JPH11148011A - Oil-in-water type organopolysiloxane emulsion and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain the subject emulsion excellent in storage stability and capable of utilizing for mold-releasing agents or the like by including a specific organopolysiloxane mixture, a specific cationic surfactant, a polyhydric alcohol and water. SOLUTION: This organopolysiloxane emulsion comprises (A) 100 pts.wt. organopolysiloxane mixture having >=10,000 mm<2> /s viscosity (at 25 deg.C) and comprising (i) 10-90 wt.% silicone having high polymerization degree, represented by the formula R<1> a SiO(4-a)/2 [R<1> is a 1-20C (un)saturated monofunctional hydrocarbon; 1.8<=(a)<=2.2] and having >=10000,000 mm<2> /s viscosity (at 25 ' C) and (ii) 10-90 wt.% silicone oil of the formula R<1> a SiOd(4-a)1/2 having 2-1,000 mm<2> /s viscosity (at 25 deg.C) or hydrocarbon solvent having 60-260 deg.C boiling point and (B) 1-20 pts.wt. cationic surfactant of quaternary ammonium salt of the formula [R<2> 4 N]<+> .X (one or more groups of R<2> are >=22C alkyl or the like and the remainders are each a 1-5C alkyl or the like; X is a halogen), (C) 1-20 pts.wt. polyhydric alcohol and (D) 10-300 pts.wt. water.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an oil-in-water type organopolysiloxane emulsion and a method for producing the same. The obtained emulsion is a cosmetic for hair such as a rinse, a conditioner and a treatment agent, a polishing agent, and a mold release. Agent,
It can be used as a fiber treatment agent.

[0002]

2. Description of the Related Art Emulsions of organopolysiloxanes are widely used as raw materials for cosmetics for hair, polishes, mold release agents, fiber treatment agents and the like. In particular, when used in cosmetics for hair, an emulsion of a silicone having a higher polymerization degree than a low-viscosity silicone is used in order to enhance the adhesion to hair. For example, it has been proposed to incorporate this into a shampoo composition (see JP-A-4-36226 and JP-A-4-224309). Here, the particle size of the organopolysiloxane emulsion is preferably less than 2 μm. It is described that a shampoo composition which does not impair the foaming property is obtained when used.
A method has also been proposed in which an organopolysiloxane emulsion is added as a microemulsion. (JP 63
-130512, JP-A-5-13994 and 5-163122).

[0003] Furthermore, these organopolysiloxane emulsions having a relatively small particle size have poor adhesion to hair and are easily washed away from hair. Therefore, it has been proposed to use an organopolysiloxane emulsion having a particle size of 3 to 100 μm for the purpose of improving the adhesion to hair (Japanese Patent Application Laid-Open No.
No. 188557). However, since this organopolysiloxane emulsion uses an anionic surfactant as an emulsifier, it is suitable as a raw material for shampoos.However, when it is incorporated into cationic hair cosmetics such as rinses, conditioners, and treatment agents, the components are separated. It is difficult to obtain a stable dispersion due to precipitation or precipitation.

In order to improve these points, an organopolysiloxane emulsion using a cationic surfactant has been proposed (see Japanese Patent Application No. 9-71336). Patent application Hei 9-71
No. 336 uses a cationic surfactant having a quaternary ammonium salt group as an emulsifier for an organopolysiloxane. The smaller the carbon number of the alkyl group or alkenyl group contained in the cationic surfactant, the stronger the activity and the more stable the emulsion can be obtained. However, cationic surfactants having a small number of carbon atoms in the alkyl group are known to have an antibacterial effect, and are highly irritating. Therefore, when used in cosmetics, the number of carbon atoms is 18 in consideration of irritation to the mucous membrane of the eye. It is desirable to have the above alkyl group. However, when a cationic surfactant having an alkyl group having about 16 carbon atoms is used, an emulsion having good stability can be obtained.However, when a cationic surfactant having an alkyl group having 18 or more carbon atoms is used, Since the particle size of the obtained emulsion is too large, there is a problem that stability is reduced.

[0005]

From the above, it can be seen that a quaternary ammonium salt type cationic surfactant having a high degree of polymerization and having an alkyl or alkenyl group having a low carbon number can be used as a base. There is a demand for an organopolysiloxane emulsion having excellent storage stability.

