JPH03184905A - Cosmetic - Google Patents

Abstract

PURPOSE:To obtain cosmetic having excellent ultraviolet ray screening effects and transparent feeling by blending a cosmetic with fine grain titanium hydroxide powder produced by adding a specific hydrocarbon and/or a specific silicone to a titanium alkoxide in hydrolyzing the above alkoxide. CONSTITUTION:Fine-grain titanium hydroxide powder obtained by adding a hydrocarbon having 100-200 deg.C boiling point and/or silicone expressed by formula I (n is integer of 3-7) and formula II (n is integer of 1-4; R is methyl or phenyl) at a ratio of silicone of 5-500 pts.wt., preferably 10-300 pts.wt. based on 100 pts.wt. titanium alkoxide to a titanium alkoxide when a titanium alkoxide is hydrolyzed to provide titanium hydroxide is blended with a cosmetic to provide the aimed cosmetic having excellent ultraviolet ray screening effect, especially excellent screening effect in 280-320nm UV-B wavelength area harmful to skin and capable of giving transparent feeling reduced in pale color.

Description

DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention provides an ultraviolet shielding effect, particularly in the range of 280 to 320 nm.
The present invention relates to a cosmetic with excellent shielding effect and transparency in the UV-B wavelength region.

<Prior Art> Titanium oxide has excellent coloring power and hiding power, is structurally stable, and is a type of highly safe white pigment. Further, when the particle size is 1 μm or less, the particles have an effect that has not been seen before, such as an ultraviolet shielding effect, due to volume effects and surface effects.

For this reason, fine-particle titanium oxide is widely used in cosmetics and the like that require UV-shielding effects.<Problems to be Solved by the Invention> Problems with the Prior ArtHowever, the fine-particle titanium oxide that is commonly used is ■UV-B wavelength range (280-3
20 nm), the UV shielding effect is not sufficient. ■Since it lacks transparency, when applied to the skin, it produces a bluish-white tinge, resulting in an unnatural finish that is undesirable in terms of cosmetic effect.

OBJECTS OF THE INVENTION The object of the present invention is to provide a highly transparent cosmetic material that has a large ultraviolet shielding effect, particularly in the UV-B wavelength region.

As a result of intensive research to achieve the above object, the present inventors found that when fine particle titanium hydroxide obtained by a new manufacturing method is blended into cosmetics, it gives a transparent feeling with less paleness when applied to the skin. The present invention was completed based on the discovery that the present invention has excellent ultraviolet shielding effects in the UV-B wavelength region of 280 to 320 nm, which is considered harmful to the skin.

<Means for Solving the Problems> In other words, the present invention provides for the production of titanium hydroxide by hydrolyzing titanium alkoxide, which has a boiling point of 100 to 200.
℃ and/or the following general formulas (I) and (II) [(CH3)2 SiO].

(In the formula, n is an integer from 3 to 7)... (I) CR
3[R2S i O]. S i (CH3) 3 (in the formula, n is an integer of 1 to 4, R represents a methyl group or a phenyl group)... By adding silicone represented by (IT) The present invention relates to cosmetics characterized by containing a silicone represented by the following formula.

The present invention will be explained in detail below.

In order to obtain the novel particulate titanium hydroxide that is incorporated into the cosmetic composition of the present invention, titanium alkoxide that is commonly used in the production of titanium hydroxide can be used. For example, tetramethoxytitanium, tetraethoxytitanium, tetra-j
-propoxytitanium, tetra-n-propoxytitanium,
Examples include tetra-n-butoxytitanium, tetra-1-butoxytitanium, tetra-8ec-butoxytitanium, tetra-t-butoxytitanium, and tetra-octadecyloxytitanium.

The titanium hydroxide can be obtained by adding specific hydrocarbons and/or silicones before, during or after the hydrolysis.

The hydrocarbons used have boiling points in the range of 100 to 200°C, for example, hydrocarbons with boiling points in the range of 100 to 143°C (average carbon number: 8.6, molecular weight: 123), boiling points in the range of 157 to 177°C. (average carbon number: 10.5, molecular weight: 1.49), hydrocarbons with a boiling point of 171 to 193°C (average carbon number: 11..3, molecular weight: 160), etc. can give.

The silicone used has the following general formula (I) and (IT
) [(CH3)2 sio,].

(In the formula, n is an integer from 3 to 7)... (I) CH
3[R2S i O]□5i(CH3)3 (in the formula, n is an integer of 1 to 4, R represents a methyl group or a phenyl group)...
(n), such as hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, hexamethyldisiloxane, octamethyltrisiloxane, decamethyltetra Examples include siloxane, dodecamethylpentasoloxane, hexamethyldiphenyltrisiloxane, hexamethyltetraphenyltetrasiloxane, and hexamethylhexaphenylpentasiloxane.

