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A kind of preparation method of specific vinyl content polysiloxane

A technology of vinyl content and polysiloxane, which is applied in the field of polysiloxane preparation, can solve the problem of fewer types of methyl vinyl polysiloxane products, and achieve the effect of increasing or decreasing the reaction time

Active Publication Date: 2017-01-04
BLUE OCEAN & BLACK STONE TECH CO LTD FUJIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that there are fewer types of existing methyl vinyl polysiloxane products, the object of the present invention is to change 1,3,5-trivinyl-1,3,5-trimethylcyclotrisiloxane and hexamethylcyclotrisiloxane monomer feed ratio, adjust the reaction time and reaction temperature, control the conversion rate of the monomer, and prepare polysiloxane with adjustable vinyl content of 0.5-11mmol / g

Method used

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  • A kind of preparation method of specific vinyl content polysiloxane
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  • A kind of preparation method of specific vinyl content polysiloxane

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Effect test

Embodiment 1

[0018] The preparation method of polysiloxane with specific vinyl content in the embodiment of the present invention, its specific method is: add 5ml solvent (freshly steamed tetrahydrofuran) in the schlenk tube of 25ml, then add hexamethylcyclotrisiloxane monomer 105mg, stir for about 20-30min, after the hexamethylcyclotrisiloxane monomer is fully dissolved, add 1,3,5-trivinyl-1,3,5-trimethylcyclotrisiloxane monomer 990 mg, after mixing for about 5 minutes, add 10 drops of n-butyllithium solution (c=2.2M), react at 40°C for 20 hours, add frozen anhydrous methanol to terminate the end group, wait for the polymer to precipitate down, carry out Centrifugal separation, and the obtained precipitate is subjected to rotary steaming treatment to obtain polysiloxane with specific vinyl content.

[0019] After testing, the vinyl content in the prepared polysiloxane was 1.0 mmol / g. figure 1 It is the FT-IR spectrum of the methyl vinyl polysiloxane in Example 1 of the present invention....

Embodiment 2

[0021] The preparation method of polysiloxane with specific vinyl content in the embodiment of the present invention, its specific method is: add 5ml solvent (freshly steamed tetrahydrofuran) in the schlenk tube of 25ml, then add hexamethylcyclotrisiloxane monomer 165mg, stir for about 20-30min, after the hexamethylcyclotrisiloxane monomer is fully dissolved, add 1,3,5-trivinyl-1,3,5-trimethylcyclotrisiloxane monomer 405 mg, after mixing for about 5 minutes, add 10 drops of n-butyllithium solution (c=2.2M), react at 40°C for 20 hours, add frozen anhydrous methanol to terminate the terminal group, wait for the polymer to precipitate, and carry out Centrifugal separation, and the obtained precipitate is subjected to rotary steaming treatment to obtain polysiloxane with specific vinyl content.

[0022] After testing, the vinyl content in the prepared polysiloxane was 3.0 mmol / g.

Embodiment 3

[0024] The preparation method of polysiloxane with specific vinyl content in the embodiment of the present invention, its specific method is: add 5ml solvent (freshly steamed tetrahydrofuran) in the schlenk tube of 25ml, then add hexamethylcyclotrisiloxane monomer 190mg, stir for about 20-30min, after the hexamethylcyclotrisiloxane monomer is fully dissolved, add 1,3,5-trivinyl-1,3,5-trimethylcyclotrisiloxane monomer 175 mg, after mixing for about 5 minutes, add 10 drops of n-butyllithium solution (c=2.2M), react at 40°C for 20 hours, add frozen anhydrous methanol to terminate the terminal group, wait for the polymer to precipitate, and carry out Centrifugal separation, and the obtained precipitate is subjected to rotary steaming treatment to obtain polysiloxane with specific vinyl content. .

[0025] After testing, the vinyl content in the prepared polysiloxane was 6.0 mmol / g.

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Abstract

The invention relates to a preparation method of polysiloxane with a specific content of vinyl groups. The preparation method concretely comprises the following steps: adding 50-300mg of a dewatered hexamethylcyclotrisioxane monomer and 100-1000m of 1,3,5-trivinyl-1,3,5-trimethylsiloxane monomer to a 5ml new distilled tetrahydrofuran solvent, add 10 drops of an n-butyl lithium solution, reacting at 40DEG C for 20h, adding frozen anhydrous methanol for end group termination, allowing a polymer to precipitate, centrifuging, and carrying out rotary evaporation on the obtained precipitate to obtain polysiloxane with special content of vinyl groups. The polymerization process can be controlled through a controllable anionic ring opening polymerization reaction by changing a monomer feeding ratio, adjusting the reaction temperature, increasing or decreasing the reaction time and adding a chain termination agent in order to realize the regulation and control of the monomer conversion rate, the molecular weight and the vinyl group content.

Description

technical field [0001] The invention relates to a method for preparing polysiloxane with specific vinyl content, and belongs to the technical field of polysiloxane preparation. Background technique [0002] Vinyl silicone oil is used as the base material for the production of high temperature vulcanized silicone rubber (HTV), and it is mixed with crosslinking agent, reinforcing agent, colorant, structure control agent, anti-aging agent, etc. to prepare high temperature vulcanized silicone rubber raw rubber; Base silicone oil is used to make liquid silicone rubber, which is the main material for injection thermoforming silicone rubber; vinyl silicone oil reacts with polyurethane, acrylic and other organic materials, and can be made into better performance (weather resistance, aging resistance, UV resistance, Enhance toughness, etc.) new materials (such as coatings are important raw materials for the production of various coatings and modified silicone oil and other products.)...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/06
Inventor 孔杰周冬黄勇顾军渭
Owner BLUE OCEAN & BLACK STONE TECH CO LTD FUJIAN
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