[0006]

SUMMARY OF THE INVENTION The present invention relates to an oil-in-water type organopolysiloxane emulsion which can solve the above-mentioned drawbacks and problems of the prior art, and a method for producing the same. ) (B) General formula R ¹ _a SiO
_{(4-a) / 2} (where R ¹ is one or more unsubstituted or substituted monovalent hydrocarbon groups having 1 to 20 carbon atoms, 1.8 ≦ a ≦
2.2)), the viscosity at 25 ° C is 1,000,000 mm
² / s or more high polymerization degree silicone 10 to 90% by weight, (b) general formula R ¹ _a SiO _{(4-a) / 2} (where R ¹ is ^one of unsubstituted or substituted ones having 1 to 20 carbon atoms ₎ Or two or more monovalent hydrocarbon groups,
1.8 ≦ a ≦ 2.2), a silicone oil having a viscosity of ² to 1,000 mm ² / s at 25 ° C. or a hydrocarbon solvent having a boiling point of 60 to 260 ° C., which is 10 to 90% by weight. from now, 10,000 mm ² / s or more organopolysiloxane mixture 100 parts by weight of a viscosity at 25 ° C., (B) the general formula _{^{[R 2 4 N] + ·}} X - [ wherein, of the four R ² At least one
One is an alkyl group or an alkenyl group having 22 carbon atoms,
The remainder is an alkyl group or benzyl group having 1 to 5 carbon atoms, and X ^- is a halogen ion.] 1 to 20 parts by weight of a cationic surfactant of a quaternary ammonium salt represented by the formula (C):
An oil-in-water organopolysiloxane emulsion comprising 1 to 20 parts by weight of a polyhydric alcohol and (D) 10 to 300 parts by weight of water.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described below in detail. In the present invention, R ^{1 in} the general formula of the organopolysiloxanes (A) (A) and (B) is a methyl group, an ethyl group, a propyl group, a butyl group, a pentyl group, a hexyl group, a heptyl group, an octyl group. Alkyl groups such as nonyl group, decyl group, dodecyl group, tetradecyl group, hexadecyl group, octadecyl group; aryl groups such as phenyl group and tolyl group; cycloalkyl groups such as cyclopentyl group and cyclohexyl group; Trifluoropropyl group,
3,3,4,4,5,5,6,6,6-nonafluorohexyl group, 3,3,4,4,5,5,6,6,7,7,
Fluorine-substituted alkyl groups such as 8,8,9,9,10,10,10-heptadecafluorodecyl group; amino-substituted alkyl groups such as 3-aminopropyl group and 3- (2-aminoethyl) -aminopropyl group An epoxy group, a mercapto group, an acryloxy group, a methacryloxy group, an acyloxyalkyl group, a carboxyl group, a hydroxyl group, a hydrocarbon group including an ether group, and among these, a methyl group and / or a phenyl group; Alternatively, an amino-substituted alkyl group is particularly preferred, and those in which 50 mol% or more are methyl groups are most preferred. The high-polymerization degree silicone of (A) (A) in the present invention preferably has a high viscosity in order to improve the adhesion to hair, and the viscosity at 25 ° C. is 1,000,000 mm ² / s or more. Is preferred. More preferably, the viscosity is 10 million mm ² / s or more.

In the present invention, the silicone oil (A) (B) preferably has a viscosity at 25 ° C. of ² to 1,000 mm ² / s. More preferably a silicone oil 10 to 500 mm ² / s. If it is less than 2 mm ² / s, it is not preferable for cosmetics because it is very irritating to the skin. If it exceeds 1,000 mm ² / s, the solubility of the high-polymerized silicone of component (a) in (b) decreases. I do. The silicone oil (b) may be linear or cyclic. Examples of the cyclic silicone include hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane,
1,3,5-tri- (3,3,3-trifluoropropyl) -1,3,5-trimethylcyclotrisiloxane,
1,3,5,7-tetra- (3,3,3-trifluoropropyl) -1,3,5,7-tetramethylcyclotetrasiloxane 1,3,5,7,9-penta- (3 ,
3,3-trifluoropropyl) -1, 3, 5, 7, 9
-Pentamethylcyclopentasiloxane, of which octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane are preferable.