Regarding the quantitative relationship between titanium alkoxide and hydrocarbon and/or silicone, titanium alkoxide 100
5 to 500 parts by weight of silicone (hereinafter referred to as part i)
parts, preferably 10 to 300 parts. The ratio of hydrocarbon to silicone can be arbitrarily selected within the above-mentioned range of parts by weight. That is, it can be arbitrarily selected depending on the properties of the intended powder.

The manufacturing method according to the present invention specifically takes the following aspects.

[Hydrolysis step]→[Concentration step]→[Drying step] This manufacturing method will be explained for each step.

[Hydrolysis step] is a step of hydrolyzing titanium alkoxide. This hydrolysis is carried out at room temperature (20 ± 10 °C
) or heating temperature (30 to 130°C).

In the usual method, a suspension of titanium hydroxide is obtained by hydrolyzing titanium alkoxide and water diluted with a solvent, and then refluxed for 0.5 to 24 hours or left as is without refluxing. When concentrated and dried, the particle size is 1 μm.
The powder becomes agglomerated before and after, and fine particle powder of submicron size or less cannot be obtained. Therefore, by adding hydrocarbons and/or silicones before, during, or after hydrolysis, it is possible to prevent particle condensation even during the subsequent concentration and drying steps. Can you get the powder?

Although there are still many unknowns about this effect, the surface tension and latent heat of vaporization of excess water during hydrolysis and the water generated by the hydrolysis reaction and the hydrocarbon and/or silicone,
It is thought that the effectiveness of the present invention is brought out by differences in boiling points, etc.

The "concentration process" is a process to remove excess water, hydrocarbons and/or silicone, and the solvent used for dilution from the suspension obtained in the hydrolysis process to increase the efficiency of the next drying process. be. Concentration methods include vacuum drying, suction filtration, pressure filtration, vibration drying, spray drying, and freeze drying, which are appropriately selected and used depending on the size of the lot to be produced and the type of hydrocarbon or silicone.

[Drying step] is a step of drying at a temperature range of 60 to 200° C. in order to completely remove water and solvent remaining in the [concentration step]. The drying temperature is appropriately selected depending on the solvent, hydrocarbon and/or silicone used in the production.

The powder thus obtained is pulverized by a known pulverization method.

The quantitative relationship between titanium alkoxide and water during hydrolysis can be selected from a very wide range, but it is usually 10 to 150 parts per 100 parts of titanium alkoxide.
Preferably it is 40 to 80 parts.

Titanium alkoxide and water during hydrolysis may be used as they are, but they are usually diluted with a solvent before use.

The diluting solvent used in the present invention is an alcohol such as methanol, ethanol, n-propanol, j-propanol, n-butanol, i-butynol, 5ec-butanol, t-butanol, etc. 8 .

[Manufacturing example]

An example of manufacturing fine particle titanium hydroxide by a new manufacturing method to be incorporated into the cosmetic of the present invention will be given below.

Add 100 parts of octamethylcyclotetrasiloxane to a solution of 100 parts of i-propoxy titanium diluted with 500 parts of i-propanol, and add 100 parts of octamethylcyclotetrasiloxane to a solution of 50 parts of water diluted with 500 parts of i-propanol while stirring. plus 25
Hydrolysis was carried out at °C. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 40 parts of stable fine powder. This powder exhibited hydrophobic properties.

33 parts of stable fine particle powder was obtained in the same manner as in Production Example 1 except that the amount of octamethylcyclotetrasiloxane added was 5 parts. This powder exhibited hydrophobic properties.

Production Example 3 The amount of octamethylcyclotetrasiloxane added was 500
40 parts of stable fine particle powder was obtained in the same manner as in Production Example I. This powder exhibited hydrophobic properties.

100 parts of type 114 soil tetramethoxy titanium and 50 parts of i-proper tool
100 parts of decamethylcyclopentasiloxane was added to the solution diluted with 0 parts, and while stirring, a solution prepared by diluting 50 parts of water with 500 parts of i-propatool was added to perform hydrolysis at 25°C. This suspension was concentrated using suction filtration and then dried at 150°C to obtain 40 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

Production target: 100 parts of tetraethoxy titanium to i-proper tool 50
100 parts of hexamethyldisiloxane in a solution diluted with 0 parts
50 parts of water with stirring.
A solution diluted with 0.00 parts was added and hydrolysis was carried out at 25°C. After concentrating this suspension using the f stage of suction filtration,
It was dried at 120°C to obtain 35 parts of stable fine powder. This powder exhibited hydrophobic properties.

