JPH0640847A - Water-in-oil type cosmetic - Google Patents

Abstract

PURPOSE:To obtain a water-in-oil type cosmetic providing an excellent feeling in use (refreshing feeling and excellent slip), having excellent stability with time. CONSTITUTION:A water-in-oil type cosmetic comprises an oil phase containing (A) 10-90wt.% pasty silicone composition and (B) 0.01-10wt.% silicic anhydride and/or hydrophobic silica and water as main component and a water phase component containing various kinds of water-soluble components. The component A is prepared by dispersing or blending 100 pts.wt. silicone polymer obtained by subjecting an organohydrogenpolysiloxane and an aliphatic unsaturated group-containing compound, in which at least one contains a polyoxyalkylene group, to addition polymerization in the presence or absence of a silicone oil and/or a polyhydric alcohol having <=100cS viscosity at 25 deg.C with 5-1,000 pts.wt., preferably 20-500 pts.wt. low-viscosity silicone oil and kneading under shear force.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a water-in-oil type cosmetic composition, and more particularly to a water-in-oil type cosmetic composition which provides an excellent feeling of use and has significantly improved stability over time.

[0002]

2. Description of the Related Art In recent years,
In a water-in-oil type emulsion composition, a silicone oil is used as an oil agent in order to obtain a fresh, less sticky product and good water repellency. When preparing such an emulsified composition, a lipophilic polyoxyalkylene-modified organopolysiloxane-based surfactant having good compatibility with silicone oil is generally used as an emulsifier. On the other hand, one of the applicants has previously stated that in the oil phase component,
An oil containing a silicone gel composition consisting of a partially crosslinked organopolysiloxane polymer and a low-viscosity silicone oil, and using a polyoxyalkylene-modified organopolysiloxane-based surfactant as an emulsifier, which has excellent temporal stability and usability We succeeded in obtaining a water-based emulsion composition (JP-A-3-79669).

However, when a combination of the above-mentioned oil agent and emulsifier is used, if a large amount of water is added in order to obtain a good feeling in use, stability with time is often impaired. Further, a mixture of an organohydrogen polysiloxane containing a polyoxyalkylene group and an organopolysiloxane containing an aliphatic unsaturated group, or a mixture of an organohydrogen polysiloxane and a polyoxyalkylene containing an aliphatic unsaturated group. Is added to the low viscosity silicone oil and / or polyhydric alcohol in the presence or absence to form a silicone polymer, which is kneaded with the silicone oil under shearing force to obtain a pasty silicone composition. Even when used as an oil agent, an excellent feeling in use is obtained, but a satisfactory one in terms of temporal stability has not yet been obtained.

Therefore, in addition to giving a good feeling of use,
It has been desired to develop a water-in-oil type cosmetic composition having excellent stability over time.

[0005]

Means for Solving the Problems As a result of intensive studies in view of such circumstances, the present inventors have found that an oil phase component containing a paste-like silicone composition and a silicic acid anhydride and / or hydrophobized silica described below and water. It was found that a water-in-oil type cosmetic containing a phase component provides a good feeling in use and stability over time, and has completed the present invention.

That is, the present invention provides an oil phase component and an aqueous phase component containing the following (a) and (b); (a) a pasty silicone composition, (b) silicic anhydride and / or hydrophobized silica. The present invention provides a water-in-oil type cosmetic characterized by containing.

The pasty silicone composition (a) used in the present invention has the following general formula (1), R ¹ _a R ² _b H _c SiO _{(4-abc) / 2} (1) (wherein R is ¹ is the same or different C 1-18 unsubstituted or substituted alkyl group, aryl group, aralkyl group or halogenated hydrocarbon group, R ² is a general formula C _n H _2n O (C ₂ H ₄ O) _d (C
₃ H ₆ O) _e R ³ [wherein R ³ is a hydrogen atom or a carbon number of 1 to 10]
A saturated aliphatic hydrocarbon group or a group represented by-(CO) -R ⁵ (R ⁵ is a saturated aliphatic hydrocarbon group having 1 to ⁵ carbon atoms), d is an integer of 2 to 200, and e is 0 to 200. Integer, d + e is 3
To an integer of 200, and n is 2 to 6, respectively, and a is 1.0 ≦ a ≦ 2.5,
b is 0.001 ≦ b ≦ 1.0, c is 0.001 ≦ c ≦
An organohydrogenpolysiloxane represented by each of 1.0 and / or the general formula (2) R ¹ _f H _g SiO _{(4-fg) / 2} (2) (wherein R ¹ is the same as above, f is 1.0 ≦ f ≦ 3.0,
g represents 0.001 ≦ g ≦ 1.5) and an organohydrogenpolysiloxane represented by

