JP3510774B2 - Oil-in-water organopolysiloxane emulsion and method for producing the same - Google Patents

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to an oil-in-water type organopolysiloxane emulsion and a method for producing the same, and the obtained emulsion is a cosmetic for hair such as a rinse, a conditioner and a treatment agent, a polish and a release agent. Agent,
It can be used as a fiber treatment agent.

[0002]

BACKGROUND OF THE INVENTION Organopolysiloxane emulsions are widely used as raw materials for hair cosmetics, polishes, release agents, fiber treatment agents and the like. Particularly 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 improve the adhesion to hair. For example, it has been proposed to add this to a shampoo composition (see JP-A-4-36226 and 4-224309), in which the organopolysiloxane emulsion preferably has a particle size of less than 2 μm. It is described that when used, a shampoo composition which does not impair foamability can be obtained.
A method of adding an organopolysiloxane emulsion as a microemulsion has also been proposed. (JP 63
-130512, Japanese Patent Laid-Open Nos. 5-13994 and 5-163122).

Further, these organopolysiloxane emulsions having a relatively small particle size have poor adhesion to hair and are therefore easily washed off from the 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 (JP-A-7-
See 188557). However, since this organopolysiloxane emulsion uses an anionic surfactant as an emulsifier, it is suitable as a raw material for shampoos, but when incorporated into cationic hair cosmetics such as rinses, conditioners, and treatment agents, the components separate. It is difficult to obtain a stable dispersion due to the precipitation and precipitation.

In order to improve these points, an organopolysiloxane emulsion with a cationic surfactant has also been proposed (see Japanese Patent Application No. 9-71336). Japanese Patent Application No. 9-71
No. 336 uses a cationic surfactant having a quaternary ammonium salt group as an emulsifier of organopolysiloxane. The smaller the carbon number of the alkyl group or alkenyl group contained in this cationic surfactant, the stronger the activity and the more stable the emulsion can be obtained. However, this cationic surfactant having a small number of carbon atoms in the alkyl group is known to have an antibacterial action, and since it has a strong stimulant property, it has a carbon number of 18 when considering the irritation to the mucous membrane of the eye when used in cosmetics. It is desirable to have the above alkyl groups. However, when a cationic surfactant having an alkyl group having about 16 carbon atoms is used, a stable emulsion can be obtained, but when a cationic surfactant having an alkyl group having 18 or more carbon atoms is used, Since the particle size of the obtained emulsion becomes too large, there is a problem that the stability is lowered.

[0005]

From the above, it is possible to use a quaternary ammonium salt type cationic surfactant having a high-polymerization degree silicone as a base and having an alkyl group or an alkenyl group having a low carbon number. An organopolysiloxane emulsion having excellent storage stability is desired.

[0006]

SUMMARY OF THE INVENTION The present invention relates to an oil-in-water type organopolysiloxane emulsion capable of solving the above-mentioned drawbacks and problems of the prior art and a method for producing the same. ) (A) General formula R ¹ _a SiO
_{(4-a) / 2} (wherein R ¹ is an unsubstituted or substituted one or more monovalent hydrocarbon group having 1 to 20 carbon atoms, 1.8 ≦ a ≦
2.2), the viscosity at 25 ° C is 1 million mm
10 to 90% by weight of a high-polymerization degree silicone of ² / s or more, (b) general formula R ¹ _a SiO _{(4-a) / 2} (wherein R ¹ is an unsubstituted or substituted one 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, 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 1
One is an alkyl group or an alkenyl group having 22 carbon atoms,
The rest is an alkyl group having 1 to 5 carbon atoms or a benzyl group, and X ⁻ is a halogen ion] 1 to 20 parts by weight of a quaternary ammonium salt cationic surfactant, (C)
It is an oil-in-water type organopolysiloxane emulsion consisting of 1 to 20 parts by weight of polyhydric alcohol and 10 to 300 parts by weight of water (D).

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below. R ^{1 in} the general formula of the organopolysiloxanes (A) and (B) of (A) in the present invention is methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group, heptyl group, octyl group. , Nonyl group, decyl group, dodecyl group, tetradecyl group, hexadecyl group, octadecyl group, and other alkyl groups; phenyl group, tolyl group, and other aryl groups; cyclopentyl group, cyclohexyl group, and other cycloalkyl groups; 3, 3, 3- Trifluoropropyl group,
3,3,4,5,5,6,6,6-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 A group selected from an epoxy group, a mercapto group, an acryloxy group, a methacryloxy group, an acyloxyalkyl group, a carboxyl group, a hydroxyl group, and a hydrocarbon group containing an ether group, among which a methyl group and / or a phenyl group and Alternatively, an amino-substituted alkyl group is particularly preferable, and one in which 50 mol% or more is a methyl group is most preferable. The high polymerization degree silicone (A) of (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.

