JPH04154715A - Metal oxide treated lamellar porous powder, its production and cosmetic using the same powder - Google Patents

Abstract

PURPOSE:To obtain a cosmetic having excellent smoothness, adhesivity and excellent ultraviolet ray preventing action, comprising porous powder prepared by sintering diatomaceous earth, plate crystalline kaolin and feldspar to give lamellar porous powder and treating the lamellar porous powder with aluminum oxide and titanium dioxide. CONSTITUTION:Diatomaceous earth, plate crystalline kaolin and feldspar are sintered to give lamellar porous powder, which is dispersed into water. The dispersion is mixed with a water-soluble salt of Al and neutralized so that 1-70wt.% hydrate aluminum oxide (base on untreated powder) calculated as Al2O3 is deposited on the surface of the lamellar porous powder. The lamellar porous powder is burnt at 300-900 deg.C. Then the burnt material is dispersed into water, similarly treated by using Ti to produce the title lamellar porous powder whose surface is treated with Al2O3 and TiO2. Further, 1-70% (preferably 5-30%) of the treated powder is added to a cosmetic base having excellent smoothness, adhesivity, air passability and excellent ultraviolet ray-preventing effects.

Description

Detailed Description of the Invention Industrial Fields of Application The present invention provides a plate-like porous powder surface-treated with aluminum oxide and titanium dioxide, a method for producing the same, and a method for improving smoothness and adhesion obtained by blending a two-tone powder. The present invention relates to a 1-piece T+ that has excellent air permeability and excellent UV protection effects.

``'Prior art'' Conventionally, cosmetics containing powder, such as makeup cosmetics such as Fanchi John, have been made with water absorbency and oil absorption in order to improve the makeup's longevity and feel. In addition, as the harmful effects of ultraviolet rays on the skin have become clearer in recent years, powders coated with ultraviolet absorbers or titanium dioxide to provide ultraviolet protection are being used. Cosmetic products containing UV rays have also been developed.Such powders include plate-shaped powders of mica, talc, etc. coated with titanium dioxide or coated with ultraviolet absorbers. However, when these powders are used in cosmetics, they have a UV protection effect,
Although it had smoothness and adhesion, it had poor air permeability.

Is there a known plate-like porous powder made by sintering a dispersed mixture of diatoms, plate-shaped crystalline cacaolin, and feldspar in Japanese Patent Application Laid-Open No. 63-239176? When coated, it has excellent smoothness and adhesion, similar to the plate-like material of ponds. Furthermore, since this powder is porous, it also has the advantage of being breathable.

Therefore, when this plate-shaped porous powder is used as a decorative crystal material, it has the advantages of being smooth, adhesive, and breathable, but it cannot be expected to have any UV protection effects. .

<Invention or Problem to be Solved> As mentioned above, a functional powder that has UV protection, smoothness, adhesion, and air permeability is ideal, but so far such powder has not been developed. There wasn't. Therefore, there were no cosmetics containing such functional powders9.In other words, the object of the present invention is to create an ideal functional powder that has both ultraviolet ray protection, smoothness, adhesion, and air permeability. There are two companies that manufacture cosmetics and provide cosmetics using them.

<Means for Solving the Problems> In order to obtain the ideal powder as described above, we have added an ultraviolet ray prevention effect to the plate-shaped porous powder disclosed in JP-A-63-239] No. 76. Try to give it.

When a plate-shaped porous powder is treated with an ultraviolet absorber, the ultraviolet absorber is adsorbed on the powder surface, and the ultraviolet absorber comes into direct contact with the skin surface, which is unfavorable from a safety standpoint. Therefore, we considered treating the above powder with titanium dioxide to give it an ultraviolet scattering effect.

At that time, by sequentially treating the surface with specific amounts of aluminum oxide and titanium dioxide, it was possible to cleanly cover the surface of the powder without the titanium dioxide particles blocking the pores of the plate-shaped porous powder. By blending this powder into cosmetics, it is possible to impart both smoothness, adhesion and breathability, as well as UV protection.