General formula (A) C _m H _2m-1 O (C ₂ H ₄ O) _h (C ₃ H ₆ O) _i C _m H _2m-1 (A) (wherein h is 2 to 200) An integer, i is an integer of 0 to 200, h + i is an integer of 3 to 200, and m is 2 to 6) and / or polyoxyalkylene represented by the general formula (B) R ¹ _j R ⁴ _k SiO _{(4 -jk) / 2} (B) (In the formula, R ¹ is the same as above, R ⁴ is a monovalent hydrocarbon group having 2 to 10 carbon atoms and having an aliphatic unsaturated group at the terminal, and j is 1.
0 ≦ j ≦ 3.0, and k represents 0.001 ≦ k ≦ 1.5) in combination with the organopolysiloxane represented by the general formula (1) and / or the general formula (A).
A total amount of 100 parts by weight of a composition containing the component represented by the formula (1) as an essential component is added to a low-viscosity silicone oil having a viscosity of 100 cS or less at 25 ° C. and / or polyhydric alcohol
It refers to a product obtained by kneading 100 parts by weight of a silicone polymer obtained by addition polymerization in the presence or absence of 00 parts by weight and 5 to 1,000 parts by weight of a low-viscosity silicone oil under shearing force.

The above-mentioned silicone polymer constituting the pasty silicone composition (a) used in the present invention is a silicone in which the organohydrogenpolysiloxane and the compound containing an aliphatic unsaturated group have a viscosity at 25 ° C. of 100 cS or less. It is addition-polymerized in the presence or absence of oil and / or polyhydric alcohol, but it is necessary that at least one of the organohydrogenpolysiloxane and the compound containing an aliphatic unsaturated group contains a polyoxyalkylene group. .

The combination of the organohydrogenpolysiloxane and the aliphatic unsaturated group-containing compound is, for example, one of the organohydrogenpolysiloxanes represented by the above general formula (1) containing a polyoxyalkylene group. R ¹ is bonded to an alkyl group such as a methyl group, an ethyl group, a propyl group and a butyl group, an aryl group such as a phenyl group and a tolyl group, an aralkyl group such as a benzyl group and a phenethyl group, or a carbon atom of these groups. Chloromethyl group in which a part or all of the hydrogen atoms are substituted with a halogen atom, the same or different C1-18 unsubstituted or substituted alkyl group or aryl group selected from trifluoropropyl group, aralkyl group or a halogenated hydrocarbon group, represented by R ² is the formula _{C n H 2n O (C 2} H 4 O) d (C 3 H 6 O) e -R 3 And R ³ is a hydrogen atom or a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group,
Saturated aliphatic hydrocarbon group having 1 to 10 carbon atoms such as heptyl group, octyl group or the formula-(CO) -R ⁵ (R ⁵ is 1 to 10 carbon atoms
5 saturated aliphatic hydrocarbon group), d is an integer of 2 to 200,
Examples thereof include those in which e is an integer of 0 to 200, d + e is an integer of 3 to 200, and n is 2 to 6, respectively. Further, in order to sufficiently disperse water in the paste composition obtained by kneading the obtained polymer with silicone oil under shearing force, d / e ≧ 1 is preferable.

When a is less than 1.0, the obtained polymer does not swell sufficiently in silicone oil, and when it is more than 2.5, the obtained polymer is kneaded with silicone oil under shearing force. Since it is not possible to sufficiently disperse water in the paste-like composition thus obtained, 1.0 ≦ a ≦ 2.5, preferably 1.0 to 2.0, and b is less than 0.001. Water was not sufficiently dispersed in the paste-like composition obtained by kneading the polymer with silicone oil under shearing force.
If it is larger, the swelling property of the resulting polymer in silicone oil becomes insufficient, so 0.001 ≤ b ≤ 1.0, preferably 0.005 to 1.0, and c is 0.001.
If it is less than 1.0, it becomes difficult to form a three-dimensional structure in the polymer obtained by addition polymerization, and therefore the silicone oil has a poor viscosity increasing property, and if it is more than 1.0, crosslinking of the three-dimensional structure formed by addition polymerization. Since the density becomes too high, the silicone oil cannot be held stably, so 0.001 ≦ c ≦ 1.0, preferably 0.005
Set to 1.0.