The hydrocarbon solvent in the present invention has a boiling point of 60 to
Preferably it is 260 ° C. If the boiling point is lower than 60 ° C., the solvent odor is too strong, which is not preferable for cosmetics. If the boiling point is higher than 260 ° C., the solubility of the high polymerization degree silicone of the component (A) decreases. Specific examples that can be used include Isopar C, E, G, H, L, M (manufactured by Exxon), IP
Solvent 1016, 1620, 2028 (manufactured by Idemitsu Petrochemical Co., Ltd.), Marcazole R (manufactured by Maruzen Petrochemical Co., Ltd.), Nisseki Aizole 300, 400 (manufactured by Nippon Petrochemical Co., Ltd.), Schelsol 71 (manufactured by Shell Chemical Co., Ltd.), Soltor 100 ,
130, 220 (manufactured by Philips), isohexadecane (manufactured by Bayer Japan), and the like.

The organopolysiloxane mixture comprising (A) (A) and (B) of the present invention preferably has a viscosity at 25 ° C. of 10,000 mm ² / s or more. If this viscosity is mixed so as to be less than 10,000 mm ² / s, the ratio of the high polymerization degree silicone (a) becomes low, and the adhesion to hair is reduced. When both (a) and (b) are dimethylpolysiloxanes, the ratio of the high polymerization degree silicone of (a) is increased so that the viscosity of the organopolysiloxane mixture composed of these is 100,000 mm ² / s or more. Is preferred.

In the present invention, the cationic surfactant of the quaternary ammonium salt (B) is such that at least one of the four R ² groups is an alkyl or alkenyl group having 22 carbon atoms, and the remainder is benzyl. A group or an alkyl group having 1 to 5 carbon atoms, and X ^- is a halogen ion. Here as an example (the number of carbon atoms is 12 to 22 alkyl group) alkyltrimethylammonium chloride, comparing concentrates viewpoint of safety according to the number of carbon atoms in the alkyl group, in the case of C ₁₂ disinfection,
It is used as a disinfectant and is naturally irritating and cannot be used for cosmetic additive emulsions. Safety because when the C ₁₆ is a LD ₅₀ (rat) 250 ~300mg / kg, there is a problem in terms of irritation. The LD ₅₀ when the C ₁₈ (rat) 1,000 mg /
It is known to be kg. 22 carbon atoms in the alkyl group
It is estimated that LD ₅₀ (rat) at the time of> 1,000 mg / kg.
Therefore, for cosmetics, _C18 or more is preferable,
C ₂₂ and more preferably than C ₁₈ in terms of safety. On the other hand, when viewed from the color plane of the storage stability, although in the case of C ₁₈ organopolysiloxane emulsion having excellent storage stability by the addition of polyether-modified silicone is obtained, the addition of polyether-modified silicone For C ₂₂ No effect,
By the addition of the polyhydric alcohol, an organopolysiloxane emulsion having excellent storage stability was obtained. Specific examples of (B) in the present invention include behenyltrimethylammonium chloride, dibehenyldimethylammonium chloride, behenyldimethylbenzylammonium chloride and the like, among which behenyltrimethylammonium chloride is preferable. The content of (B) in the present invention is from 1 to 20 parts by weight, but if it is less than 1 part by weight, an emulsion cannot be obtained, and if it exceeds 20 parts by weight, a hair cosmetic using the obtained emulsion is used for hair. It is not preferable because the dried film after application to the surface has a sticky property.

In the present invention, the polyhydric alcohol (C) is an essential component as an active aid. When this active auxiliary is not used and emulsified only with the cationic surfactant (B), the active power Is too weak to obtain a good emulsion. Specific examples of the polyhydric alcohol (C) include ethylene glycol, propylene glycol, diethylene glycol,
Examples thereof include 1,3-butylene glycol, 1,4-butylene glycol, glycerin, diglycerin, triglycerin, and trimethylolpropane. Among them, glycerin and 1,3-butylene glycol are preferable. The addition amount of the polyhydric alcohol (C) in the emulsion of the present invention is from 1 to
20 parts by weight. If the amount is less than 1 part by weight, sufficient activity cannot be obtained, and it takes too much time to obtain an emulsion having a target particle size. When the amount exceeds 20 parts by weight, the emulsified particles are easily broken, so that the emulsion becomes unstable.