100 parts of octamethyltrisiloxane is added to a solution of 100 parts of tetra-n-propoxytitanium diluted with 500 parts of i-propanol, and while stirring, a solution of 50 parts of water diluted with 500 parts of i-propanol is added. was added to perform hydrolysis at 25°C. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 37 parts of stable fine powder. This powder exhibited hydrophobic properties.

Add 100 parts of hexamethyltetraphenylpentasiloxane to a solution of 100 parts of utetra-n-butoxytitanium diluted with 500 parts of i-propatool, and add 5 parts of water while stirring.
A solution prepared by diluting 0 parts with 500 parts of i-propatool was added to perform hydrolysis at 25°C. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 40 parts of stable fine powder. This powder exhibited hydrophobic properties.

Production aim 1 50 parts of octamethylcyclotetrasiloxane and 5 parts of octamethyltrisiloxane are added to a solution of 100 parts of tetra-1-butoxytitanium diluted with 500 parts of i-propatool.
0 parts was added thereto, and while stirring, a solution prepared by diluting 50 parts of water with 500 parts of i-propatool was added to carry out hydrolysis at 25°C. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 37 parts of stable fine powder. This powder exhibited hydrophobic properties.

Production Example 9 50 parts of hexamethyldisiloxane and 50 parts of octamethyltrisiloxane were added to a solution of 100 parts of tetra-5ee-butoxytitanium diluted with 500 parts of i-propanol, and while stirring, 50 parts of water was added with i-propanol. 500
A diluted solution was added to carry out hydrolysis at 25°C.

After concentrating this suspension using means of suction filtration, 13
It was dried at 0°C to obtain 40 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

100 parts of octamethylcyclotetrasiloxane was added to a solution prepared by diluting 50 parts of IL Tosui with 500 parts of i-propatool, and the solution was mixed with 10 parts of tetra-1-proxytitanium.
A solution prepared by diluting 0 parts with 500 parts of i-propatool was added to perform hydrolysis at 25°C.

After concentrating this suspension using means of suction filtration, 13
It was dried at 0°C to obtain 40 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

A solution prepared by diluting 50 parts of water with 500 parts of i-propertool was added to a solution prepared by diluting 100 parts of tetra-i-propoxy titanium with 500 parts of i-propertool while stirring, and the mixture was prepared for 25 minutes.
Hydrolysis was carried out at °C. 100 parts of octamethylcyclotetrasiloxane was added to this suspension and stirred. After concentrating this suspension using means of suction filtration,
The mixture was dried to obtain 40 parts of stable fine particle powder. This powder exhibits hydrophobic properties and is prepared by adding 100 parts of octamethylcyclotetrasiloxane to a solution of 100 parts of tetra-t-butoxytitanium diluted with 500 parts of i-propatool, and adding 50 parts of water with stirring.
- Add a solution diluted with 500 parts of propatool and keep at 25°C.
Hydrolysis was carried out at 90° C., followed by refluxing at 90° C. for 10 hours.

After concentrating this suspension using means of suction filtration, 13
It was dried at 0°C to obtain 40 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

100 parts of octamethylcyclotetrasiloxane was added to a solution prepared by diluting 100 parts of 3J-Rotitraoctadecyloxytitanium with 500 parts of i-propatool and heated at 50°C. This solution was added with stirring to a solution prepared by diluting 50 parts of water with 500 parts of i-propatool, and hydrolysis was carried out at 50°C. After concentrating this suspension using means of suction filtration, 1
It was dried at 30°C to obtain 40 parts of stable fine powder.

This powder exhibited hydrophobic properties.

4 Regarding the powders and commercially available products obtained in Production Examples 1 to 13, the absorbance in the ultraviolet region (300 parts m) and the visible region (420,550 parts m)
The reflectance of part m) is shown in the table. The absorbance in the ultraviolet region is powder 1
% by weight was dispersed in castor oil, coated on a quartz plate to a thickness of 5 μm, and measured using a spectrophotometer. The reflectance in the visible region was measured by dispersing IO powder in castor oil and applying it to a thickness of 0.101 mm on a black hiding rate test paper, using a colorimeter.

(Results) As shown in the table, the cosmetics of this production example have a UV shielding effect,
Good results were shown in both transparency.