What is combined with the organohydrogenpolysiloxane represented by the above general formula (1) is the organopolysiloxane represented by the above general formula (B), wherein R ¹ is the same as above and R ⁴ is A three-dimensional structure which is a monovalent hydrocarbon group having 2 to 10 carbon atoms and having an aliphatic unsaturated group such as a vinyl group and an allyl group at the terminal, and when j is less than 1.0, it is formed by addition polymerization. The cross-linking density of the polymer is too high to obtain a polymer that stably retains the silicone oil. When it is more than 3.0, the formation of the three-dimensional structure in the polymer obtained by the addition polymerization becomes insufficient and the silicone oil Is poor in thickening,
1.0 ≦ j ≦ 3.0, preferably 1.0 to 2.5,
When k is less than 0.001, it becomes difficult to form a three-dimensional structure in the intended polymer, so that the silicone oil is poor in viscosity increasing, and when it is more than 1.5, k is formed by addition polymerization. Since the crosslinking density of the three-dimensional structure becomes too high, it becomes impossible to obtain a polymer capable of stably holding silicone oil.
Examples thereof include those containing an aliphatic unsaturated group with k ≦ 1.5, preferably 0.005 to 1.0. The mixture of the organohydrogenpolysiloxane represented by the general formula (1) and the organopolysiloxane represented by the general formula (B) is abbreviated as mixture-I hereinafter.

It is also possible to use a combination of the organohydrogenpolysiloxane represented by the general formula (1) and the polyoxyalkylene represented by the general formula (A).

Another combination of the organohydrogenpolysiloxane represented by the general formula (1) and the aliphatic unsaturated group-containing compound is, for example, the organohydrogenpolysiloxane represented by the general formula (2). When R ¹ is the same as above and f is less than 1.0, the swelling property of the obtained polymer in silicone oil cannot be sufficiently obtained.
When it is more than 3.0, it becomes difficult to form a three-dimensional structure in the polymer obtained by addition polymerization, so that the silicone oil has a poor viscosity increasing property, so 1.0 ≦ f ≦ 3.
When it is 0, preferably 1.0 to 2.5, and g is less than 0.001, it becomes difficult to form a three-dimensional structure in the polymer obtained by addition polymerization. When it is more than 1.5, the cross-linking density of the three-dimensional structure formed by addition polymerization becomes too high, and the polymer obtained does not stably hold the silicone oil, so 0.001 ≦ g ≦ 1. 5, preferably 0.00
A polyoxyalkylene represented by the general formula (A), wherein h is 2 to 200, preferably 5 to 100, and i is 0 to 200, preferably 0 to 100.
In order to sufficiently disperse water in the obtained polymer, preferably h / i ≧ 1, and m is 2 to 6, preferably 3 to 6 (hereinafter abbreviated as Mixture-II). Yes).

In the present invention, mixture-I or mixture-
Examples of the low-viscosity silicone oil having a viscosity of 100 cS or less at 25 ° C. used for addition polymerization of II include linear or branched methyl polysiloxane, methylphenyl polysiloxane, ethyl polysiloxane, ethyl methyl polysiloxane. Examples thereof include siloxane, ethylphenylpolysiloxane, and cyclic dimethylpolysiloxane such as octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane. Their viscosity at 25 ° C is 100
It may be cS or less, and particularly preferably 50 cS or less. These may be used alone or as a mixture of two or more kinds.

Examples of the polyhydric alcohol include ethylene glycol, 1,3-butylene glycol, propylene glycol, dipropylene glycol, glycerin and diglycerin. These may be used alone or in combination of two or more. May be.

The amount of the low-viscosity silicone oil and / or polyhydric alcohol is preferably 3 to 200 parts by weight, when 100 parts by weight of the mixture-I or mixture-II is used. When addition polymerization is carried out in the presence of a low-viscosity silicone oil and / or a polyhydric alcohol, a polymer containing these is obtained, but this is compared with that obtained by addition polymerization in the absence of these. Shows a high swelling property with respect to silicone oil, and exhibits an excellent thickening property.