In the present invention, a general formula R ¹ _b R ³ _c SiO is used together with the polyhydric alcohol (C) as an auxiliary component of the active assistant.
_{(4-bc) / 2} [where R ³ is a general _formula- (C _d H _2d ) O (C ₂ H ₄ O) _e (C ₃ H ₆
O) represented by _f R ^4. B, c, d, e and f are respectively 1.0 ≦ b ≦ 2.5, 0.005 ≦ c ≦ 1.2, d is an integer of 2 to 15, e is an integer of 3 to 200, f is an integer of 0 to 100, R ⁴ is a hydrogen atom or a monovalent alkyl group or an acyl group having 1 to 20 carbon atoms]. However, if the compounding amount is large, the particle size of the emulsion
Since it exceeds 20 μm, the content is preferably 5 parts by weight or less. b is 1.0
If it is less than 3, the polyoxyalkylene content becomes too high, so that the dispersibility in the organopolysiloxane mixture becomes poor, and the action as an active aid decreases. Also,
If it exceeds 2.5, the hydrophilicity becomes poor, and similarly, the effect as an active aid decreases. More preferably 1.2 to 2.3
It is. c is from 0.005 to 1.2, but if it is less than 0.005, the hydrophilicity is poor, and if it is more than 1.2, the polyoxyalkylene content is too high, so that the action as an active aid decreases. More preferably, it is 0.01 to 1.0. d is 2 to 15, but is more preferably 3 to 12. e is 3 to 200, preferably 5 to 100. If e is less than 3, sufficient hydrophilicity cannot be obtained.
Further, f is from 0 to 100, and e / f is preferably 1 or more in order to obtain solubility in water.

If the molecular weight of the polyether-modified silicone is high, the dispersibility in the organopolysiloxane mixture will be poor, and if the HLB is low, the solubility in water will be low. If the surface tension of this aqueous solution is high, the surface activity decreases. Therefore, it is more preferable that the molecular weight is 3,000 or less, the HLB is 7 or more, and the surface tension of the 0.1% by weight aqueous solution is 30 dyne / cm or less. The structure may be linear, cyclic, or branched.

The water of (D) in the present invention is from 10 to 300 parts by weight, but if it is less than 10 parts by weight, the viscosity of the obtained emulsion is too high, and the handling becomes troublesome. If it exceeds, the stability of the obtained emulsion becomes poor. Preferably it is 20 to 100 parts by weight.

The process for producing the organopolysiloxane emulsion of the present invention is carried out, for example, by the weight ratio of each component (A) / (B) /
The mixture of (C) / (D) having a ratio of 100/1 to 20/1 to 20 / 0.5 to 20 is phase-changed from a water-in-oil type to an oil-in-water type under high shearing force and emulsified. And / or by dilution with water. In this production method, if (B) is smaller than 1, the phase-inversion from water-in-oil type to oil-in-water type will not occur, and if it is larger than 20, a dry film after applying the cosmetic for hair using this emulsion to hair will be formed. It is not preferable because it has stickiness. If (C) is less than 1, no phase inversion from water-in-oil type to oil-in-water type occurs, and if it is larger than 20, the particle size exceeds 20 μm. (B), (C) and (D) may be added separately or as a mixture.

(A) In the present invention, (A) R ¹ in (A) is a methyl group, the viscosity at 25 ° C. is 20 to 80% by weight of a high-polymerization degree silicone having a viscosity of 10 million mm ² / s or more; In
R ¹ is a methyl group, and the viscosity at 25 ° C. is 20 to 500 mm ² / s
When an organopolysiloxane mixture comprising 20 to 80% by weight of silicone oil and having a viscosity at 25 ° C. of 100,000 mm ² / s or more is emulsified with the cationic surfactant (B), the mixing ratio of each component is Is (A) / (B) /
(C) / (D) was set to 100/1 to 10/1 to 10 / 0.5 to 20 (weight ratio), the phase was changed from a water-in-oil type to an oil-in-water type under high shearing force, emulsified, and (B) ) Is diluted with an aqueous solution and / or water to obtain an emulsion.