(Left below) 814 A solution prepared by diluting 100 parts of tetra-1-propoxy titanium with 500 parts of i-propatool has a boiling point of 116 to 143°C.
Add 100 parts of hydrocarbon and add 50 parts of water with stirring.
- Add a solution diluted with 500 parts of propatool and keep at 25°C.
Hydrolysis was performed with This filtrate was concentrated using suction filtration and then dried at 120°C to obtain 35 parts of stable fine particle powder.

Production Garden □ 34.5 parts of stable fine powder was obtained in the same manner as in Example 14 except that the amount of hydrocarbon having a boiling point of 116 to 143°C was 5 parts.

37 parts of stable fine powder was obtained in the same manner as in Example 14 except that the amount of hydrocarbon having a boiling point of 116 to 143° C. was 500 parts.

100 parts of Tetramethoxytitanium produced by Juku was added to 50 parts of i-Proper Tools.
100 parts of a hydrocarbon having a boiling point of 157 to 177° C. was added to the solution diluted with 0 parts, and while stirring, 50 parts of water and i-propatool were added to perform hydrolysis. This suspension was concentrated using suction filtration, dried at 130°C, and
5 parts of stable fine powder was obtained.

100 copies of Tetraethoxy Titanium, 50 copies of i-Proper Tools
100 parts of a hydrocarbon having a boiling point of 171-193° C. was added to the solution diluted with 0 parts, and while stirring, a solution of 50 parts of water diluted with 500 parts of i-propatool was added to perform hydrolysis. After concentrating this suspension using means of suction filtration,
It was dried at 140°C to obtain 35 parts of stable fine powder.

A solution prepared by diluting 100 parts of tetra-n-propoxy titanium with 500 parts of i-propatool has a boiling point of 116 to 143.
50 parts of hydrocarbon and 50 parts of octamethylcyclotetrasiloxane were added, and while stirring, a solution prepared by diluting 50 parts of water with 500 parts of i-propatool was added to carry out hydrolysis. After concentrating this suspension using means of suction filtration,
Drying at 130°C yielded 35 parts of 8 stable microparticle powder. This powder exhibited hydrophobic properties.

Production Example 20 A solution prepared by diluting 100 parts of tetra-n-butoxytitanium with 500 parts of j-propanol has a boiling point of 157 to 1770C.
50 parts of the hydrocarbon and 50 parts of decamethylcyclopentasiloxane were added, and while stirring, a solution prepared by diluting 50 parts of water with 500 parts of j-propatool was added to perform hydrolysis.

After concentrating this suspension using means of suction filtration, 1
It was dried at 30°C to obtain 35 parts of stable fine powder. This powder exhibited hydrophobic properties.

Production Example 21 A solution prepared by diluting 100 parts of tetra-1-butoxytitanium with 500 parts of i-propatool has a boiling point of 171 to 1930C.
Add 50 parts of hydrocarbon and 50 parts of hexamethyldisiloxane, and add 50 parts of water with stirring to 500 parts of i-propatool.
Hydrolysis was carried out by adding a solution diluted in 50%. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 35 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

] Production Example 22 A solution of 100 parts of tetra-5ec-butoxytitanium diluted with 500 parts of i-, propatool has a boiling point of 116 to 14
50 parts of hydrocarbon at 3°C and 5 parts of hydrocarbon at 157-177°C
Hydrolysis was carried out by adding a solution prepared by diluting 50 parts of water with 500 parts of i-propatool while stirring. After concentrating this suspension using means of suction filtration,
It was dried at ℃ to obtain 35 parts of stable fine powder.

Production Example 23 A solution of 100 parts of tetra-1-propoxy titanium diluted with 500 parts of i-propatool was added to a solution having a boiling point of 11.6 to 14.
50 parts of hydrocarbon at 3°C and 50 parts of hydrocarbon at 171-193°C were added, and while stirring, a solution prepared by diluting 50 parts of water with 500 parts of i-propatool was added to perform hydrolysis. After concentrating this suspension using means of suction filtration, 1
It was dried at 30°C to obtain 35 parts of stable fine powder.

100 parts of a hydrocarbon with a boiling point of 1.1.6 to 143°C is added to a solution prepared by diluting 50 parts of tatami water with 500 parts of i-propatool and stirred.
00 parts was added to a solution diluted with 500 parts of i-propatool, and hydrolysis was performed at 25°C. This suspension was concentrated using suction filtration and then dried at 130'C to obtain 35 parts of stable fine powder.

A solution prepared by diluting 50 parts of water with 500 parts of J-propertool was added to a solution prepared by diluting 100 parts of Tetra-1-propoxy titanium with 500 parts of i-Propertool while stirring, and the mixture was heated to 25%.
Hydrolysis was carried out at °C. This suspension has a boiling point of 171-1
．． 100 parts of hydrocarbon at 93°C was added and stirred. This suspension was concentrated using suction filtration and then dried at 130°C to obtain 35 parts of stable fine particle powder.

