# US 10,870,734 B2 · Production method for organopolysiloxane emulsion composition

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- Number: US 10,870,734 B2
- Document ID: US10870734B2
- Status: Granted
- Kind: B2
- Application number: 15/757,521
- Filed: 2016-09-01
- Published: 2018-09-06
- Granted: 2020-12-22
- Earliest claimed: 2015-09-04
- Assignees: Shin-Etsu Chemical Co., Ltd.
- Applicants: Shin-Etsu Chemical Co., Ltd.
- Inventors: Akihiro Kobayashi; Yuko Takada; Takuya Abe
- Web page: https://patentgrep.com/patent/US10870734B2

## CPC

- C08J 3/05: from solid polymers
- A61K 8/06: Emulsions
- A61K 8/89: Polysiloxanes
- A61Q 5/002: {Preparations for repairing the hair, e.g. hair cure}
- A61Q 5/02: Preparations for cleaning the hair
- C08G 77/06: Preparatory processes
- C08G 77/08: characterised by the catalysts used
- C08G 77/16: to hydroxy groups
- C08K 5/42: Sulfonic acids; Derivatives thereof
- C08L 83/04: Polysiloxanes
- C09D 183/06: containing silicon bound to oxygen-containing groups (C09D183/12 takes precedence)
- B29C 33/62: based on polymers or oligomers
- C08J 2383/06: containing silicon bound to oxygen-containing groups (C08J2383/12 takes precedence)
- D06M 15/643: containing silicon in the main chain
- D06M 2200/12: Hydrophobic properties
- D06M 2200/50: Modified hand or grip properties; Softening compositions
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- D06M: TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS

## Abstract

A production method for an organopolysiloxane emulsion composition, wherein (I) an emulsion composition is prepared from an organopolysiloxane (A) that is represented by formula (1) and that has an octamethylcyclotetrasiloxane content of 1,000 ppm or less HO(R12SiO)nH (1), (wherein R1 is H or a monovalent hydrocarbon group and n is a number that makes the viscosity, at 25° C., of the organopolysiloxane 200 mm2/s or more but less than 2,000 mm2/s), a surfactant (B) that is represented by formula (2) and that has an alkyl naphthalene skeleton R2a—C10H(7-a)—SO3M (2), (wherein R2 is an alkyl group, M is H+, an alkali metal ion, an alkali earth metal ion, NH4+, or a tertiary NH4+, and m is 1-3), and water (C-1), and wherein (II) water (C-2) is added as necessary and then emulsion polymerization is performed in the presence of an acid catalyst (D).

## Claims

### Claim 1

A method for producing an organopolysiloxane oil-in-water emulsion composition, the method comprising the steps of:
(I) preparing an emulsion composition by emulsifying a mixture comprising
(A) 100 parts by weight of an organopolysiloxane of general formula (1) below which has an octamethylcyclotetrasiloxane content of not more than 1,000 ppm
HO(R12SiO)nH (1)
(wherein each R1 is independently a hydrogen atom or a substituted or unsubstituted monovalent hydrocarbon group of 1 to 20 carbon atoms, and n is a number such that the organopolysiloxane has a viscosity at 25° C. of at least 200 mm2/s and less than 2,000 mm2/s),
(B) from 1 to 8 parts by weight of a surfactant of general formula (2) below having an alkylnaphthalene skeleton
R2a—C10H(7-a)—SO3M (2)
(wherein R2 is a linear or branched alkyl group of 1 to 30 carbon atoms; M is a hydrogen ion, an alkali metal ion, an alkaline earth metal ion, an ammonium ion or a tertiary ammonium ion; and a is an integer from 1 or 3), and
(C-1) from 1 to 10,000 parts by weight of water; and
(II) after optionally adding to the resulting emulsion composition
(C-2) from 0 to 10,000 parts by weight of water, carrying out emulsion polymerization at a temperature below 40° C. in the presence of
(D) an acid catalyst, which is optional when component (B) is catalytic,
wherein the organopolysiloxane that forms has a viscosity at 25° C. of at least 300,000 mPa·s, the amount of octamethylcyclotetrasiloxane included in the organopolysiloxane that forms is not more than 3,000 ppm, and the size of the resulting emulsion particles is not more than 500 nm,
wherein the organopolysiloxane emulsion composition that forms after Step (II) is stable at 50° C. for at least 3 months.

### Claim 2 (depends on 1)

The production method of claim 1 wherein, when the emulsion composition is prepared in Step (I) using an emulsifier that employs a high pressure to reduce the size of the emulsion particles, the amount of component (C-1) water used per 100 parts by weight of component (A) is from 1 to 10,000 parts by weight.

### Claim 3 (depends on 1)

The production method of claim 1 wherein, when the emulsion composition is prepared in Step (I) using an emulsifier that employs shear forces to reduce the size of the emulsion particles, the amount of component (C-1) water used per 100 parts by weight of component (A) is from 1 to 10 parts by weight.

### Claim 4 (depends on 1)

The production method of claim 1, wherein the amount of the acid catalyst of component (D) present (including, when the surfactant of component (B) has a catalytic action and is encompassed by the acid catalyst of component (D), the amount of the surfactant of component (B) present) is at least 0.1 part by weight per 100 parts by weight of component (A).

### Claim 5 (depends on 1)

The production method of claim 1 wherein, in Step (I), the particle size of the emulsion composition is set to not more than 500 nm.

### Claim 6 (depends on 1)

The production method of claim 1, wherein the emulsion polymerization step is carried out at a temperature below 25° C.

### Claim 7 (depends on 1)

The production method of claim 1, wherein the polymerization time in the emulsion polymerization step is not more than 48 hours.

### Claim 8 (depends on 1)

The organopolysiloxane emulsion composition production method of claim 1, wherein the particles of the organopolysiloxane emulsion composition that forms after Step (II) have an average size of not more than 200 nm.

### Claim 9 (depends on 1)

The organopolysiloxane emulsion composition production method of claim 1, wherein the organopolysiloxane that forms in the organopolysiloxane emulsion composition that forms after Step (II) has a viscosity at 25° C. of at least 1,000,000 mPa·s.

### Claim 10 (depends on 1)

The organopolysiloxane emulsion composition production method of claim 1, wherein the amount of octamethylcyclotetrasiloxane included in the organopolysiloxane that forms within the organopolysiloxane emulsion composition that forms after Step (II) is not more than 2,000 ppm.