[Operation] That is, one of the present invention is a plate-shaped porous powder disclosed in JP-A-61239176, that is, a sintered body obtained by sintering a dispersed mixture of diatomaceous earth, plate-shaped crystal kaolin, and feldspar. is a metal oxide-treated plate-shaped porous powder coated with aluminum oxide and titanium dioxide.

More specifically, in the first layer of the plate-shaped porous powder disclosed in JP-A-63-239176, 1 to 70% by weight of aluminum as ^1203 is added to the untreated plate-shaped porous powder. After treatment with a hydrated oxide, it is fired, and then the second layer is applied to the untreated plate-shaped porous powder in an amount of 1 to 70 times TiO2!
% titanium hydrated oxide and then calcined, it is a metal oxide-treated plate-shaped porous powder that has an ultraviolet protection effect, smoothness, adhesion, and air permeability.

We first applied metal oxides, such as titanium dioxide, to the plate-shaped porous powder disclosed in JP-A No. 63-239176.
By coating with acid (hyaluminum, silicon oxide, etc.),
We considered how to impart an ultraviolet protection effect without sacrificing the inherent smoothness, adhesion, and breathability. As a result, they discovered that coating with acid f-hyaluminum and titanium dioxide was extremely effective in preventing ultraviolet rays.

Furthermore, the smoothness and adhesion properties of the porous powder which is the base material are improved, and surprisingly, the string pores of this powder are even though they are coated with oxide. It was found that these coatings, namely aluminum oxide and titanium dioxide, were not occluded.

Furthermore, when coating with either aluminum oxide or titanium dioxide was attempted, the surface of the powder could not be densely coated with titanium dioxide alone, and the smoothness and adhesion were poor. Furthermore, coating with only aluminum oxide had no effect of preventing ultraviolet rays. In this way, by coating with either aluminum oxide or titanium dioxide, it is not possible to obtain a plate-like polyurethane powder that has the ultraviolet ray prevention effect as well as smoothness, adhesion, and air permeability, which are the objects of the present invention. 1-Δ1,0. and TiO: and 1-
1 to 70 heavy benefits each! By coating the powder with an acid (hyaluminum and titanium dioxide), a metal oxide plate-like porous powder having ultraviolet protection, smoothness, adhesion, and air permeability was obtained for the first time.

Another aspect of the present invention is a method for producing a plate-like porous powder treated with a metal acid. The plate-shaped porous powder disclosed in JP-A No. 63-239176 was suspended in water for 50 to 300 y,/
Adjust the concentration to /. Next, an aqueous solution of a water-soluble aluminum salt such as aluminum sulfate or sodium aluminate is added while stirring to obtain a desired coating amount. After that, it is heated and a base such as ammonia water, caustic soda solution or sulfuric acid,
Neutralize with acid such as hydrochloric acid. Depending on the case, urea may be added and heated to be hydrolyzed, thereby allowing it to be used as a substitute for the above base. Thereafter, after filtering, washing and drying, the plate-shaped porous powder is coated with aluminum oxide by firing at 300 to 900° C. for 30 minutes. Subsequently, the fired product was suspended in water to a concentration of 50 to 300 g7'l, and titanyl sulfate, titanyl sulfate, and
An aqueous solution of a water-soluble titanium salt such as titanium tetrachloride is added and stirred. After that, it is coated with a hydrated oxide of titanium by adding an acid such as sulfuric acid or hydrochloric acid to neutralize and hydrolyze it, or by heating it to coat it with a hydrated oxide of titanium, followed by filtration, washing,
The plate-shaped porous powder is coated with aluminum oxide and titanium dioxide by drying and firing at 300 to 900° C. for 30 minutes or more. The hydrated oxide treatment of titanium may be performed on the fired product after the hydrated oxide treatment of aluminum as described above, but after the treatment with the hydrated oxide of aluminum, the hydrated oxide of titanium 30 minutes for more than 30 minutes after treatment with
It may be fired at ~900°C. By carrying out the treatment as described above, the surface of the plate-like porous powder can be densely coated with aluminum oxide and titanium dioxide without blocking the pores of the plate-shaped porous powder.

