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A kind of preparation method of modified polymethylsilane

A polymethylsilane modification technology, applied in the field of polymethylsilane modification, can solve problems such as introduction barriers

Active Publication Date: 2022-03-25
内蒙古三友化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in the previous PMS and its modification process, in order to completely react the Si-Cl bond, an excessive amount of metal sodium was often used. On the one hand, the residual metal sodium brought certain safety risks and costs to the post-processing, and at the same time, it brought a certain safety risk and cost to vinyl, etc. The introduction of carbon-carbon unsaturated bonds brings certain obstacles

Method used

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  • A kind of preparation method of modified polymethylsilane
  • A kind of preparation method of modified polymethylsilane
  • A kind of preparation method of modified polymethylsilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 19 L of dibutyl ether, 15.0 kg of methyl dichlorosilane, 2.943 kg of chloromethyl methyl dichlorosilane and 0.7 kg of 1,1-dichlorosilyl cyclobutane were added to the feeding tank, and they were mixed for later use.

[0027] A 100L reaction kettle was evacuated and replaced with nitrogen for 1 to 3 times. Under nitrogen protection, 20L of dibutyl ether was added to the reaction kettle, and 7.2kg of fresh sodium was added. The water was removed by heating the built-in 110°C oil bath in the reactor until the sodium melted, and stirring and refluxing for 1 hour to remove the entrained water in the butyl ether. The temperature in the reaction kettle is 106-115 DEG C, and the sodium sand is formed by stirring at a rotating speed of 350 RPM.

[0028] Then slowly add the above mixture in the feeding tank to the reaction kettle through the dropping funnel for reaction, while controlling the temperature of the mixture in the reaction kettle at 106-115 °C, the addition is complet...

Embodiment 2

[0036] 19L of dibutyl ether, 14kg of methyldichlorosilane, 3.75kg of chloromethylmethyldichlorosilane, and 1.08kg of 1,1-dichlorosilylcyclobutane were added into the feeding tank, and they were mixed for later use.

[0037] 100L reaction kettle, evacuated and replaced with nitrogen for 1-3 times. Under nitrogen protection, 20 L of dibutyl ether was added to the reaction kettle, 7.2 kg of fresh sodium was added, and the sodium was melted by heating the system in an oil bath at 110° C. in the reaction kettle, and stirred and refluxed for 1 hour to remove the water entrained in the butyl ether. The temperature in the reaction kettle is 106-115 DEG C, and the sodium sand is formed by stirring at a rotating speed of 350 RPM.

[0038] Then slowly add the above mixture in the feeding tank to the reaction kettle through the dropping funnel for reaction, while controlling the temperature of the mixture in the reaction kettle at 106 ~ 115 ℃, the dropwise addition is completed in about 2...

Embodiment 3

[0046] 19L of dibutyl ether, 15.8kg of methyldichlorosilane, 2kg of chloromethylmethyldichlorosilane, and 0.43kg of 1,1-dichlorosilylcyclobutane were added into the feeding tank, and they were mixed for later use.

[0047] A 100L reaction kettle was evacuated and replaced with nitrogen for 1 to 3 times. Under nitrogen protection, 20 L of dibutyl ether was added to the reaction kettle, 7.2 kg of fresh sodium was added, the sodium was melted by the 110° C. oil bath heating system in the reaction kettle, and the water entrained in the butyl ether was removed by stirring and refluxing for 1 hour. The temperature in the reaction kettle is 106-115 DEG C, and the sodium sand is formed by stirring at a rotating speed of 350 RPM.

[0048] Then slowly add the above mixture in the feeding tank to the reaction kettle through the dropping funnel for reaction, while controlling the temperature of the mixture in the reaction kettle at 106 ~ 115 ℃, the dropwise addition is completed in about ...

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Abstract

A preparation method of modified polymethylsilane, which relates to the technical field of modification of polymethylsilane. The present invention uses dibutyl ether as a solvent, first performs sodium condensation reaction with various chlorosilanes and metal sodium, and then uses dibutyl ether to Propylmagnesium chloride is alkylated for capping to obtain a product with relatively uniform molecular weight distribution and stable properties. The obtained modified polymethylsilane has the advantages of being liquid at room temperature, low viscosity and high ceramic yield.

Description

technical field [0001] The present invention relates to the technical field of modification of polymethylsilane. Background technique [0002] Silicon carbide polymer ceramic precursor is a key raw material for the preparation of silicon carbide fiber, as the matrix resin for the preparation of silicon carbide matrix composites by PIP method, and for the high temperature bonding and connection of silicon carbide matrix and the preparation of multiphase ceramics. Among the many silicon carbide precursors researched and developed at home and abroad, the most mature and widely used one is the Kumada produced by polydimethylsilane (PDMS) invented by Yajima through high temperature cracking (about 470 ℃). Rearranged polycarbosilane (PCS). Among them, PDMS is obtained by the reductive coupling polycondensation of dimethyldichlorosilane by excess molten metal sodium in xylene solvent; and the cracking of PDMS requires high temperature or high temperature and pressure, and there ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 李辉宁张才山张扬李明成
Owner 内蒙古三友化学有限公司
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