The addition polymerization of the mixture-I or the mixture-II is carried out in the presence of a known platinum compound catalyst or rhodium compound catalyst such as chloroplatinic acid, alcohol-modified chloroplatinic acid or chloroplatinic acid-vinylsiloxane complex. Under,
The reaction may be performed at room temperature or under heating at 50 to 150 ° C.

In this case, an organic solvent may be used if necessary, and examples thereof include aliphatic alcohols such as methanol, ethanol, 2-propanol and butanol, aromatic hydrocarbons such as benzene, toluene and xylene, and n-pentane. Or aliphatic hydrocarbons such as n-hexane and cyclohexane, and halogenated hydrocarbons such as dichloromethane, chloroform, carbon tetrachloride, trichloroethane, trichloroethylene and fluorochlorohydrocarbons can be used.

To 100 parts by weight of the thus obtained silicone polymer, 5 to 1,000 parts by weight, preferably 20 to 500 parts by weight of a low-viscosity silicone oil is dispersed and mixed, and then kneaded under a shearing force. A paste-like uniform silicone composition is obtained.

When the amount of the silicone polymer is less than the above range, a stable and good gel structure cannot be maintained. On the contrary, when the amount exceeds the above range, heaviness is felt on the skin and usability and usability are deteriorated. Therefore, it is not preferable.

The silicone oil used here is linear,
It may be branched, for example, methyl polysiloxane, methylphenyl polysiloxane, ethyl polysiloxane, ethyl methyl polysiloxane, ethyl phenyl polysiloxane, octamethyl cyclotetrasiloxane, decamethyl cyclopentasiloxane, or other cyclic Examples include dimethylpolysiloxane, which may be used alone or as a mixture of two or more kinds.

The paste-like silicone composition (a) thus obtained contains 10 to 10 parts of the oil phase component used in the present invention.
It is preferable to add 90% by weight (hereinafter simply referred to as “%”).

As the silicic acid anhydride (b) used in the present invention, commercially available EROSIL 200 and EROSIL 300 are available.
(Both manufactured by Degussa Co., Ltd.), etc., and as the hydrophobized silica, commercially available Cavosil TS-530 (trimethylsiloxylated silica, manufactured by Cabot Co.) and Erosir R are also commercially available.
Preferred examples include −972 (dimethylsiloxylated silica, manufactured by Degussa), Erosil R-805 (octylsiloxylated silica, ibid.), And Erosil R-202 (silicone oil treated silica, ibid.).

Silicic anhydride and / or hydrophobized silica (b)
Is 0.01 to 10% in the oil phase component used in the present invention.
It is preferable to mix them. When it exceeds 10%, the feeling of use is deteriorated and the stability with time is deteriorated, which is not preferable.

In the oil phase component used in the present invention, in addition to the above-mentioned (a) and (b), an oil agent used in a usual emulsion composition for cosmetics is blended within a range in which the uniformity of the oil phase is not impaired. can do. Such oil agents include natural animal and vegetable oils,
Any of synthetic oils can be used, and specifically, liquid paraffin, liquid hydrocarbon such as squalane, paste or solid hydrocarbon, wax, higher fatty acid, higher alcohol,
Examples thereof include esters, glycerides, silicone oils and the like.

The oil phase component is blended in the water-in-oil type cosmetic of the present invention in an amount of 10 to 99%. If it is less than 10%, it is difficult to make the cosmetic into a water-in-oil type, and if it exceeds 99%, the feel of the cosmetic itself deteriorates, which is not preferable.

The water phase component used in the present invention contains water as a main component and various water-soluble components, and 1 to 90% should be added to the water-in-oil type cosmetic composition of the present invention. Is preferred. If it is less than 1%, it is difficult to obtain the characteristic that water is added, and if it exceeds 90%, it becomes difficult to make a water-in-oil type.

In the water-in-oil type cosmetic composition of the present invention, in addition to the above-mentioned essential components, commonly used water-based components and oil-based components such as moisturizers, preservatives, antioxidants, ultraviolet absorbers, cosmetic ingredients, fragrances, Water-soluble polymers, extender pigments, coloring pigments, volatile pigments, organic powders, hydrophobized pigments, tar dyes, etc.
It can be blended within a range that does not impair the effects of the present invention.

The water-in-oil type cosmetic of the present invention can be produced by emulsification according to a usual method except that the pasty silicone composition (a) is prepared and used in advance, and is suitable as a cosmetic base material or the like. Can be used.