Furthermore, one aspect of the present invention is a cosmetic containing a plate-like porous powder whose surface is coated with hyaluminum acid and titanium dioxide. Similarly, it can be incorporated into various cosmetics. The appropriate amount is 1 to 70 weight 0°, particularly preferably 5 to 30 weight, 1E06.

Cosmetics come in the form of milky lotions, lotions, creams,
Examples include various forms of general cosmetics such as ointments, sticks, powders, and pressed products.

In addition, it can be used for a variety of purposes such as skin care, makeup, hair, body, and fragrance, but it is most suitable for makeup cosmetics such as foundation, cheek color, eye color, lipstick, and nail enamel. It is.

<Effects> Furthermore, the effects of the present invention will be explained in detail with reference to Examples.

, Example 1 The average particle size was 3,3) in 1.5 iJ of purified powder; plate shape; Pouring: 187.5 g of powder was added and dispersed at 92 k at room temperature without stirring. Add and dissolve 552 g of aluminum acid and 34 g of urea, boil in about 30 minutes at
02te-). After stirring to maintain the boiling point for another 4 hours, filter and purify using the usual method, and add the resulting cake to purified water)
5p, h-sanji, hydroxy acid (hinato 1p, 7m water) pH
After adjusting the temperature to 7.0, it is filtered and washed. The resulting cake is dried at 105°C for 24 hours and further baked at 800°C for 2 hours.

Next, 140 g of the above baked product was dispersed in 934xl of purified water, and 456g, 1 of a titanyl sulfate aqueous solution was added and mixed in 66M1 at room temperature. After that, it is heated to reach the boiling point (102°C) in about 30 minutes, and after maintaining the boiling point for an additional 3 hours, it is filtered and washed by a conventional method - The resulting cake is dispersed in purified water 11 and hydroxylated. After adjusting the pH to 70 using 7 volumes of water, filter and wash. The resulting cake was dried at 105°C for 24 hours and further dried at 800°C.
Bake for 2 hours. The aluminum oxide and titanium dioxide in the obtained resin are respectively ^l+o,
, Tie: as 1.05 and 964 weight 1. Tej
)sand.

] Example 2 Purified Water 178 g of plate-shaped porous powder with an average particle size of 3.3) and tβ was added and dispersed in 5Q with stirring. 783 g of aluminum sulfate and 4892 g of urea were added and dissolved therein at room temperature, and heated to reach the boiling point (102° C.) in about 30 minutes. After maintaining the boiling point for an additional 4 hours, filter and wash using a conventional method. Disperse the resulting cake in purified water and hydroxide. Adjust the pH to 70 with a helium aqueous solution, then filter and wash. . The resulting cake is dried at 105° C. for 24 hours and further baked at 800″C for 2 hours.

Next, the fired product 1302 is dispersed in purified water 93411, and 142 zff of a 456 g/l titanyl sulfate aqueous solution is added and mixed at room temperature. After that, heat it for about 30 minutes
After reaching the boiling point (102°C) in minutes and maintaining the boiling point for an additional 3 hours, it is filtered and washed in a conventional manner.

The resulting cake was dispersed in purified +1p and hydrated with hydroxyl (chicken
After adjusting IIH to 70 with an aqueous solution of aluminum, filter and wash the resulting cake. Dry at +05°C for 24 hours.
．． It is further baked at soo'c for 2 hours. The aluminum oxide and titanium dioxide contents in the obtained fired product are respectively ^
913 and 1985 NOo as l, 03, TiO□
There was.

