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Preparation method of epoxy phenyl silicone rubber

A technology of phenyl silicone rubber and epoxidized benzene, which is applied in the field of silicone rubber, can solve problems such as corrosion of metal reactors and troublesome construction of industrial production lines, and achieve the effects of improving efficiency, shortening reaction time, and mild reaction process

Active Publication Date: 2019-10-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And chloroform has a serious corrosion effect on metal reactors, which will cause great trouble to the construction of industrial production lines

Method used

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  • Preparation method of epoxy phenyl silicone rubber
  • Preparation method of epoxy phenyl silicone rubber
  • Preparation method of epoxy phenyl silicone rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 200mL of chlorobenzene and vinyl content to 14.13% in the 250mL round-bottomed flask equipped with magnetic stirring, and 10g of phenyl silicone rubber (self-made) with phenyl content of 22.30%, control the temperature of the water bath at 55°C and 250 rpm stirring rate. After the phenyl silicone rubber is completely dissolved, add 3.68g m-chloroperoxybenzoic acid (the ratio of peroxyacid to double bond is 1:1.3) to start the reaction. After 72 hours, it is precipitated with methanol, washed 2-3 times, and placed in a vacuum Oven dry for 12h, take out.

[0041] Wherein the preparation method of phenyl silicone rubber:

[0042] (1) Add 48.20 g of octamethylcyclotetrasiloxane and 12.92 g of tetramethyltetravinylcyclotetrasiloxane into the reaction flask, vacuumize and remove water at 45-50°C for 1 hour, and then under nitrogen protection Add 0.75g of alkali gel catalyst and 0.03g of decamethyltetrasiloxane as an end-capping agent, and finally add 39.66g of octapheny...

Embodiment 2

[0049] Add 200mL chlorobenzene and vinyl content to 250mL round-bottomed flask equipped with magnetic sub-stirring and be 14.13%, phenyl silicone rubber (self-made) 6g that phenyl content is 22.30%, control water bath temperature to be 55 ℃ and 250 to rotate stirring rate. After the phenyl silicone rubber is completely dissolved, add 2.21g of m-chloroperoxybenzoic acid (the ratio of peroxyacid to double bond is 1:1.3) to start the reaction. After 72 hours, it is precipitated with methanol, washed 2-3 times, and placed in a vacuum Oven dry for 12h, take out. Characterized by NMR, the epoxidation conversion rate was 94.2%.

[0050] Wherein the preparation method of phenyl silicone rubber is the same as that of Example 1.

Embodiment 3

[0052]Add 200mL of chlorobenzene and vinyl content to 14.13% in the 250mL round-bottomed flask equipped with magnetic stirring, and 10g of phenyl silicone rubber (self-made) with phenyl content of 22.30%, control the temperature of the water bath at 55°C and 250 rpm stirring rate. After the phenyl silicone rubber is completely dissolved, add 3.68g m-chloroperoxybenzoic acid (the ratio of peroxyacid to double bond is 1:1.3) to start the reaction. After 96h, it is precipitated with methanol, washed 2-3 times, and placed in a vacuum Oven dry for 12h, take out. Characterized by NMR, the epoxidation conversion rate was 96.3%.

[0053] Wherein the preparation method of phenyl silicone rubber is the same as that of Example 1.

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Abstract

The invention discloses a preparation method of epoxy phenyl silicone rubber. The method includes the steps that (1) chlorobenzene and phenyl silicone rubber are added into a reaction kettle, and stirring is conducted until the phenyl silicone rubber is completely dissolved; and (2) meta-chloroperoxybenzoic acid is added for reaction, and then precipitation, washing and drying are carried out, wherein the mole ratio of the double-bond content in the meta-chloroperoxybenzoic acid to the double-bond content in the phenyl silicone rubber is 1 to (1.1-1.5). The phenyl silicone rubber with the vinyl content being 5-40% can be efficiently and successfully epoxidized, and the epoxidation conversion rate can reach 90% or above. Compared with existing phenyl silicone rubber epoxidation modificationprocesses, the reaction time is successfully shortened by 25%, the dissolution concentration of the phenyl silicone rubber is successfully increased, and efficiency is greatly improved. More importantly, using of a trichloromethane dissolvent which is highly toxic and can corrode metal containers is omitted, and possibility is provided for industrialization of phenyl silicone rubber epoxidation.The reaction process is mild, and less side reaction occurs.

Description

technical field [0001] The invention relates to the technical field of silicone rubber, in particular to a preparation method of epoxidized phenyl silicone rubber. Background technique [0002] After the epoxidation functional group is introduced into the side chain structure of phenyl silicone rubber, it can destroy the low-temperature crystallization of silicone rubber itself, improve its low-temperature performance, increase the rigidity of the main chain of silicone rubber, and increase the thermal stability of silicone rubber in a nitrogen atmosphere. Decomposition temperature, improve its high temperature resistance. At the same time, the introduction of epoxidized functional groups can also endow epoxidized phenyl silicone rubber with better interfacial interaction with fumed silica and improve its physical and mechanical properties. Most importantly, as the degree of epoxidation increases, the polarity of phenyl silicone rubber also increases, which improves the oil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C08G77/20
CPCC08G77/20C08G77/38
Inventor 赵秀英王美豪张立群卢咏来
Owner BEIJING UNIV OF CHEM TECH
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