[0031]

The water-in-oil type cosmetic composition of the present invention has remarkably improved stability over time without impairing the feeling of use (freshness, non-greasiness, spreadability, etc.).

[0032]

EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited thereto. First, as shown in Reference Examples 1 to 10 below, paste-like silicone compositions were sequentially manufactured.

Reference Example 1 (a) Average composition formula (3) in the reactor

[0034]

[Chemical 1]

68 g of an organohydrogenpolysiloxane represented by, 100 g of ethanol, and the average composition formula is C
H ₂ ═CHCH ₂ O (C ₂ H ₄ O) ₁₀ CH ₃ 32 g of polyoxyalkylene and 3 wt% chloroplatinic acid in ethanol solution.
After charging 3 g, stirring the mixture for 2 hours while maintaining the internal temperature at 70 to 80 ° C., and removing the solvent under reduced pressure, the average composition formula (4) was obtained.

[0036]

[Chemical 2]

An organohydrogenpolysiloxane represented by the following formula was obtained. (B) In the reactor, 100 g of the organohydrogenpolysiloxane obtained in (a) above, 100 g of ethanol and the average composition formula (5).

[0038]

[Chemical 3]

28.9 g of dimethylvinylsilyl end-capped dimethylpolysiloxane represented by and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid were charged and the internal temperature was 70 to
After maintaining at 80 ° C. and stirring for 2 hours, the solvent was removed under reduced pressure to obtain an elastic polymer.

After 20 parts by weight of this polymer and 80 parts by weight of dimethylpolysiloxane (viscosity 6 cS) were dispersed and mixed,
A three-roll mill was sufficiently kneaded under shear to prepare a silicone composition. The composition had a smooth feel and was a uniform pasty composition with a viscosity of 32,000 cP.

Reference Example 2 In the reactor, the average composition formula (6) was used.

[0042]

[Chemical 4]

100 g of an organohydrogenpolysiloxane represented by :, 62 g of ethanol, and an average composition formula of C
H ₂ = CHCH ₂ O- (C ₂ H ₄ O) ₁₀ -CH ₂ CH = CH ₂ Charge 23.6 g of a polyoxyalkylene represented by (7) and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid, Inner temperature is 70-80 ° C
After stirring at room temperature for 2 hours, the solvent was removed under reduced pressure,
A granular polymer was obtained.

33 parts by weight of the obtained polymer and 67 parts by weight of dimethylpolysiloxane (viscosity 6 cS) were dispersed and mixed, and then sufficiently kneaded under a shearing force by a three-roll mill and swollen to prepare a silicone composition. did. The composition had a smooth feel and was a uniform pasty composition with a viscosity of 24,800 cP.

Reference Example 3 The average compositional formula (3) obtained in (a) of Reference Example 1 was placed in a reactor.
Organohydrogenpolysiloxane represented by
00 g, ethanol 75 g, polyoxyalkylene 49.4 represented by the average composition formula (7) used in Reference Example 2
g and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid were charged, the internal temperature was maintained at 70 to 80 ° C., and the mixture was stirred for 2 hours, then, the solvent was removed under reduced pressure to obtain a granular polymer.

After 33 parts by weight of this polymer and 67 parts by weight of dimethylpolysiloxane (viscosity 6 cS) were dispersed and mixed,
The mixture was sufficiently kneaded by a three-roll mill under shearing force and swollen to prepare a silicone composition. The composition had a smooth feel and was in the form of a uniform paste with a viscosity of 10,600 cP.

Reference Example 4 In the reactor, the average composition formula (8)

[0048]

[Chemical 5]

100 g of the organohydrogenpolysiloxane represented by the formula, 57 g of ethanol, 13.5 g of the polyoxyalkylene represented by the average composition formula (7) used in Reference Example 2 and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid. Was charged, the internal temperature was maintained at 70 to 80 ° C., and the mixture was stirred for 2 hours, then, the solvent was removed under reduced pressure to obtain a granular polymer.

20 parts by weight of this polymer and 80 parts by weight of dimethylpolysiloxane (viscosity 6 cS) were dispersed and mixed, then sufficiently kneaded under a shearing force by a three-roll mill and swollen to prepare a silicone composition. The composition had a smooth feel and was a uniform paste with a viscosity of 22,800 cP.