When the powders according to Example] and Example 2 were observed using a scanning electron microscope, it was found that the pores of the plate-shaped porous powder used as the raw material were not blocked and the surface was densely coated. Ta.

In addition, in the above, it is possible to change the thickness of the titanium dioxide film by adjusting the amount of aluminum sulfate and titanyl sulfate aqueous solution added, and as a result, the ultraviolet protection effect, breathability, etc. can be controlled. Can be rolled.

Next, examples of cosmetics prepared using the powders obtained in Example 1 and Example 2 above will be shown together with comparative examples.

"Example 3" Solid foundation Example 3 Comparative example 1 (weight 0 active) (1) Titanium oxide 10.0 10
．． 0(2) Sericite 15,0 3
0.0(3) Talc 23.3
33.3(4) Powder prepared in Example 1 250
-(5) Pen color 1.0
1.0(6) Yellow iron oxide 20 20
(7) Black iron oxide 03 03(8)
Liquid paraffin 15.0 15.0 (
9) Silicone oil 8.0 8.0 (
10) Methylparaben 0.2 0.2
Mix and grind (1) to (7) to make it homogeneous, and add (8) to this.
-(11) are added to mix and homogenize. Thereafter, this is filled into a metal plate and press-molded using a compression molding machine.

[6fUM4: Pour fantain yon example 4
Comparative Example 2 (Weight 0°) (1) Titanium oxide 12.0 12.
0(2) Sericite 14,1 32
．． Powder prepared in 1(3) Example] 18.0 −
(4) Hengara 11 ]1
(5) Yellow iron oxide 21 2] (6)
Black iron oxide 0.3 0.3(7)
Liquid paraffin 30.0 30.0 (8
) Vaseline 10.0 10.0
(9) Silicone oil 50 50 (10
) Microcrystallinwa, 2s
70 70(11) Methylparaben
0.2 0.2〈12) Incense 1”l
O, 20, 2 (1) to (6) were mixed and pulverized to make it homogeneous, and this was mixed to a rough condition and heated and dissolved (7
) to (12), stirred and homogenized, and then poured into a predetermined container.

, Example 1 Milk (H-type fanchiejon Example 5 Comparative example 3 (heavy f!1-01) (1) Acid (hytitane 1,90 1
．． 90(2) Talc 1.12
6.12 (3) Powder prepared in Example 2 9.00
-(4) Hengara 0.15
0.15 (5) Yellow iron oxide 0.2
7 0.27 (6) Black iron oxide 0.
06 0.06(7) Kaolin 6
．． 00 10.00 (8) Ceresin
3.50 3.50 (9) Paraffin wax
1.50 1.50 (10) Liquid lanolin
1,50 1.50 (11) Liquid paraffin 13.50 13.50 (12) Polyoquinoethylene (20) Tsuru E-tan 1,
00 1.00 Mopareate (13) Crane [Tanmopareate]
1,00 1.00 (14) mo/2 thea'J>acidg'++'l>
0.70 0.70 (15) Purified water
55.20 55.20 (16) Karuiki 7I Chiru Shichiru Kanosu 0.40 0
．． 40(17) Prorange Recall
3,00 3.00 (18)
Methylparaben 0.10 0.10 (1
9) Incense flo, +o o, 1° (1) to (7) were mixed and pulverized to homogenize, and this was mixed and heated (
Add to 12) to (17) and homogenize with a homomixer. After that, this was mixed and heated in advance to make it homogeneous (8
)~ri] 1) is gradually added and emulsified using a homomixer. Then, (18) and (19) are added.

The above examples and comparative examples were subjected to sensory evaluation to examine their gas permeability and UV protection effect.

Sensory evaluation was conducted using 30 female panelists aged 20 to 30 as test subjects, and evaluated the "spreadiness", "adherence", and [
Makeup durability was evaluated using a five-point evaluation method. The results are shown in Table 1.

