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A kind of low viscosity polysiloxane and its preparation method and application

A polysiloxane, low-viscosity technology, used in adhesives, polymer adhesive additives, adhesive additives, etc., can solve the problems of methylchlorosilane monomer technical differences, complex cracking process flow, strict operation requirements, etc. , to achieve the effect of shortening the reaction induction period, simple process flow, high yield and purity

Active Publication Date: 2021-11-02
HUBEI POWER THE SILICON & FLUORINE TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the different components of methylchlorosilane high boilers, there are significant differences in the technology of different manufacturers to prepare methylchlorosilane monomers by high boiling cracking; at the same time, the cracking process has complex processes, strict operating requirements, and low yields. , low added value of products, generation of three wastes and other issues

Method used

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  • A kind of low viscosity polysiloxane and its preparation method and application
  • A kind of low viscosity polysiloxane and its preparation method and application
  • A kind of low viscosity polysiloxane and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] A low-viscosity polysiloxane with a molecular weight of 15,000 to 50,000 is prepared by the following steps in sequence:

[0065] Step 1. Co-hydrolyze methylchlorosilane high boiler, dimethyldichlorosilane, and methylhydrogendichlorosilane at normal temperature and pressure to obtain the mass percentage content of hydrogen 0.5% high-boiling silicone oil, wherein the weight ratio of methylchlorosilane high-boiler, dimethyldichlorosilane, methylhydrogendichlorosilane, and water is 85:10:5:100;

[0066] Step 2: Put the high-boiling silicone oil prepared in Step 1 into the Venturi mixer in the vertical reaction kettle through a centrifugal pump, then add divinyldimethylsilane dropwise to stir and mix and circulate, and then add 50PPm platinum complex Compound catalyst, circulate reaction at 45°C and 65r / min for 2h to obtain the intermediate, and finally dehydrate the intermediate at 110°C and vacuum -0.04MPa for 1.5h, wherein the high boiling The weight ratio of silicone o...

Embodiment 2

[0070] Step is with embodiment 1, and difference is:

[0071] In step 1, the weight ratio of the methylchlorosilane high boiler, dimethyldichlorosilane, methylhydrogendichlorosilane, and water is 80:10:10:100, and the mass of hydrogen in the high boiling silicone oil The percentage content is 0.4%;

[0072] In step 2, the weight ratio of the high boiling silicone oil to divinyldimethylsilane is 100:7, the addition amount of the platinum complex catalyst is 70PPm, the rotating speed is 100r / min, and the reaction time is 4h. The dehydration temperature is 120°C;

[0073] In step 3, the basic catalyst is an aqueous potassium hydroxide solution with a concentration of 50% by weight, and its addition is 125ppm. The temperature of the catalytic polymerization is 165°C, the vacuum degree is -0.05MPa, and the time is 35min, usually The time of continuing the reaction under pressure is 4h, after the polycondensation reaction is completed, before removing low boilers, adding neutraliz...

Embodiment 3

[0076] Step is the same as embodiment 2, and difference is:

[0077] In step 1, the weight ratio of the methylchlorosilane high boiler, dimethyldichlorosilane, methylhydrogendichlorosilane, and water is 84:10:6:100, and the mass of hydrogen in the high boiling silicone oil The percentage content is 0.6%;

[0078] In step 2, the weight ratio of the high boiling silicone oil to divinyldimethylsilane is 100:8, the addition amount of the platinum complex catalyst is 150PPm, the reaction temperature is 25°C, and the reaction time is 6h. The dehydration temperature is 145°C, the vacuum degree is -0.05MPa, and the dehydration time is 2h;

[0079] In step 3, the temperature of the catalytic polymerization is 160° C., the degree of vacuum is -0.04 MPa, and the time for continuing the reaction under normal pressure is 5 hours.

[0080] The viscosity of the prepared polysiloxane (25°C mm 2 / s) was 5000, the specific gravity was 0.98, the purity was 86%, and the yield was 85%.

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Abstract

A low-viscosity polysiloxane with a molecular weight of 15,000-50,000. The preparation method is to firstly mix methylchlorosilane high-boiler with dimethyldichlorosilane, methylhydrogendichlorosilane and water in a weight ratio of 80-90 :8~12:4~6:100 co-hydrolysis to obtain high-boiling silicone oil, and then carry out addition reaction of high-boiling silicone oil and divinyldimethylsilane in a weight ratio of 100:5-10 to obtain an intermediate, and then to the intermediate Add a basic catalyst to the body for polycondensation reaction, and finally remove the low boilers. This product not only increases the added value of methyl chlorosilane high boilers, but also can be used as silicone sealant plasticizer, powder surface treatment agent, defoamer or mold release agent for silicone glue color paste, Wide range of applications.

Description

technical field [0001] The invention belongs to the technical field of polysiloxane production, and in particular relates to a low-viscosity polysiloxane and its preparation method and application. Background technique [0002] Organosilicon is a kind of polymer material. Because of its excellent weather resistance, UV resistance, high and low temperature resistance and stable performance, it is widely used in military, civil, aerospace and marine, construction and industrial manufacturing. However, in the production process of organosilicon monomer methyl chlorosilane, a large amount of by-product methyl chlorosilane high boilers will be formed. Due to its low added value and cumbersome treatment process, it is easy to cause serious safety and environmental problems, and has become a domestic single product. The outstanding problems that body manufacturers generally have. [0003] At present, methylchlorosilane high boilers are mainly used for cracking and converting into ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04C08G77/06C08G77/08C09J11/08C09J183/04C08K9/06C08K3/34C08L21/00
CPCC08G77/04C08G77/06C08G77/08C08K3/34C08K3/346C08K9/06C08L2205/025C09J11/08C09J183/04C08L83/04C08L21/00
Inventor 李建华何蕊希何敬国
Owner HUBEI POWER THE SILICON & FLUORINE TECH
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