Further, more than 90 mole% of component (i) of R ¹ in the present invention (A) is a methyl group, the remainder is an amino group-containing alkyl group, and a viscosity at 25 ° C. 1,000
10-80% by weight of high polymerization degree silicone of 10,000 mm ² / s or more,
R ¹ is a methyl group in the component (ii), the viscosity is a silicone oil 20 to 90% by weight is 10 to 500 mm ² / s at 25 ° C., is the viscosity at 25 ° C. is 10,000 mm ² / s or more organo Similarly, when the polysiloxane mixture is emulsified with the cationic surfactant (B), the mixing ratio of each component is (A) / (B) / (C) / (D) from 100/1 to 10/1.
1010 / 0.5 し て 20 (weight ratio), phase-inversion emulsification from water-in-oil type to oil-in-water type under high shearing force, and further diluting with the aqueous solution of (B) and / or water to obtain an emulsifier.

The particle size of the organopolysiloxane emulsion particles of the present invention is 1 to 20 μm. If it is less than 1 μm, the adhesiveness to hair of a hair cosmetic containing the same decreases, and
If it exceeds μm, the stability of hair cosmetics containing this compound will decrease. Preferably it is 2 to 15 μm. Examples of an apparatus used to obtain the emulsion of the present invention include an emulsifier capable of obtaining a high shear force as represented by an ultra mixer, a planetary mixer, and a combination mixer (trade names). When the stirring time after the phase inversion and the emulsification are changed from the water-in-oil type to the oil-in-water type, if the stirring time is too short, the degree of dispersion of the particle size tends to be widened, resulting in insufficient stability. If the stirring time after the phase inversion is too long, the particles of the phase inversion will be destroyed, so that even if diluted with water, the oil will be separated and a uniform oil-in-water emulsion cannot be obtained. Therefore, the stirring time is preferably 20 minutes or more and 3 hours or less.

As similar to the emulsion of the present invention,
Emulsifying the organopolysiloxane mixture of (A) with a nonionic surfactant represented by polyoxyethylene alkyl ether and a cationic surfactant of (B),
Some are obtained by emulsifying the organopolysiloxane mixture of (A) with a nonionic surfactant represented by polyoxyethylene alkyl ether, and adding a cationic surfactant at the time of dilution. However, hair cosmetics obtained by blending these emulsions have insufficient adhesion to hair as compared with hair cosmetics obtained by blending the emulsion of the present invention. Therefore, the present invention uses only the cationic surfactant of (B) or the combination of (B) and the polyether-modified silicone, and other nonionic surfactants, betaine surfactants and anionic surfactants Is not preferred. But thickeners,
It is optional to add preservatives, fragrances, dyes, pigments and the like within a range that does not impair the purpose of the present invention. Ethanol, 2-propanol,
It is also optional to add alcohols such as butanol in an amount of 10 parts by weight or less.

[0021]

EXAMPLES The present invention will be described in more detail with reference to the following Examples, but it should not be construed that the present invention is limited thereto.
The viscosity in Preparation Example is a value at 25 ° C.
The numerical values of the composition are parts by weight.

(Preparation Example 1) 40 parts by weight of a high-polymerization degree dimethylpolysiloxane having a viscosity of 20 million mm ² / s and 60 parts by weight of a dimethylpolysiloxane (viscosity of 20 mm ² / s) are uniformly dissolved.
An organopolysiloxane mixture of 800,000 mm ² / s was obtained (hereinafter referred to as mixture 1). (Preparation Example 2) 50 parts by weight of highly polymerized methylphenylpolysiloxane having a viscosity of 15 million mm ² / s (phenyl group content 5 mol%) and 50 parts by weight of dimethylpolysiloxane (viscosity 200 mm ² / s) are uniformly dissolved. Thus, an organopolysiloxane mixture having a viscosity of 1,000,000 mm ² / s was obtained (hereinafter referred to as mixture 2). (Preparation Example 3) 20 parts by weight of an amino group-containing high-polymerization degree dimethylpolysiloxane having a viscosity of 30 million mm ² / s (amino group unit is 3-aminopropyl group, amine equivalent is 700,000 g / mol), dimethylpolysiloxane ( 80 parts by weight (viscosity 10 mm ² / s) were uniformly dissolved to obtain an organopolysiloxane mixture having a viscosity of 20,000 mm ² / s (hereinafter referred to as mixture 3). (Preparation Example 4) 20 parts by weight of dimethylpolysiloxane having a high degree of polymerization having a viscosity of 10 million mm ² / s and 80 parts by weight of decamethylcyclopentasiloxane (viscosity 4.0 mm / s) were uniformly dissolved.
An organopolysiloxane mixture of 10,000 mm ² / s was obtained (hereinafter referred to as mixture 4).