Add 100 parts of a hydrocarbon with a boiling point of 171 to 193°C to a solution prepared by diluting 100 parts of tetra-1-butoxy titanium with 500 parts of i-propatool, and add 50 parts of water while stirring.
A solution diluted with 500 parts of propatool was added to carry out hydrolysis at 25°C, followed by refluxing at 90°C for 10 hours. After concentrating this suspension using means of suction filtration,
It was dried at ℃ to obtain 35 parts of stable fine powder.

A solution prepared by diluting 1.00 parts of tetraoctadecyloxytitanium extracted from the cram school with 500 parts of i-propatool has a boiling point of 171 to 19.
100 parts of hydrocarbon at 3°C, 100 parts of octamethyltrisiloxane and 100 parts of hexamethyltetraphenyltetrasiloxane were added, and the mixture was heated to 50°C.

This solution was added to a solution prepared by diluting 50 parts of water with 500 parts of i-propertool while stirring, and hydrolysis was carried out at 50°C. After concentrating this suspension using means of suction filtration,
It was dried at 130°C to obtain 35 parts of stable fine particle powder. This powder exhibited hydrophobic properties.

Regarding the powders and commercial products obtained in Production Examples 14 to 27,
Absorbance in the ultraviolet region (300,350 parts m), visible region (55
The reflectance of 0 part m) is shown in the table. The absorbance of ultraviolet rays was measured using a spectrophotometer after dispersing 1% by weight of the powder in castor oil and applying it to a thickness of 5 μm on a quartz plate.

2. The reflectance in the visible region was measured by dispersing 10% by weight of the powder in castor oil, applying it to a thickness of 0.101 mm on a black hiding rate test paper, and using a colorimeter.

(Results) As shown in the table, the powder of this production example showed good results in both ultraviolet shielding effect and transparency.

(Hereinafter, blank) The amount of titanium hydroxide in the cosmetic of the present invention varies depending on the type of cosmetic, but it is usually required to be 0.1% by weight or more based on the total weight of the cosmetic. If the amount is less than %, the effect is not significant. The usual amount is 0.1 to 6
0% by weight, preferably in the range of 0.5 to 20% by weight.

The cosmetic of the present invention can take the form of powder, cake, pencil, stick, ointment, liquid, etc.
For example, facial cosmetics such as lotion, milky lotion, cream, makeup cosmetics such as foundation, rouge, eye shadow, blush, eyeliner, nail enamel, mascara, hair cosmetics such as hair treatment, hair liquid, setting lotion, etc. is included.

In addition to the above-mentioned essential ingredients, the cosmetics of the present invention may contain ingredients commonly used in cosmetics within a range that does not impair the effects of the present invention. For example, solid and semi-solid oils such as vaseline, lanolin, ceresin, carnauba wax, candelilla wax, higher fatty acids, and higher alcohols, liquid oils such as squalane, liquid paraffin, ester oil, and triglyceride, and oils such as silicone oil. , moisturizing agents such as sodium hyaluronate and glycerin, surfactants such as cationic surfactants and nonionic surfactants, pigments, preservatives, fragrances, activators, etc. can be appropriately blended.

(Margins below) [Example] Next, the present invention will be explained in more detail with reference to comparative examples and examples, but the present invention is not limited only to these examples. The blending amount is in weight%.

! JLLL Emulsified Foundation l) Ion-exchanged water 60.92) Distearyldimethylammonium chloride 0.13) Sodium L-glutamate 2.04) Polyoxyalkylene-modified organopolysiloxane (MW 3000) (18% polyoxyalkylene groups) 4. 05) Decamethylcyclopentasiloxane 12.06) Liquid paraffin (120
cs ) 5.07) 5.0 fine particles of titanium hydroxide obtained in Production Example 1 8) Sericite 5.36
9) Kaolin 4.010
) Titanium oxide 0.32=
2 11) Iron oxide yellow 0.801
2) Iron oxide red o, 361
3) Iron oxide black o, 16 (manufacturing method) After heating and stirring components 1) to 3) to 70°C, the fine particle titanium hydroxide powder obtained in Example I and components 8) to 13) were added and dispersed. . This was added to components 4) to 6) that had been heated to 70°C in advance and emulsified and dispersed. Thereafter, the mixture was stirred and cooled to room temperature to obtain the desired emulsified foundation. This foundation exhibited hydrophobic properties.