Table 1 Sensory evaluation results 1g) 4.7. '3.24. :j 24.4.9
:3.21 Adhesion l 4.81 3,01 4.9
1 3,51 4,712.71.1 All of the examples were highly rated compared to the comparative examples in terms of elasticity, adhesion, and long-lasting makeup, demonstrating that they were excellent in smoothness and adhesion. Ta.

The scum permeability was tested by the side-by-side method.

Apply the reagent to a certain area (16 cm') of the human forearm,
After fitting the gas collector tightly and purging the inside with nitrogen gas, the pressure was set to 055 Kg/Cff12 and left as it was for 2 hours. Thereafter, the collected gas was analyzed by gas chromatography to measure the carbon dioxide concentration. The gas permeability of Examples and Comparative Examples was determined by setting the carbon dioxide concentration of the uncoated portion of the sample to 100%. The results are shown in Table 2 as an average value of n·10 for each sample.

Table ヱ Gas permeability test result Song test fl Gas permeability book (0,, □l) Example 399
3 Comparative Example 1 865 Example = 41 79.6 Comparative Example 21 68.7 □ Example 5908 □ Comparative Example 3' 824 ' Each example shows higher scum permeability than the comparative example and has excellent air permeability. was shown.

Next, regarding the ultraviolet ray prevention effect, a test was conducted under rJ.

402 g of sample V was heated and dissolved in 9.8 g of vaseline, and dispersed using a Miki roller. This was sandwiched between quartz plates using a 55μ spacer, held down with crimps at both ends, and the absorbance was measured at 200 to 400 nm using a spectrophotometer with an integrating sphere.The measured absorbance was integrated, and this integrated value was calculated as follows. The ultraviolet protection rate was calculated by substituting it into the formula.

5-IB 14, Is test 11.7'1 absorbance accumulation value 1B pair! ! 3 (in the case of kwaseline only)
, o, I over the entire measurement wavelength range] 00 'o Absorbance integral value when absorbed - 200 Results are not shown in Table 3 7 Table 3 Ultraviolet protection effect In each example, Due to the scattering effect of the coated fine particle titanium dioxide, compared to the comparative example
\The high UV protection rate was set in the figure.

According to the present invention, like ν month 2 (the first makeup is conventional makeup 1)
Compared to No. 1, it clearly has superior smoothness, adhesion, and air permeability, and has a high ultraviolet protection effect.

Patent application) Noevir Co., Ltd.

Claims (4)

[Claims] (1) A plate-shaped porous powder formed by sintering diatomaceous earth, plate-shaped crystal kaolin, and feldspar, Al_2O_3 and TiO_2
A metal oxide-treated plate-like porous powder, characterized in that it has been treated with aluminum oxide and titanium dioxide in an amount of 1 to 70% by weight each (weight ratio to the untreated plate-like porous powder). (2) A. By dispersing the plate-shaped porous powder in water, adding a water-soluble salt of aluminum to the dispersion and neutralizing it, the surface of the plate-shaped porous powder is coated with 1 as Al_2O_3.
~70% by weight (weight ratio to untreated plate-like porous powder)
a step of depositing a hydrated oxide of aluminum and then firing at 300 to 900°C; (b) subsequently dispersing the fired product in water, adding an aqueous salt of titanium to the dispersion, and neutralizing or A step of depositing a hydrated oxide of titanium as TiO_2 in an amount of 1 to 70 weights (weight ratio to the untreated plate-like porous powder) on the surface of the fired product by heating and hydrolyzing it and firing it at 300 to 900°C. The method for producing a metal oxide-treated plate-like porous powder according to claim 1, comprising the following steps. (3) A cosmetic comprising the metal oxide-treated plate-like porous powder according to claim 1. (4) The amount of metal oxide-treated plate-shaped porous powder is 1 to 7.
The cosmetic composition according to claim 3, wherein the content is 0% by weight.