Reference Example 5 100 g of the organohydrogenpolysiloxane of the average composition formula (6) used in Reference Example 2 and 103 g of ethanol in the reactor, and the poly of the average composition formula (7) used in Reference Example 2 23.6 g of oxyalkylene, dimethylpolysiloxane having a viscosity of 6 cS at 25 ° C. 82.
0.3 g of ethanol solution of 4 g and chloroplatinic acid 3% by weight
Was charged, the internal temperature was maintained at 70 to 80 ° C., the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure to obtain a silicone polymer.

Next, 100 parts by weight of this silicone polymer was dispersed and mixed with 100 parts by weight of dimethylpolysiloxane having a viscosity of 6 cS at 25 ° C., and the mixture was sufficiently kneaded by a three-roll mill under shearing force to swell to give a silicone composition. The thing was made. This was a homogeneous paste-like composition with a smooth feel and a viscosity of 82,800 cP.

Reference Example 6 Organohydrogenpolysiloxane 100 represented by the average composition formula (8) used in Reference Example 4 was placed in a reactor.
g, ethanol 95 g, polyoxyalkylene 13.5 g of the average composition formula (7) used in Reference Example 2, and dimethylpolysiloxane 75.7 having a viscosity at 25 ° C. of 5 cS.
g and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid were charged and treated in the same manner as in Reference Example 5 to prepare a polymer.

Next, 100 parts by weight of this polymer and 200 parts by weight of octamethylcyclotetrasiloxane were dispersed and mixed, and then sufficiently kneaded under a shearing force by a three-roll mill to produce a swollen silicone composition. This was a uniform paste-like composition having a smooth feel and a viscosity of 44,000 cP.

Reference Example 7 Average composition formula (9)

[0056]

[Chemical 6]

100 g of organohydrogenpolysiloxane represented by
CH ₂ = CHCH ₂ O (C ₂ H ₄ O) ₃₀ CH ₂ CH = CH ₂ 18.5 g of polyoxyalkylene represented by (10), 29.6 g of dimethylpolysiloxane having a viscosity of 6 cS at 25 ° C. and platinum chloride Charge 0.3 g of an ethanol solution containing 3% by weight of acid,
A polymer was prepared by treating in the same manner as in Reference Example 5.

Then, 100 parts by weight of this polymer and 200 parts by weight of phenyltris (trimethylsiloxy) silane were dispersed and mixed, and then sufficiently kneaded under a shearing force by a three-roll mill to make a swollen silicone composition. . This was a homogeneous paste-like composition having a smooth feel and a viscosity of 25,500 cP.

Reference Example 8 The average compositional formula (4) obtained in (a) of Reference Example 1 was placed in a reactor.
Organohydrogenpolysiloxane represented by
00 g, ethanol 72 g, average composition formula (11)

[0060]

[Chemical 7]

28.9 g of dimethylpolysiloxane whose end is blocked with a dimethylvinylsilyl group represented by 2
A polymer was prepared by charging 14.3 g of dimethylpolysiloxane having a viscosity of 30 cS at 5 ° C and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid and treating in the same manner as in Reference Example 5.

Then, 22.2 parts by weight of this polymer and 25 ° C.
Dimethylpolysiloxane 7 with a viscosity of 6 cS at
7.8 parts by weight were dispersed and mixed, and then thoroughly kneaded under a shearing force with a three-roll mill to prepare a silicone composition.
This product has a smooth feel and a viscosity of 48,000 cP
Was a uniform paste-like composition.

Reference Example 9 100 g of the organohydrogenpolysiloxane of the average composition formula (6) used in Reference Example 2 and 103 g of ethanol in the reactor, and the polyoxyalkylene of the average composition formula (7) used in Reference Example 2 23.6 g, 1,3-butylene glycol 82.4 g and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid were charged, the mixture was stirred for 2 hours while maintaining the internal temperature at 70 to 80 ° C., and then the solvent was added under reduced pressure. After removing
A silicone polymer was obtained.

Then, 100 parts by weight of this silicone polymer was dispersed and mixed with 100 parts by weight of dimethylpolysiloxane having a viscosity of 50 cS at 25 ° C., and then sufficiently kneaded and swelled by a three-roll mill under shearing force to obtain a silicone composition. The thing was made. This was a homogeneous paste-like composition with a smooth feel and a viscosity of 65,000 cP.

Reference Example 10 The average compositional formula (12) was added in the reactor.