An internal volume 5 equipped with a high-shear load device having an anchor-type stirrer capable of stirring the entire inside of the container and a disk-type stirrer provided with tooth-shaped projections on the periphery alternately in the vertical direction.
Each component was charged into a 1-liter stainless steel emulsifier / TK Combimix M type (trade name, manufactured by Tokushu Kika Kogyo Co., Ltd.) at the compounding ratios shown in Table 1, and an anchor type stirrer was used at 40 rpm and a disk type. An agitator was simultaneously stirred at 1,500 rpm to phase invert to obtain an emulsion. Next, only the disk-type stirrer was stopped, the remaining purified water and a surfactant aqueous solution were added, and the mixture was uniformly dissolved with an anchor-type stirrer to obtain a desired emulsion. The average particle size was measured using a Coulter Counter TA (trade name, manufactured by Coulter Electronics Co., USA).

The storage stability of the emulsion was 100 g for each emulsion.
Was placed in a glass bottle, left standing for one month in a 45 ° C. constant temperature bath, observed for appearance, and evaluated according to the following criteria. ：: Separation of the oil phase and the aqueous phase was not observed. ：: Slightly separated layer was formed.

Reference Example Demonstration Test on Prior Art The composition shown in Table 1 was emulsified. The stirring time during the phase inversion was 30 minutes.

[0026]

[Table 1]

From Table 1, it is found that an organopolysiloxane mixture containing a silicone having a high degree of polymerization does not easily produce an emulsion as compared with a single dimethylpolysiloxane. In addition, even when the organopolysiloxane mixture contains a silicone having a high degree of polymerization, cetyltrimethylammonium chloride (as an alkyl group having a carbon number of
Using 16 cetyl groups) can provide an emulsion with excellent stability, but it has strong skin irritation due to its small carbon number. If the number of carbon atoms is large, the skin irritation is weakened, but the emulsifying power is also weakened accordingly. For example, behenyl trimethylammonium chloride containing only one alkyl group having 22 carbon atoms can be used as an emulsifier as in this reference example. It is understood that the desired product having the desired particle size and stability cannot be obtained. In the present invention, in order to solve these problems, the polyhydric alcohol (C) is additionally added.

(Examples 1 to 4, Comparative Examples 1 to 4) (Table 2)
Were subjected to phase inversion and emulsification using the same emulsifier as described above to obtain an emulsion. The stirring time during the phase inversion was 1 hour, and the average particle size after the completion of the stirring was measured by the above-mentioned method and shown in Table 2. The chemical formula of the polyether-modified silicone used here is shown in (Chemical Formula 1).

[0029]

[Table 2]

[0030]

Embedded image

In Example 1, a good emulsion is obtained.
When the amount of the polyhydric alcohol added was small as in Comparative Example 1, no emulsion was obtained. When the amount of the polyhydric alcohol added was too large as in Comparative Example 3, an emulsion having good stability could not be obtained because the particle size exceeded 20 μm. In Example 2, both the polyhydric alcohol and the polyether-modified silicone were added. In this case, the desired emulsion was obtained.
However, as in Comparative Example 2, the intended emulsion could not be obtained by using only the polyether-modified silicone without using the polyhydric alcohol. From the above, it is understood that the polyhydric alcohol is an essential component in the present invention, and the amount of the polyhydric alcohol has an optimum range. Further, when the amount of water at the time of phase inversion and dilution was too large as in Comparative Example 4, a stable emulsion could not be obtained.

[0032]

The oil-in-water organopolysiloxane emulsion of the present invention has low irritation due to the surfactant used and is excellent in stability despite being a large particle size emulsion.
When incorporated into hair cosmetics such as rinses, conditioners, treatment agents, etc., they do not separate or precipitate, can be made into a stable dispersion, and can provide a hair cosmetic excellent in hair protection. .

