Preparation method of modified polymethylsilane

A technology of polymethylsilane and methyldichlorosilane is applied in the field of modification of polymethylsilane, which can solve problems such as introduction obstacles, and achieve the effects of stable storage, high ceramic yield, and stable and controllable process.

Active Publication Date: 2020-08-28
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 broug...

Method used

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  • Preparation method of modified polymethylsilane
  • Preparation method of modified polymethylsilane
  • Preparation method of modified polymethylsilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 19L of dibutyl ether, 15.0kg of methyldichlorosilane, 2.943kg of chloromethylmethyldichlorosilane and 0.7kg of 1,1-dichlorosilylcyclobutane into the feeding tank, mix and set aside.

[0027] 100L reactor, evacuate and replace with nitrogen for 1 to 3 times. Under nitrogen protection, 20 L of dibutyl ether and 7.2 kg of fresh sodium were added to the reactor. Heat the reaction kettle with an oil bath at 110°C until the sodium melts, and stir and reflux for 1 hour to remove the moisture entrained in the butyl ether. The temperature in the reaction kettle is 106-115°C, stirring at 350RPM to form sodium sand.

[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, and drop it in about 2 hours; continue to heat to 110-115°C for 3 hours , and then raised the temperature to 120°C for 3h, and the sodium shrinkage rea...

Embodiment 2

[0036] Add 19L of dibutyl ether, 14kg of methyldichlorosilane, 3.75kg of chloromethylmethyldichlorosilane, and 1.08kg of 1,1-dichlorosilylcyclobutane into the feeding tank, mix and set aside.

[0037] 100L reactor, evacuate and replace with nitrogen for 1-3 times. Under the protection of nitrogen, add 20 L of dibutyl ether to the reactor, add 7.2 kg of fresh sodium, melt the sodium through the 110°C oil bath heating system in the reactor, and stir and reflux for 1 hour to remove the water entrained in the butyl ether. The temperature in the reaction kettle is 106-115°C, stirring at 350RPM to form sodium sand.

[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°C, and drop it in about 2 hours; continue to heat to 110-115°C for 3 hours , and then raised the temperature to 120°C for 3h, and the sodium shrinkage reaction wa...

Embodiment 3

[0046] Add 19L of dibutyl ether, 15.8kg of methyldichlorosilane, 2kg of chloromethylmethyldichlorosilane, and 0.43kg of 1,1-dichlorosilylcyclobutane into the feeding tank, mix and set aside.

[0047] 100L reactor, evacuate and replace with nitrogen for 1 to 3 times. Under the protection of nitrogen, add 20 L of dibutyl ether to the reactor, add 7.2 kg of fresh sodium, use the 110°C oil bath heating system in the reactor to melt the sodium, and stir and reflux for 1 hour to remove the water entrained in the butyl ether. The temperature in the reaction kettle is 106-115°C, stirring at 350RPM to form sodium sand.

[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°C, and drop it in about 2 hours; continue to heat to 110-115°C for 3 hours , and then raised the temperature to 120°C for 3h, and the sodium shrinkage reaction w...

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Abstract

The invention discloses a preparation method of modified polymethylsilane. The invention relates to the technical field of modification of polymethylsilane. According to the preparation method, dibutyl ether is used as a solvent, various chlorosilanes and metal sodium are subjected to sodium condensation reaction firstly, then allyl magnesium chloride alkylation is used for end capping, and thereby a product with uniform molecular weight distribution and stable properties is obtained. The modified polymethylsilane has the advantages of being liquid at normal temperature, low in viscosity and high in ceramic yield.

Description

technical field [0001] The invention relates to the technical field of polymethylsilane modification. Background technique [0002] The silicon carbide polymer ceramic precursor is the key raw material for the preparation of silicon carbide fibers, as the matrix resin for the preparation of silicon carbide-based composite materials by the PIP method, and for the preparation of silicon carbide-based high-temperature resistant bonding, connection, and composite ceramics. Among the many silicon carbide precursors researched and developed at home and abroad, the most mature technology and widely used is Kumada, which is produced by polydimethylsilane (PDMS) through high temperature cracking (about 470°C) invented by Yajima. Rearrangement of polycarbosilane (PCS) obtained. Among them, PDMS is obtained by reductive coupling polycondensation of dimethyldichlorosilane in xylene solvent by excessive molten metal sodium; while the cracking of PDMS requires high temperature or high te...

Claims

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Application Information

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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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