X-Obanyu Powder Leaf Amp-John 1) Production Example 3
Fine particles of titanium hydroxide obtained in 7.0 40.0 26°3 12.0 1.0 2.0 0.2 Talcum nylon powder Iron oxide red Iron oxide yellow Iron oxide black 8) Dimethylpolysiloxane 1.09 )
2-ethylhexyl palmitate 9.010) Sorbitan sesquioleate 1.011) Preservatives 0.312) Antioxidants 0.113) Fragrances
0.1 (Production method) Ingredients 1) to 7) were mixed in a Henschel mixer, and to this mixture, heated and dissolved components 8) to 13) were added and mixed. After this, 58P pulper laser (micron for wire)
The target powder leaf amplifier was obtained by pulverizing the powder and molding it into a medium plate.

g-Oil-based stick foundation 1) Fine particle titanium hydroxide obtained in Production Example 7 13.0 8.0 2.0 3.0 2.0 1.0 2) Kaolin 3) Talc 4) Iron oxide red 5) Oxidation Iron yellow 6) Iron oxide black 7) Squalane 27.08)
Cetyl 2-ethylhexanoate 11.09) Sorbitan sesquioleate 1.010) Aristowax 3.4II) Carnauba wax 1.012) Preservative
0.313) Antioxidants
0.114) Fragrance
0.2 (Production method) Mix ingredients 7) to 9) at 80°C, and add ingredients 1) to 6 to this.
) was added, mixed with a disper, and then treated with a roller. Components 10) to 13) were dissolved by heating, added and mixed, and then degassed. After gently mixing component 14), the mixture was filled into a container at 80° C. and cooled to obtain the target stick foundation.

Example 4 Emulsified lipstick 1) Polyethylene 7.02) Ceresin 4.03) Candelilla wax 7.04) Carnauba wax 1.00 5) Castor oil 20.06
) Liquid paraffin 18.37) Glycerol tristearate 20.08) Titanium cotoid mica 5.09) Fine particle titanium hydroxide obtained in Production Example 9 5.0 10) Yellow No. 4 A Luki i.

11) Carmino Al Lake 0,3
12) Red No. 201 0.21
3) Dibutylhydroxytoluene 0.114
)Fragrance 0.115)
Sorbitan sesquioleate 2.016) Ion-exchanged water 5゜017) Propylene glycol 2.018) Sorbit 2.0 (Production method) Ingredients ■) to 7) are heated and dissolved at 90°C, then ingredients 8) to
Add and disperse ingredients 14), and then add ingredients 15) and 18).
was gradually added and mixed by stirring. Next, component 16),
17) was gradually added at 80° C., stirred and mixed, and (1) filled and molded into a predetermined container to obtain the desired emulsified lipstick.

Trakeio J Sunken Cream ■) Ion exchange water 57.252
)L-sodium glutamate 3.03)L
3-butylene glycol 5.04) Silicone wax 0.55) Dimethylpolysiloxane (100cs) 5.06) Decamethylcyclopentasiloxane 15.07) Dioctadecyldimethylammonium chloride 0.18) Polyoxyalkylene-modified organopolysiloxane (MW) 6000) (Polyoxyalkylene group 20%) 5.09) Palmitic acid
0.210) 4-tert-butyl-4°-methoxydibenzoylmethane
0.311) Glyceryl mono-2-ethylhexanoyl diprammethoxycinnamate 1.012) Antioxidant 0.0513) Preservative 0.314) Fragrance
0.315) Production example 27
Fine particle titanium hydroxide obtained in 5.0 16) Kaolin 0.37
17) Iron oxide yellow 0.318
) Iron oxide world 0.1819)
Iron oxide black 0.1520) Titanium oxide coated mica 1.0 (manufacturing method) After heating and stirring components 1) to 3) to 70°C, components 15) to 2
0) was added and dispersed, and this was added to components 4) to 14) that had been previously heated to 70°C to emulsify and disperse. Thereafter, the mixture was stirred and cooled to room temperature to obtain the desired sunken cream.

In the cosmetics of Examples 1 to 5 above, fine titanium oxide powder (Degussa, P-25) obtained by vapor phase oxidation of titanium chloride was used instead of fine titanium hydroxide. The manufactured cosmetics were each used as a comparative example. This powder is a mixture of anatase and rutile crystals.