[0066]

[Chemical 8]

100 g of organohydrogenpolysiloxane represented by: 160 g of ethanol, average composition formula is CH ₂ = CHCH ₂ O (C ₂ H ₄ O) _30- (C ₃ H ₆ O) ₁₀ -CH ₂ CH = CH ₂ (1
34.7 g of polyoxyalkylene represented by 3), 20 g of ethylene glycol, and a viscosity at 25 ° C. of 10 cS
13.7 g of dimethylpolysiloxane and 0.3 g of an ethanol solution containing 3% by weight of chloroplatinic acid were charged, and Reference Example 5
A polymer was prepared in the same manner as described above.

Next, 100 parts by weight of this polymer and 300 parts by weight of decamethylcyclopentasiloxane were dispersed and mixed, and then sufficiently kneaded and swollen by a three-roll mill under shearing force to prepare a silicone composition. This was a uniform paste-like composition having a smooth feel and a viscosity of 52,000 cP.

Examples 1 and 2 and Comparative Example 1 (water-in-oil type cream) Water-in-oil type creams having the compositions shown in Table 1 below were produced by the following method.

(Manufacturing Method) The following steps A, B and C are used. A: (1) to (4) are mixed. B: (5) to (8) are heated and mixed uniformly. C: Add B to A with stirring and cool.

The water-in-oil type cream thus obtained was evaluated for stability over time (40 ° C., after 1 month and after 3 months) and feeling of use (freshness and spreadability) according to the following evaluation criteria. The results are also shown in Table 1.

(Evaluation criteria for stability over time) A: Good with no change. ◯: Some gelation is recognized. Δ: Some drainage is observed. X: Drainage or separation is recognized.

(Evaluation Criteria for Usability) A: Very good ○: Good. Δ: Neither can be said. X: Bad.

[0074]

[Table 1]

As is clear from the results shown in Table 1, the products of the present invention have remarkably improved stability over time, and do not impair the usability improved by the incorporation of the pasty silicone composition. Met.

Example 3 (Cream Eyeshadow) A creamy eyeshadow having the following composition was produced by the following method.

(Manufacturing Method) The following steps A and B are used. A: After mixing (1) to (4), (5) to (8) are added and uniformly dispersed. B: (9), (10) and (12) are heated and dissolved. C: Mix B with A while stirring, add (11) and cool.

[0078]

Table 2 Composition (% by weight) (1) Paste-like silicone composition (obtained in Reference Example 9) 10 (2) Dimethylpolysiloxane (6cS) 10 (3) Glyceryl trioctanoate 20 (4) Hydrophobization Silica (Erosir R-972) 0.3 (5) Mica titanium 5 (6) Iron oxide mica titanium 5 (7) Mica 3 (8) Color pigment 2 (9) 1,3-butylene glycol 10 (10) Preservative Appropriate amount (11) Perfume Appropriate amount (12) Purified water Remaining amount

Example 4 (Sunscreen cream) A sunscreen cream having the following composition was produced by the following method.

(Manufacturing Method) The following steps A and B are used. A: (1) to (5) are uniformly mixed. B: (7) to (9) are heated and dissolved. C: Mix B with A while stirring, add (6) and cool.

[0081]

[Table 3] Composition (% by weight) (1) Paste-like silicone composition (obtained in Reference Example 6) 15 (2) Methylphenylpolysiloxane 5 (3) Cetyl 2-ethylhexanoate 5 (4) Hydrophobic Silica (Cabosil TS-530) 0.5 (5) UV absorber 5.5 (6) Fragrance 0.5 (7) 1,3-butylene glycol 10 (8) Preservative proper amount (9) Purified water balance

The water-in-oil type cosmetics of the present invention obtained in Examples 3 and 4 were refreshing and non-greasy, and at the same time, were extremely good in stability over time.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Koji Sakuda 1 Hitomi, Oita, Matsuida-cho, Usui-gun, Gunma Prefecture 10 Shin-Etsu Chemical Co., Ltd. Silicone Electronic Materials Research Laboratory (72) Kenichi Isobe Matsuda-cho, Usui-gun, Gunma Prefecture Hitomi, Daiji 10 Shin-Etsu Chemical Co., Ltd. Silicon Electronic Materials Research Laboratory

Claims (1)

[Claims] 1. An oil phase component and an aqueous phase component containing the following (a) and (b); (a) a pasty silicone composition, (b) silicic acid anhydride and / or hydrophobized silica. A water-in-oil type cosmetic characterized by: