JPH0532788A - Production of organopolysiloxane emulsion - Google Patents

Abstract

PURPOSE:To efficiently obtain an oil-in-water type emulsion containing a high- viscosity silicone oil and an organopolysiloxane having a high polymerization degree as a base without receiving restriction of ionic properties of an emulsifying agent and requiring an emulsifier under a high shearing force. CONSTITUTION:A liquid crystal-forming emulsifying agent (e.g. octadecyltrimethylammonium or polyoxyethylene nonyl phenyl ether phosphate) is mixed with water to form liquid crystals, which are then mixed and stirred with a liquid organopolysiloxane. Water is subsequently added to produce an oil-in-water type emulsion of the organopolysiloxane. The emulsifying agent is used in an amount within the range of 1-100 pts.wt., preferably 2-40 pts.wt. based on 100 pts.wt. liquid organopolysiloxane.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an organopolysiloxane emulsion, more specifically, a cosmetic, a hairdressing agent, a fiber treatment agent, a lubricant, a release agent, a glass fiber treatment agent, and a polish. The present invention relates to a method for producing an organopolysiloxane emulsion which is effectively used as a defoaming agent.

[0002]

2. Description of the Related Art Hitherto, as a method for producing an organopolysiloxane, there has been known a method of producing it by emulsion polymerization using alkylbenzene sulfonic acid, aliphatic sulfonic acid, etc. (Japanese Patent Publication No. 41-13995). 43-
No. 18800), it is possible to relatively easily produce a polymer having a viscosity of more than 1 million cS, and the obtained emulsion particles can be fined to a particle size of about 0.2 μm, which is excellent in stability.

However, in the production method by emulsion polymerization, the emulsifier is limited to anionic or cationic type, and 10% of the starting organosiloxane is used.
The front and back remain unpolymerized. For this reason, the organopolysiloxane emulsion produced by the emulsion polymerization method may be restricted in application and cannot be used in cosmetics and hair styling products.

There is also known a method of producing an emulsion by emulsifying an organopolysiloxane with an emulsifier using a high shear emulsifying device such as a homomixer or a general stirring device.

However, in the method using a high-shear emulsifying device such as a homomixer, the substance to be emulsified is sucked from the holes provided in the stator and emulsified by shearing of the high-speed rotor, so that the viscosity is about 10,000 cS. Must be
Highly viscous organopolysiloxanes cannot be emulsified.

On the other hand, when using a general stirring device,
It is possible to emulsify up to about 100,000 cS of organopolysiloxane, but since the shearing is weak, the particle size of the emulsion becomes as large as 1 to several μm. Therefore, the storage stability of the emulsion is poor, and the emulsion particles coalesce.

[0007]

DISCLOSURE OF THE INVENTION The present invention produces an emulsion of an organopolysiloxane which is fine and has good stability, without using an emulsion polymerization method, with a small amount of emulsifier, without the need for a high-shear emulsifying device. The purpose is to

[0008]

The method for producing an organopolysiloxane emulsion of the present invention is described in the following (a) to (a).
It is characterized by including each step of (c). (A) A step of forming a liquid crystal with a liquid crystal forming emulsifier. (B) A step of mixing and stirring the liquid crystal and the liquid organopolysiloxane. (C) A step of mixing the mixture obtained in the step (b) with water to form an emulsion.

[0009]

DETAILED DESCRIPTION OF THE INVENTION

Step (a): In the present invention, first, a liquid crystal emulsifier is formed. This is an emulsifier with the property of forming liquid crystals,
This can be done by adding a sufficient amount of water to form a liquid crystal phase. The ionicity of the emulsifier is not particularly limited, and a normal liquid crystal-forming nonionic surfactant, anionic surfactant, cationic surfactant, amphoteric surfactant, etc. can be used.

Specific examples of the surfactant used include:
Nonionic surfactants such as polyoxyethylene alkyl ether, polyoxyethylene alkylphenyl ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene glycerin fatty acid ester, polyoxyethylene polyoxypropylene alkyl ether, sorbitan fatty acid ester; alkyl sulfates , Polyoxyethylene alkyl ether sulfate, polyoxyethylene alkyl ether acetate, N-acyl amino acid and its salt, alkylsulfocarboxylate, α-olefinsulfonate, α-sulfofatty acid alkyl ester salt, alkylphosphate , Anionic surfactants such as polyoxyethylene alkyl ether phosphate and its salts; cationic surfactants such as alkyl ammonium salts and alkyl benzyl ammonium salts; Examples include amphoteric surfactants such as ruquilbetaine type, imidazolinium betaine, and lecithin. These surfactants may be used alone,
Moreover, you may use combining several.

The amount of the emulsifier used may be 1 to 100 parts by weight, preferably 2 to 40 parts by weight, based on 100 parts by weight of the liquid organopolysiloxane used as the base oil.

Step (b): Next, the liquid crystal obtained in the above step (a) and the liquid organopolysiloxane to be emulsified are uniformly mixed. Liquid organopolysiloxanes can be used from low-viscosity organopolysiloxanes of about 1 cS (25 ° C., the same applies below) to high-viscosity organopolysiloxanes of 1 million cS or higher. Viscosity silicone oils and even polyorganopolysiloxanes having a high degree of polymerization in the raw rubber region can be used as base oils.

The addition amount of the organopolysiloxane is preferably such that the liquid crystal is 0.02 part by weight or more, more preferably 0.08 part by weight or more, relative to 1 part by weight of the organopolysiloxane.

