 μm, aspect ratio 50) produced, pulverized and classified by the method described in Example-1 was dispersed in 100 ml of water, and 8
It was kept at 0 ° C. Here, 100 g of titanium oxysulfate aqueous solution corresponding to 11 g of titanium dioxide and 50% of 50%
Sulfuric acid was added slowly. After boiling it for about one and a half hours, the slurry is filtered and washed with water to remove sulfuric acid,
It was dried at 120 ° C. for 2 hours.

The obtained titanium oxide precursor-coated flake silica glass was heat-treated at 1000 ° C. for 1 hour to obtain a yellow powder (titanium oxide-coated flake silica glass) having high transparency. When observed with a scanning electron microscope, the thickness of the titania layer was about 65 nm.

This titanium oxide-coated flake silica glass was dispersed in a vinyl resin (having a refractive index after curing of about 1.5) by about 10% by weight to obtain a film having a thickness of about 0.15 mm and a spectrophotometer. The transmittance was measured with a wavelength of 6
The visible light transmittance of 00 to 800 nm is 7 over the entire area.
It was confirmed that the transmittance was 5 to 90%, and the ultraviolet transmittance at a wavelength of 300 to 350 nm was 0 to 5%, the transparency to visible light was high, and the ultraviolet rays were effectively shielded.

50 g of freshly boiled and cooled water was added to 5 g of the above-mentioned flake silica-titania glass coated with titanium oxide, and the mixture was stirred well for 3 minutes, and the pH of the filtered solution was measured and found to be 6.2. It was confirmed to be neutral.

Further, a small amount of the above-mentioned flake-shaped silica glass coated with titanium oxide was picked up by hand, and a sensory test was conducted to examine the slip on the skin, the spread, etc., and it was found that it was very smooth and spreads well.

Comparative Example-8 In Example-5, instead of flake silica glass (thickness 0.6 μm, particle size 30 μm, aspect ratio 50), crushed and classified muscovite (thickness 0.6 μm, particle size 3)
Titanium oxide having a thickness of 65 nm was coated by the same method except that 0 μm and an aspect ratio of 50) were used. The obtained titanium oxide-coated muscovite was glossy yellow, but the transparency was not very noticeable.

About 10% by weight of this titanium oxide-coated muscovite was dispersed in a vinyl resin (having a refractive index after curing of about 1.5), and a film having a thickness of about 0.15 mm was transmitted through a spectrophotometer. When the rate was measured, the wavelength was 600 to 800 nm
Has a visible light transmittance of 45 to 65% over the entire area, and has an ultraviolet transmittance of 0 to 0 at a wavelength of 300 to 350 nm.
5%. It was confirmed that although it effectively shields ultraviolet rays, its transparency to visible light is not so good.

50 g of freshly boiled and cooled water was added to 5 g of the above titanium oxide-coated muscovite, and after stirring well for 3 minutes, the pH of the filtered solution was measured and found to be 8.5, indicating that it was alkaline. I understood. It can be said that this is because the alkali content was eluted from the muscovite.

Further, a small amount of the above-mentioned titanium oxide-coated muscovite was picked up by hand, and a sensory test was conducted to examine slipping on the skin, spread and the like. It was slightly inferior to the titanium oxide-coated flake silica glass produced in Example-5.

Example-6 and Comparative Example-9 A powder foundation was prepared by the following procedure.

In place of the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1 in Example-2, the titanium oxide-coated flake silica glass prepared in Example-5 ( Substrate thickness 0.6 μm,
With the exception of adding a particle size of 30 μm and an aspect ratio of 50),
Product-7 (Example-6) was obtained in exactly the same manner as in Example-2.

Further, in place of the titanium oxide-coated flake silica glass of the present invention prepared in Example-1 in Component-1, the titanium oxide-coated muscovite prepared in Comparative Example-8 (base material thickness 0. 6 μm, grain size 30 μm, aspect ratio 5
Product-8 (Comparative Example-9) was obtained in exactly the same manner as in Example-2, except that 0) was added.

Table 4 shows the results of the sensory test evaluated by a 5-step method of 1 to 5 points, in which 20 female panelists used the above two kinds of products for 10 days and the maximum score was 5. .

[0089]

[Table 4] Table-4 =============================== Powder of the present invention Comparative powder (Product-7) (Product-8) (Example-6) (Comparative Example-9) ------------------ Nobito 4.8 3.8 Addition 4.6 4.5 Transparency 4.5 3.0 Gloss 4.6 4.8 Color 4.1 4.1 3.5 Performance sustainability 4.6 4.0 ======= ======================

As described above, it was confirmed that the cosmetic of the present invention spreads better, has a good transparency, and is excellent in color feeling, as compared with the conventional cosmetics having a base material of muscovite. .

[0091]

The above detailed description and embodiments of the present invention,
As is clear in Comparative Examples, according to the present invention, a flaky powder having a high ultraviolet ray shielding ability, high transparency to visible light, no unevenness, excellent feeling in use, and almost no alkali elution and High-quality cosmetics containing it can be obtained.

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[Procedure amendment]

[Submission date] September 25, 1995

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] Claim 1

[Correction method] Change

[Correction contents]

[Procedure amendment 2]

[Document name to be amended] Statement

[Correction target item name] 0008

[Correction method] Change

[Correction contents]

That is, the present invention has an average thickness of 0.1 to 1.
In [mu] m, the metal oxide flake powder surface aspect ratio as the main component an amorphous silica which is a 5 to 5 0, 5
A titanium oxide-coated metal oxide flake powder coated with a titanium oxide layer having a thickness of 400 nm, and a cosmetic containing the powder.

Claims (3)

[Claims] 1. Oxidation with a thickness of 5 to 400 nm on the surface of a metal oxide flake powder mainly composed of amorphous silica having an average thickness of 0.1 to 1 μm and an aspect ratio of 5 to 100. Titanium oxide-coated metal oxide flake powder coated with a titanium layer. 2. The metal oxide flake powder is at least 70 wt% amorphous silica 70-100 wt%,
The titanium oxide-coated metal oxide flake powder according to claim 1, comprising a total of 0 to 30% by weight of at least one selected from titania, zirconia, and alumina. 3. A cosmetic comprising the titanium oxide-coated metal oxide flake powder according to any one of claims 1 and 2.