The silicone oil (B) of (A) in the present invention preferably has a viscosity at 25 ° C. of ² to 1,000 mm ² / s. More preferably, it is 10 to 500 mm ² / s of silicone oil. If it is less than 2 mm ² / s, it is not suitable for cosmetics because it is highly irritating to the skin, and if it exceeds 1,000 mm ² / s, the solubility of component (a) of highly polymerized silicone in (b) decreases. To do. The silicone oil (b) may be linear or cyclic. Examples of cyclic silicones 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 is mentioned, and among them, octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane are preferable.

The hydrocarbon solvent in the present invention has a boiling point of 60 to
It is preferably 260 ° C. When the boiling point is less than 60 ° C, the solvent odor is too strong, which is not preferable for cosmetics. When the boiling point exceeds 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
Solvents 1016, 1620, 2028 (manufactured by Idemitsu Petrochemical Co., Ltd.), Marcazole R (manufactured by Maruzen Petrochemical Co., Ltd.), Nisseki Isol 300, 400 (manufactured by Nippon Petrochemical Co., Ltd.), Shell Sol 71 (manufactured by Shell Chemical Co., Ltd.), Saltor 100. ,
130, 220 (made by Philips), isohexadecane (made by Bayer Japan), etc. can be mentioned.

The organopolysiloxane mixture of (A) (A) and (B) in 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 of (a) will be low, and the adhesion to hair will be reduced. When both (a) and (b) are dimethylpolysiloxane, increase the ratio of the high-polymerization degree silicone of (a) so that the viscosity of the organopolysiloxane mixture composed of these is 100,000 mm ² / s or more. It is preferable.

In the cationic surfactant of the quaternary ammonium salt of (B) in the present invention, at least one of the four R ² groups is an alkyl group or an alkenyl group having 22 carbon atoms, and the balance is benzyl. A group or an alkyl group having 1 to 5 carbon atoms, and X ⁻ is a halogen ion. Here, taking alkyl trimethyl ammonium chloride (wherein the carbon number of the alkyl group is 12 to 22) as an example and comparing the safety focusing on the carbon number of the alkyl group, in the case of C ₁₂ , sterilization,
It is used as a disinfectant, naturally has a strong stimulant, and cannot be used in cosmetic emulsions. The LD ₅₀ (rat) of C ₁₆ is 250 to 300 mg / kg, which is problematic in terms of safety and irritation. LD ₅₀ (rat) 1,000 mg / C ₁₈
It is known to be kg. The number of carbon atoms in the alkyl group is 22
It is estimated that the LD ₅₀ (rat) at 1,000 is> 1,000 mg / kg.
Therefore, _C18 or higher is preferable for cosmetics,
From the viewpoint of safety, C ₂₂ is more preferable than C ₁₈ . On the other hand, from the viewpoint of storage stability, in the case of C ₁₈ , the addition of the polyether-modified silicone gives an organopolysiloxane emulsion having excellent storage stability, whereas in the case of C ₂₂ , the addition of the polyether-modified silicone is added. No effect,
By adding 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, of which behenyltrimethylammonium chloride is preferred. The content of (B) in the present invention is 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 cosmetic for hair using the obtained emulsion is used for hair. It is not preferable because the dry film after being applied to the composition becomes sticky.

The polyhydric alcohol (C) in the present invention is an essential component as an activating aid, and when it is emulsified only with the cationic surfactant (B) without using this activating aid, the activating power is increased. 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, with glycerin and 1,3-butylene glycol being preferred. The addition amount of the polyhydric alcohol (C) in the emulsion of the present invention is 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 long to obtain an emulsion having a target particle size. If it exceeds 20 parts by weight, the emulsified particles are likely to be broken, and the emulsion becomes unstable.

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

If the polyether-modified silicone has a high molecular weight, the dispersibility in the organopolysiloxane mixture will be poor, and if the HLB is low, the solubility in water will be low. Further, when the surface tension of this aqueous solution is high, the surface activity is lowered. 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 wt% aqueous solution is 30 dyne / cm or less. Structurally, it may be linear, cyclic, or branched.

The amount of water (D) used in the present invention is 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. When it exceeds, the stability of the obtained emulsion becomes poor. It is preferably 20 to 100 parts by weight.

The method for producing the organopolysiloxane emulsion of the present invention is, for example, a weight ratio of each component (A) / (B) /
A mixture of (C) / (D) of 100/1 to 20/1 to 20 / 0.5 to 20 is phase-inverted and emulsified from a water-in-oil type to an oil-in-water type under high shearing force, and an aqueous solution of (B) is further added. And / or obtained by diluting with water. In this production method, when (B) is less than 1, phase inversion from water-in-oil type to oil-in-water type does not occur, and when it is greater than 20, a dry film after applying a cosmetic for hair using this emulsion to hair is obtained. It is not preferable because it is sticky. If (C) is less than 1, phase inversion from water-in-oil type to oil-in-water type will not occur, and if it is greater than 20, the particle size will exceed 20 μm. Further, (B), (C) and (D) may be added separately or may be added as a mixture.

In the present invention, (A), ( ¹ ) R ¹ is a methyl group, and the viscosity at 25 ° C. is 20 to 80% by weight of a highly polymerized 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 the organopolysiloxane mixture consisting of 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) is 100/1 to 10/1 to 10 / 0.5 to 20 (weight ratio), and the water-in-oil type is subjected to phase inversion and emulsification under high shearing force, and further (B ) And an aqueous solution and / or water to obtain an emulsion.

Further, 90 mol% or more of R ¹ of the component (A) of (A) in the present invention is a methyl group, the rest is an amino group-containing alkyl group, and the viscosity at 25 ° C. is 1,000.
With 10 to 80% by weight of highly polymerized 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 When the polysiloxane mixture is emulsified with the cationic surfactant (B), the mixing ratio of each component is (A) / (B) / (C) / (D) 100/1 to 10/1.
To 10 / 0.5 to 20 (weight ratio), phase inversion emulsification from water-in-oil type to oil-in-water type under high shearing force, and further diluted with the aqueous solution (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 adhesion of hair cosmetics containing it to the hair is reduced, and 20
If it exceeds μm, the stability of the cosmetic for hair containing this decreases. It is preferably 2 to 15 μm. Examples of the apparatus used to obtain the emulsion of the present invention include an emulsifier capable of obtaining a high shearing force represented by an ultra mixer, a planetary mixer, and a combi mixer (above trade name). When the phase inversion from water-in-oil type to oil-in-water type and emulsification is performed, if the stirring time after phase inversion is too short, the dispersity 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 product will break, and the oil will separate even if diluted with water, 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.

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 of them 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, the cosmetics for hair obtained by blending these emulsions have insufficient adhesion to hair as compared with the cosmetics for hair obtained by blending the emulsion of the present invention. Therefore, the present invention uses only the cationic surfactant (B) or the combination of (B) and the polyether-modified silicone, and other nonionic surfactants, betaine surfactants and anionic surfactants are used. Is not preferred. But thickener,
It is optional to add a preservative, a fragrance, a dye, a pigment and the like within a range that does not impair the object of the present invention. Further, in order to prevent the viscosity of the emulsion from becoming thick or pasting at a low temperature and deteriorating the fluidity, ethanol, 2-propanol,
It is also optional to add alcohols such as butanol in an amount of 10 parts by weight or less.

[0021]

The present invention will be described in more detail with reference to the following examples, but the present invention is not limited thereto.
The viscosity in the preparation example is the value at 25 ° C.
Numerical values of the composition are parts by weight.

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

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

The storage stability of the emulsion is 100 g of each emulsion.
Was placed in a glass bottle and allowed to stand for 1 month in a thermostat at 45 ° C., and then the appearance was observed and evaluated according to the following criteria. ◯: Separation of oil phase and water phase was not observed Δ: Slight separation layer was formed ×: Complete separation into two layers

(Reference Example) The composition shown in the verification test (Table 1) of the prior art was emulsified. The stirring time at the phase inversion was 30 minutes.

[0026]

[Table 1]

From Table 1, it is difficult to obtain an emulsion from the organopolysiloxane mixture containing a high degree of polymerization silicone, as compared with a single dimethylpolysiloxane. Even in the case of an organopolysiloxane mixture containing a high degree of polymerization silicone, cetyltrimethylammonium chloride as a cationic surfactant (carbon number as an alkyl group)
(Containing 16 cetyl groups) makes it possible to obtain an emulsion with excellent stability, but since it has a small number of carbons, it has strong skin irritation. When the carbon number is large, the skin irritation is weakened, but the emulsifying power is weakened accordingly. Therefore, for example, as in this reference example, it is only necessary to use behenyltrimethylammonium chloride containing one alkyl group having 22 carbons as an emulsifier. It is understood that the desired product having a desired particle size and stability cannot be obtained. In the present invention, in order to solve these problems, the polyhydric alcohol (C) is added in addition to this.

(Examples 1 to 4, Comparative Examples 1 to 4) (Table 2)
The composition of each composition shown in 1 above was phase-inverted and emulsified by the same emulsifying machine as described above to obtain an emulsion. The stirring time at the phase inversion was 1 hour, and the average particle size after the stirring was measured by the above method and is shown in Table 2. The chemical formula of the polyether-modified silicone used here is shown in (Chemical formula 1).