Regarding the cosmetics obtained in Examples 1 to 5 and Comparative Examples 1 to 5, the absorbance in the ultraviolet region (300 nm) and the visible region (420 nm
The reflectance at 550 nm) is shown in the table. The absorbance was determined by applying 0.02 g of sample on a transparent quartz plate in Example 5 and Comparative Example 5 to a thickness of 5 μm on a transparent quartz plate, and in Examples 1 to 4 and Comparative Examples 1 to 4, applying a sample of 0.02 g to a thickness of 4 × 5 Cm on a transparent quartz plate. It was applied almost uniformly over the area and measured using a spectrophotometer.

The reflectance of Example 5 and Comparative Example 5 remained unchanged;
Example 4 and Comparative Examples were melted by heating and applied to a black hiding rate test paper to a thickness of 0.35 nm, and Examples 1 to 3 and Comparative Examples 1 to 3 were coated with sample 0 on a black hiding rate test paper. .7g
was coated almost uniformly on an area of 4 x 5 cm, and measured using a colorimeter.

(Results) As shown in the table, the cosmetic of this example showed good results in both the ultraviolet scattering effect and transparency.

5 LLLL Emulsified foundation 1) Ion-exchanged water 2) Dipropylene glycol 3) Sodium L-aspartate 4) Sodium L-glutamate 5) Decamethylpolysiloxane 6) Dimethylpolysiloxane 7) Dioctadecyldimethylammonium chloride 8) Polyoxy Alkylene-modified organopolysiloxane (polyoxyalkylene group 9) Palmitic acid 10) Fine particle titanium hydroxide obtained in Production Example 13 11) Antioxidant 12) Preservative 13) Fragrance 14) Ceritonite 15) Titanium oxide 0JW 6000) 20 %) 5.0 0.5 46,65 3.0 2.0 2,O 15,0 5,0 0,2 5゜0 0.05 0゜3 0.3 8.03 6.0 16) Oxidation Iron yellow 0.617
) Iron oxide world 0.2518)
Iron oxide black 0.12ul-emulsified foundation 1) Ion exchange water 25,02)
1.3 Butylene glycol 5.03) Caustic potassium 0.14) Dioctadecyldimethylammonium chloride 1.05) Sodium L-glutamate 2.06) Sodium hyaluronate 0.17) Liquid paraffin (120cs) 5.08) Octamethylcyclo Tetrasiloxane 1O109) Decamethylcyclopentasiloxane 10.010) Dimethylpolysiloxane 5.011) Sorbitan sesquiisostearate 2.012) Polyoxyalkylene modified 4.0 Organopolysiloxane (20% polyoxyalkylene groups) 13) Oxidation Inhibitor 0.114
) Preservative 15) Fragrance 16) Fine particle titanium hydroxide obtained in Production Example 14 17) Kaolin 18) Sericite 19) Talc 20) Zinc oxide 21) Titanium oxide 22) Iron oxide yellow 23) Iron oxide field 24) Oxidation Iron Black Seed 1 Seibun” - Emulsion l) Octamethylcyclotetrasiloxane 2) Dimethylpolysiloxane (6cs) 3) Cetyl isooctanate 4) Liquid paraffin (120cs) 5) Sorbitan diisostearate 6) Polyoxyalkylene modification 0.3 0.3 0.1 5.0 7.4 3.0 3.0 IO80 1,0 0,4 0,2 10,0 10,0 2,0 2,0 3,0 Organopolysiloxane ( MW 6000) (Polyoxyalkylene group 20%) 7) Antioxidant 8) Fragrance 9) Ion exchange water 10) Sodium dextran sulfate 11) Sodium chondroitin sulfate 12) Glycerin 13) Sodium hyaluronate 14) Ammonium glycyrrhizinate 15) Preservative Agent 16) Microparticle titanium hydroxide obtained in Production Example 18 .05 0.3 53, 25 1.0 2.0 3.0 0.1 0.1 0.2 10.0 46.15 1.5 1.0 5.0 1.0 9 6) L-glutamic acid Sodium 7) Cetanol 8) Stearic acid 9) Sorbitan diisostearate 10) Silicone wax 11) Decamethyloctasiloxane 12) Liquid paraffin (70cs) 13) Olive oil 14) Lanolin 15) Vitamin E acetate 16) Antioxidants 17) Preservative 18) Fragrance 19) Fine particle titanium hydroxide obtained in Production Example 21 Example IO Sunscreen Lotion 1) Dimethylpolysiloxane (6cs) 2) Decamethylcyclopentasiloxane 3) Olive oil 4) Liquid paraffin (70cs) 3. 5 0.5 0.5 8.0 1.0 15.0 3.0 2.0 1.0 0.1 0.05 0.3 0.3 35.0 5.0 3.0 5゜0 5 .0 5) 4-tert-butyl-4'-methoxydibenzoylmethane 0.36) Glyceryl mono-