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[Procedure amendment]

[Submission date] January 19, 1999

[Procedure amendment 1]

[Document name to be amended] Statement

[Correction target item name] 0030

[Correction method] Change

[Correction contents]

[0030]

Embedded image

Continuation of the front page (51) Int.Cl. ⁶ Identification code FI C08K 5/053 C08K 5/053 5/19 5/19 (72) Inventor Teruki Ikeda 1 Hitomi, Matsuida-cho, Usui-gun, Gunma Prefecture 10 Shinetsu Chemical Industrial Co., Ltd. Silicone Electronic Materials Technology Laboratory

Claims (5)

[Claims] (A) (a) a compound represented by the general formula: R ¹ _a SiO _{(4-a) / 2} (where R ¹ is one or more monovalent or unsubstituted monovalent having 1 to 20 carbon atoms ₎ Hydrocarbon group, 1.8 ≦ a ≦ 2.2)
In shown, 25 high degree of polymerization silicone 10-90 wt% viscosity is at least 1 million mm ² / s at ° C., (ii) the general formula R ¹ _a SiO
_{(4-a) / 2} (where R ¹ is one or more unsubstituted or substituted monovalent hydrocarbon group having 1 to 20 carbon atoms, 1.8 ≦ a ≦
2.2) and a viscosity at 25 ° C of 2 to 1,00.
0 mm ² / s silicone oil, or boiling point 60-260
° C. of consists one 10-90 wt% either hydrocarbon solvent, 100 parts by weight of a viscosity at 25 ° C. is 10,000 mm ² / s or more organopolysiloxane mixture, (B) the general formula [R ² ₄ N]
⁺ · X ^- [wherein, at least one of the four R ² is an alkyl or alkenyl group having 22 carbon atoms, the remainder is an alkyl group or a benzyl group having 1 to 5 carbon atoms, X ^- is An oil-in-water type comprising 1 to 20 parts by weight of a cationic surfactant of a quaternary ammonium salt represented by the following formula: (C) 1 to 20 parts by weight of a polyhydric alcohol, and (D) 10 to 300 parts by weight of water. Organopolysiloxane emulsion. Wherein R ¹ of the (A) (b) is a methyl group, highly polymerized silicone 20 to 80 wt% viscosity is more than 10 million mm ² / s at 25 ° C., R ¹ in (b) Is a methyl group, comprises 20 to 80% by weight of a silicone oil having a viscosity of ² to 500 mm ² / s at 25 ° C., and 100 parts by weight of an organopolysiloxane mixture having a viscosity of 100,000 mm ² / s or more at 25 ° C. (B) 1 to 10 parts by weight of cationic surfactant of quaternary ammonium salt (C) Polyhydric alcohol 1 to
2. The oil-in-water organopolysiloxane emulsion according to claim 1, comprising 10 parts by weight and (D) 10 to 300 parts by weight of water and having an average particle size of 1 to 20 [mu] m. (A) In (A), 90 mol% or more of R ¹ in (A) is a methyl group, the remainder is an amino group-containing alkyl group, and the viscosity at 25 ° C. is 10,000,000 mm ² / s or more. high degree of polymerization silicone 10 to 80 wt%, in R ¹ is a methyl group, consists of silicone oil 20 to 90% by weight is. 2 to 500 mm ² / s viscosity at 25 ° C., a viscosity at 25 ° C. (b) 100 parts by weight of an organopolysiloxane mixture of 10,000 mm ² / s or more, (B) 1 to 10 parts by weight of a cationic surfactant of a quaternary ammonium salt, (C) 1 to 10 parts by weight of a polyhydric alcohol, (D 2. The composition according to claim 1, wherein the composition comprises 10 to 300 parts by weight of water and has an average particle size of 1 to 20 μm.
The oil-in-water type organopolysiloxane emulsion according to the above. 4. A mixture having a weight ratio of (A) / (B) / (C) / (D) of from 100/1 to 20/1 to 20 / 0.5 to 20 under water-in-oil type under high shearing force. The method for producing an oil-in-water type organopolysiloxane emulsion according to claim 1, wherein the phase-inversion and emulsification to an oil-in-water type and further dilution with the aqueous solution (B) and / or water are carried out. 5. A mixture of (A) / (B) / (C) / (D) having a weight ratio of 100/1 to 10/1 to 10 / 0.5 to 20 under water-in-oil type under high shearing force. The method for producing an oil-in-water type organopolysiloxane emulsion according to claim 1, wherein the phase-inversion and emulsification to an oil-in-water type and further dilution with the aqueous solution (B) and / or water are carried out.