[0029]

[Table 2]

[0030]

[Chemical 1]

In Example 1, a good emulsion is obtained, but
When the amount of 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, the emulsion with 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, but in this case, the intended emulsion was obtained.
However, unlike Comparative Example 2, no polyhydric alcohol was used and only the polyether-modified silicone was used, but the intended emulsion could not be obtained. From the above, it can be seen that the polyhydric alcohol is an essential component in the present invention, and the addition amount thereof has an optimum range. Further, as in Comparative Example 4, when the amount of water at the time of phase inversion and dilution was too large, a stable emulsion could not be obtained.

[0032]

EFFECT OF THE INVENTION The oil-in-water type organopolysiloxane emulsion of the present invention has a small irritation attributed to the surfactant used, is an emulsion having a large particle size, and is excellent in stability.
When added to hair cosmetics such as rinses, conditioners and treatment agents, it does not cause separation or precipitation and can be made into a stable dispersion, and hair cosmetics with excellent hair protection can be obtained. .

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁷ Identification code FI C08K 5/053 C08K 5/053 5/19 5/19 (72) Inventor Teruki Ikeda 1 Hitomi, Oita, Matsuida-cho, Usui-gun, Gunma Prefecture 10 Shin-Etsu Chemical Co., Ltd., Silicon Electron Materials Research Laboratory (56) Reference JP-A-6-234918 (JP, A) JP-A-9-316331 (JP, A) JP-A-7-285836 (JP, A) ) JP-A-9-278626 (JP, A) (58) Fields investigated (Int.Cl. ⁷ , DB name) C08L 83/00-83/16 C08K 3/00-13/08

Claims (5)

(57) [Claims] 1. (A) (a) General formula R ¹ _a SiO _{(4-a) / 2} (wherein R ¹ is an unsubstituted or substituted one or more monovalent one having 2 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} (wherein R ¹ is an unsubstituted or substituted one or more monovalent hydrocarbon group having 1 to 20 carbon atoms, 1.8 ≤ a ≤
2.2), the viscosity at 25 ° C is 2 to 1,00
Silicone oil is a 0 mm ² / s or boiling point from 60 to 260,
100 parts by weight of organopolysiloxane mixture consisting of 10 to 90% by weight of any one of hydrocarbon solvents at 25 ° C and having a viscosity at 25 ° C of 10,000 mm ² / s or more, (B) general formula [R ² ₄ N]
⁺ · X ⁻ [wherein at least one of the four R ² is an alkyl group or an alkenyl group having 22 carbon atoms, the remainder is an alkyl group having 1 to 5 carbon atoms or a benzyl group, and X ⁻ is An oil-in-water type composed of 1 to 20 parts by weight of a cationic surfactant of a quaternary ammonium salt represented by the formula: (C) a polyhydric alcohol 1 to 20 parts by weight, and (D) water 10 to 300 parts by weight. Organopolysiloxane emulsion. 2. A high-polymerization degree silicone having a viscosity of 10 million mm ² / s or more of 20 to 80% by weight, wherein R ¹ of (A) in (A) is a methyl group, and R ¹ in (B) is Is a methyl group, consisting of 20 to 80% by weight of silicone oil having a viscosity of ² to 500 mm ² / s at 25 ° C., 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 quaternary ammonium salt cationic surfactant (C) 1 to polyhydric alcohol
The oil-in-water type organopolysiloxane emulsion according to claim 1, which comprises 10 parts by weight and (D) 10 to 300 parts by weight of water and has an average particle size of 1 to 20 µm. 3. In (A), 90 mol% or more of R ¹ in (a) is a methyl group, the rest is an amino group-containing alkyl group, and the viscosity at 25 ° C. is 10 million mm ² / s or more. High-polymerization degree silicone 10 to 80% by weight, R ¹ in (b) is a methyl group and consists of 20 to 90% by weight of silicone oil having a viscosity of 2 to 500 mm ² / s at 25 ° C. 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 quaternary ammonium salt cationic surfactant, (C) 1 to 10 parts by weight of a polyhydric alcohol, (D) ) It comprises 10 to 300 parts by weight of water and has an average particle size of 1 to 20 µm.
The oil-in-water organopolysiloxane emulsion described. 4. A mixture of (A) / (B) / (C) / (D) in a weight ratio of 100/1 to 20/1 to 20 / 0.5 to 20 is added from a water-in-oil type under high shear. The method for producing an oil-in-water type organopolysiloxane emulsion according to claim 1, wherein the phase-inversion to oil-in-water type, emulsification, and further dilution with the aqueous solution (B) and / or water. 5. A mixture of (A) / (B) / (C) / (D) in a weight ratio of 100/1 to 10/1 to 10 / 0.5 to 20 is added from a water-in-oil type under a high shearing force. The method for producing an oil-in-water type organopolysiloxane emulsion according to claim 1, wherein the phase-inversion to oil-in-water type, emulsification, and further dilution with the aqueous solution (B) and / or water.