2-ethylhexanoyl diparamethoxycinnamate
1.07) Polyoxyalkylene-modified organopolysiloxane (MW 6000) (polyoxyalkylene group 20%) 6.08) Fine particle titanium hydroxide obtained in Production Example 22 2.59) Production Example 8
Fine particle titanium hydroxide obtained in 2.510) Antioxidant 0.05II) Fragrance
0.312) Ion exchange water 57.0513) Dipropylene glycol 5,014) Sodium L-glutamate 5.015) Sodium pyrrolidone carboxylate 2.016) Preservatives
0.3X Salmon Dan Makeup base 1 14) 15) 16) Ion exchange water 54.05L-Sodium aspartate 2. OL-Serine
1.0 Sodium citrate
0.51.3 Butylene glycol
5.0 Preservatives 0.
3 Organically modified montmorinite 0.5 Cetineisooctanate 2.0 Octamethylcyclotetrasiloxane 2.0 Decamethylcyclopentasiloxane 5.0 Dimethylpolysiloxane (6cs)
5.0 liquid paraffin (120cs)
3.0 Dioctadecyldimethylammonium chloride 0.2 Polyoxyalkylene-modified organopolysiloxane (MW 6000) (polyoxyalkylene group 20%) 5.04-tert-butyl-4'-methoxydibenzoylmethane
0.3 Glyceryl mono-2-ethylhexanoyl diparamethoxycinnamate 1.017) Fine particle titanium hydroxide obtained in Production Example 24 5.018) Oleyl alcohol 0.519) Stearic acid 0.520) Sorbitane di Isostearate 4.021) Antioxidant
0.0522) Fragrance
0.323) Cobalt titanate 0.324) Talc
1.525) Nylon powder (particle size 5 microns)1. OX Shikisake ■ Blushing l) Ion exchange water 49.252
) Monohexadecyl monophenyl dimethyl ammonium chloride 0.53) Sodium L-glutamate 2.04) Glycerin
5.05) Sodium pyrrolidone carboxylate 2.06) Decamethylcyclopentasiloxane 20.07) Glyceryldiolate 2.0 - 11) 12) Stearic acid silicone wax polyoxyalkylene modified organopolysiloxane (MW 6000) (polyoxy Alkylene group 20%) 4-tert-butyl-4°-methoxydibenzoylmethane Fine particles obtained in Production Example 5 Titanium hydroxide Antioxidant Preservative Fragrance Titanium oxide Iron oxide world Sericite 1.0 0.5 5. 0 0.3 5゜0 0.05 0.2 0.2 4.0 1.0 2.0 Example 13 Oil-based stick foundation 1) Fine particle titanium hydroxide obtained in Production Example 7 45.0 2) Kaolin 8.0-3) Talc 2.04)
Iron oxide world 3.05) Iron oxide yellow 2.06) Iron oxide black
1.07) Squalane
27.08) Cetyl 2-ethylhexanoate 11.09) Sorbitan sesquioleate 1.010) Aristowax
3.411) Carnauba wax
1.012) Preservatives
0,313) Antioxidant
0,■1.4. )Fragrance
0.2 (Production method) Mix ingredients 7) to 9) at 80°C, and add ingredients 1) to 6 to this.
) was added, mixed with a disper, and then treated with a roller. Components 10) to 13) were dissolved by heating, added and mixed, and then degassed. After gently mixing component 14), the mixture was filled into a container at 80° C. and cooled to obtain the target stick foundation.

<Effects of the Invention> The cosmetic of the present invention has an excellent ultraviolet shielding effect, particularly in the UV-B wavelength region of 280 to 320 nm, which could not be achieved sufficiently by blending conventional fine-particle titanium oxide powder. It was also excellent in that it gave a transparent feeling with little blanching.

In addition to the above-mentioned properties, the cosmetic containing the fine-particle titanium hydroxide powder obtained by silicone treatment was also excellent in hydrophobicity.

Claims (1)

[Claims] (1) When producing titanium hydroxide by hydrolyzing titanium alkoxide, hydrocarbons having a boiling point of 100 to 200°C and/or the following general formulas (I) and (II) [(CH_3)_2SiO]_n ( In the formula, n is an integer from 3 to 7)...(I)CH
_3[R_2SiO]_nSi(CH_3)_3 (in the formula, n is an integer of 1 to 4, R represents a methyl group or a phenyl group)...... Silicone represented by (II) 1. A cosmetic product characterized by containing fine particle titanium hydroxide powder obtained by adding the powder.