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Low-cost environment-friendly method for preparing epoxidized silicone rubber

A silicone rubber and epoxidation technology, which is applied in the field of low-cost and environmentally friendly preparation of epoxidized silicone rubber, can solve the problems of low glass transition temperature, and the preparation method is not suitable for industrial scale-up use, so as to shorten the time and reduce the post-processing time , The effect of simple production process

Active Publication Date: 2020-07-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this regard, some people have carried out research on methyl vinyl silicone rubber by increasing the content of vinyl groups, and then converting vinyl groups into epoxy groups by adding epoxy reagents, which can not only increase the polarity of methyl vinyl silicone rubber Improve oil resistance, and can inhibit the occurrence of crystallization at -50°C and have a lower glass transition temperature, so that silicone rubber can be used at around -100°C, but its preparation method is not suitable for industrial scale-up use

Method used

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  • Low-cost environment-friendly method for preparing epoxidized silicone rubber
  • Low-cost environment-friendly method for preparing epoxidized silicone rubber
  • Low-cost environment-friendly method for preparing epoxidized silicone rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Take 1525g of octamethylcyclotetrasiloxane and 443g of tetramethyltetravinylcyclotetrasiloxane and put them into a 5L strong dispersing reaction kettle, keep the vacuum degree below -0.1MPa at 45°C, and remove water under a small amount of nitrogen gas for 1 After 1 hour, 9.77 g of catalyst and 1.62 g of end-capping agent were added, and water was removed at -0.1 MPa at 45° C. under a small amount of nitrogen for 1.5 hours. After removing water and returning to normal pressure, set the temperature to 110° C., and react for 3 hours under nitrogen atmosphere. After the reaction, set the temperature at 170°C, and at the same time start vacuuming at -0.1MPa under a small amount of nitrogen to remove low molecules, and the time for removing low molecules is 6h. After removal of low molecules, a high vinyl silicone rubber with a vinyl segment molar content of 20% is obtained.

[0055] Take 3g of high-vinyl silicone rubber with a vinyl content of 20% and a 250ml three-necked fl...

Embodiment 2

[0062] Take 1525g of octamethylcyclotetrasiloxane and 443g of tetramethyltetravinylcyclotetrasiloxane and put them into a 5L strong dispersing reaction kettle, keep the vacuum degree below -0.1MPa at 45°C, and remove water under a small amount of nitrogen gas for 1 hours, then add 9.77g of catalyst and 1.62g of end-capping agent, and remove water at -0.1MPa at 45°C for 1.5 hours under a small amount of nitrogen. After removing water and returning to normal pressure, set the temperature to 110° C., and react for 3 hours under nitrogen atmosphere. After the reaction, set the temperature at 170°C, and at the same time start vacuuming at -0.1MPa under a small amount of nitrogen to remove low molecules, and the time for removing low molecules is 6h. After removal of low molecules, a high vinyl silicone rubber with a vinyl segment molar content of 20% is obtained.

[0063] Take 3g of high-vinyl silicone rubber with a vinyl content of 20% and a 250ml three-necked flask, add 100g of ...

Embodiment 3

[0065] Take 1335g of octamethylcyclotetrasiloxane and 662.4g of tetramethyltetravinylcyclotetrasiloxane and put them into a 5L strong dispersing reaction kettle, keep the vacuum degree below -0.1MPa at 45°C, and remove water under a small amount of nitrogen gas After 1 hour, 9.74 g of catalyst and 1.60 g of end-capping agent were added, and water was removed at -0.1 MPa at 45° C. under a small amount of nitrogen for 1.5 hours. After removing water and returning to normal pressure, set the temperature to 110° C., and react for 3 hours under nitrogen atmosphere. After the reaction, set the temperature at 170°C, and at the same time start vacuuming at -0.1MPa under a small amount of nitrogen to remove low molecules, and the time for removing low molecules is 6h. After removal of low molecules, a high vinyl silicone rubber with a vinyl segment molar content of 30% is obtained.

[0066] Take 3g of high-vinyl silicone rubber with a vinyl content of 30% and a 250ml three-necked flas...

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Abstract

The invention discloses a low-cost and environment-friendly method for preparing epoxidized silicone rubber. The method comprises the following steps: taking 1-10 parts of high vinyl silicone rubber,100 parts of an organic peroxy acid poor solvent and 0.5-12 parts of an epoxidation reagent; mixing the high vinyl silicone rubber with the organic peroxy acid poor solvent; after complete dissolution, adding the epoxidation reagent for reaction to obtain epoxidized silicone rubber solution; storing the obtained solution at low temperature to separate out a deoxidation product of the epoxidation reagent and an unreacted epoxidation reagent, then precipitating epoxidized silicone rubber; and performing washing and drying to obtain the epoxidized silicone rubber. The preparation method is more scientific and reasonable, the produced epoxidized silicone rubber has the molecular weight of original high vinyl silicone rubber and is free of gel, the performance of the epoxidized silicone rubberis more stable, the strength of the epoxidized silicone rubber is higher, meanwhile, the production cost is reduced, and the method is more suitable for mass production.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a low-cost and environment-friendly method for preparing epoxidized silicon rubber. Background technique [0002] The silicone rubber molecule has a main chain with a silicon-oxygen bond as the repeating unit, and two organic groups are connected to the silicon atom. Ordinary silica gel mainly has methyl groups and other organic groups. Due to the certain characteristics of the bond length and bond energy of the silicon-oxygen bond, the silicone rubber molecular chain interaction is small, it has good flexibility and thermal stability, and has good high and low temperature resistance. The Si-O bond distance is 1.64A, which is shorter than the sum of the covalent radii (1.76A), implying that the Si-O bond has the characteristics of a partial double bond. In fact, siloxanes are less basic than ethers. However, both the barrier for rotation about the Si-O bond axis and ...

Claims

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Application Information

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IPC IPC(8): C08G77/38C08G77/20
CPCC08G77/20C08G77/38
Inventor 卢咏来乔治刚王美豪张立群岳冬梅赵秀英
Owner BEIJING UNIV OF CHEM TECH
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