The apparatus used for uniformly mixing the liquid crystal and the organopolysiloxane is not particularly limited,
Does not require high shear force, but low shear force (eg 5m / sec)
The following general stirring device may be used, and the stirring blade may be a propeller type, a turbine type, an anchor type, a ribbon type, etc., and it is sufficient that the entire mixing is possible.

Step (c): Then, when water is added to the homogeneous mixture obtained in the step (b), phase inversion occurs and the average particle size of the particles is 0.5 μm or less and highly stable organopolysiloxane in water is added. An oil emulsion is obtained. Any amount of water may be added as long as the emulsion is produced.

[0016]

According to the manufacturing method of the present invention, the following operational effects can be obtained.

(1) A wide range of liquid organopolysiloxanes can be used without being restricted by viscosity, and based on silicone oil, particularly high-viscosity silicone oil, and highly-polymerized organopolysiloxane in the raw rubber region. An oil-in-water emulsion is obtained.

(2) A fine and stable emulsion can be obtained. (3) Since the ionicity of the emulsifier is not restricted,
An appropriate emulsifier can be selected depending on the application.

(4) Efficiently organopolysiloxane without the need for a high-shear emulsifier (high-pressure emulsifier, homomixer, colloid mill, etc.), which has been required for emulsifying high-viscosity organopolysiloxane. An emulsion can be produced.

[0020]

EXAMPLES The present invention will be specifically described below with reference to examples. All parts and% in the examples are by weight. The average particle size of the emulsions obtained in the examples is the submicron particle analyzer (Coulter) manufactured by Nikkaki Co., Ltd.
It was measured using N4.

Example 1 12 parts of octadecyltrimethylammonium chloride and 3 parts of purified water are mixed to form a liquid crystal. To this, 40 parts of dimethyl silicone (100,000 cS) as an oil phase is added and mixed with a stirrer such as a paddle and a propeller. When it became a viscous transparent state, 45 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion is 0.25μ.
It was m.

Example 2 POE (p = 9.5) nonylphenyl ether phosphoric acid 6 parts Purified water 3 parts are mixed to form a liquid crystal. Add 30 parts of dimethyl silicone (1 million cS) as an oil phase to the paddle,
Mix with a stirrer such as a propeller. When it became viscous and transparent, 61 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion is 0.35
was μm. POE is polyoxyethylene,
Moreover, p shows the average addition mole number of ethylene oxide.

Example 3 A liquid crystal is formed by mixing 8 parts of POE (p = 5) lauryl ether and 6 parts of purified water. To this, 40 parts of dimethyl silicone (5000 cS) was added as an oil phase and paddle was added.
Mix with a stirrer such as a propeller. When it became a viscous transparent state, 46 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion is 0.35
was μm.

Example 4 POE (p = 20) nonylphenyl ether 8 parts Purified water 2 parts are mixed to form a liquid crystal. Add 40 parts of epoxy silicone (7000 cS) as an oil phase to this and paddle,
Mix with a stirrer such as a propeller. When it became a viscous transparent state, 50 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion is 0.27.
was μm.

Comparative Example 1 12 parts of octadecyltrimethylammonium chloride and 20 parts of purified water are mixed. This is an emulsifier solution and does not form liquid crystals. Dimethyl silicone (10
Add 40 parts of 10,000 cS) and mix with a stirrer such as a paddle and propeller. When it became a viscous transparent state, 28 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion was 1.2 μm.

Comparative Example 2 6 parts of POE (p = 9.5) nonylphenyl ether phosphoric acid and 20 parts of purified water are mixed. This is an emulsifier solution and does not form liquid crystals. Dimethyl silicone (10
30 parts of (10,000 cS) is added and mixed with a stirrer such as a paddle and a propeller. When it became a viscous transparent state, 44 parts of purified water was added and mixed again to obtain an emulsion. The average particle size of the obtained emulsion was 1.5 μm.

The evaluation results of the above emulsions are summarized in Tables 1 and 2. Criteria for stability ◯: Separation is not observed by visual inspection. Δ: A slight separation is recognized by visual inspection. X: Separation is clearly recognized by visual judgment.

[0028]

[Table 1]  Example 1 2 3 4  Organopolysiloxane content (%): Dimethyl silicone − − 40.0 − (5000cS) Dimethyl silicone 40.0 − − − (100,000 cS) Dimethyl silicone − 30.0 − − (1 million cS) 40.0 Epoxy silicone − − −(7000cS)  Liquid crystal compounding amount (%): Emulsifier 12.0 6.0 8.0 8.0Purified water 3.0 3.0 6.0 2.0  Physical properties of emulsion: Average particle size (μm) 0.25 0.35 0.35 0.27 Stability (1 week) ○ ○ ○ ○ Stability (1 month) ○ ○ ○ ○Stability (3 months) △ ○○ 〜 △ ○ 〜 △  Note) All formulation percentages are based on the final emulsion.

[0029]

[Table 2]  Comparative example 1 2  Organopolysiloxane content (%): Dimethyl silicone − − (5000cS) Dimethyl silicone 40.0 − (100,000 cS) Dimethyl silicone − 30.0 (1 million cS) Epoxy silicone − −(7000cS) Mixing amount of emulsifier (%) 12.0 6.0  Physical properties of emulsion: Average particle size (μm) 0.2 1.5 Stability (1 week) △ △ Stability (1 month) × ×Stability (3 months) × ×  Note) All formulation percentages are based on the final emulsion.

Claims (1)

Claims: 1. (a) a step of forming a liquid crystal with a liquid crystal forming emulsifier, (b) a step of mixing and stirring the liquid crystal and a liquid organopolysiloxane, (c) the step (b) A method for producing an organopolysiloxane emulsion, comprising a step of mixing the obtained mixture with water to form an emulsion.