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A kind of alkyne-terminated branched liquid polysilane impregnating agent and preparation method thereof

A technology of polysilane and impregnating agent, which is applied in the preparation field of the alkyne-terminated branched liquid polysilane impregnating agent, and can solve the problems of reducing the ceramization yield of the impregnating agent, limiting performance, reducing the silicon content of the impregnating agent system, etc.

Active Publication Date: 2021-12-10
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But currently Si-H and Si-CH=CH 2 The introduction of the impregnating agent can increase the cross-linking density of the impregnating agent to a certain extent, but it still needs to be further improved; and relying on the introduction of active monomers and polymers to increase the cross-linking density of the impregnating agent can reduce the silicon content of the impregnating agent system, thereby limiting its performance.
In addition, the commonly used polysilanes are mostly linear, and they are prone to "bite back reaction" to form small cyclic silane molecules during the synthesis and curing process, which greatly reduces the ceramicization yield of the impregnating agent.

Method used

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  • A kind of alkyne-terminated branched liquid polysilane impregnating agent and preparation method thereof
  • A kind of alkyne-terminated branched liquid polysilane impregnating agent and preparation method thereof
  • A kind of alkyne-terminated branched liquid polysilane impregnating agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Anhydrous LiCl, ZnCl 2 Add 500ml four-necked flask, oxygen evacuated nitrogen, magnesium powder were added to the flask and 12.0g of tetrahydrofuran 100ml (THF), methyl vinyl dichlorosilane (0.09mol) 12.69g and vinyltrichlorosilane (0.01mol) 1.62g was dissolved in THF and added to a constant pressure funnel, under conditions of a cold water bath, was slowly added dropwise a tetrahydrofuran solution of the silane, the system controlling the temperature below 15 ℃. After the dropwise addition, the reaction temperature was raised to 70 deg.] C 15H, cooled to room temperature. Under conditions of a cold water bath, slowly added dropwise tetrahydrofuran solution of ethynyl magnesium bromide After completion of the dropwise addition was heated to 70 ℃, the reaction was continued for 4 hours. Filtered off with suction, washed with water desalting the organic phase, dried and distilled to remove the solvent to obtain a capped branched alkynyl polysilane liquid impregnant under redu...

Embodiment 2

[0024] Anhydrous LiCl, ZnCl 2 Add 500ml four-necked flask, oxygen evacuated nitrogen, magnesium powder were added to the flask and 11.0g of tetrahydrofuran 100ml (THF), methyl vinyl dichlorosilane (0.06mol) 9.87g, methyldichlorosilane (0.01mol) 1.15g and vinyltrichlorosilane (0.01mol) 1.62g was dissolved in THF and added to a constant pressure funnel, under conditions of a cold water bath, was slowly added dropwise a tetrahydrofuran solution of the silane, the system controlling the temperature below 15 ℃. After the dropwise addition, the reaction temperature was raised to 70 deg.] C 15H, cooled to room temperature. Under conditions of a cold water bath, slowly added dropwise tetrahydrofuran solution of ethynyl magnesium bromide After completion of the dropwise addition was heated to 70 ℃, the reaction was continued for 6 hours. Filtered off with suction, washed with water desalting the organic phase, dried and distilled to remove the solvent to obtain a capped branched alkynyl po...

Embodiment 3

[0026] Anhydrous LiCl, ZnCl 2 Add 500ml four-necked flask, oxygen evacuated nitrogen, magnesium powder were added to the flask 100ml tetrahydrofuran and 11.5g (toluene), methyl vinyl dichlorosilane (0.08mol) 11.28g and vinyltrichlorosilane (0.01mol) 1.62g was dissolved in toluene and added to a constant pressure funnel, under conditions of a cold water bath, was slowly added dropwise a tetrahydrofuran solution of the silane, the system controlling the temperature below 15 ℃. After the dropwise addition, the reaction temperature was raised to 110 15H deg.] C, cooled to room temperature. Under conditions of a cold water bath, slowly added dropwise tetrahydrofuran solution of ethynyl magnesium bromide After completion of the dropwise addition was heated to 70 ℃, the reaction was continued for 4 hours. Filtered off with suction, washed with water desalting the organic phase, dried and distilled to remove the solvent to obtain a capped branched alkynyl polysilane liquid impregnant unde...

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Abstract

The invention discloses an alkynyl-terminated branched liquid polysilane impregnating agent and a preparation method thereof. The impregnating agent is characterized as an alkynyl-terminated and branched silane-containing liquid polymer. In the present invention, magnesium powder is used as reducing agent, Lewis salt is used as catalyst, dichlorosilane and trichlorosilane are used as silicon source for polymerization reaction, and then acetylene metal compound is used as end-capping agent for reaction to prepare alkynyl-terminated branched liquid polymer. Silane impregnating agent. The process of the invention is simple, safe and easy to operate, and the process conditions are mild and easy to control. The alkynyl-terminated branched liquid polysilane impregnating agent prepared by the present invention is a brown low-viscosity liquid, which is easy to impregnate, can be solidified after impregnation, and has a high ceramic yield and good oxidation resistance, and can be used to prepare C / C‐SiC binary matrix composites.

Description

Technical field [0001] The present invention relates to a capped branched alkynyl polysilane liquid impregnating agent, also relates to a method for preparing the capped branched alkynyl polysilane liquid impregnating agent. Background technique [0002] Polysilane main chain is a polymer composed only of silicon atoms. The special structure so that it has wide application prospects in the photoresist, photon initiator, the waveguide, the nonlinear optical material, and the like. Further, since the polysilane high silicon content, as a ceramic precursor, may be prepared by high-temperature pyrolysis temperature oxidation of silicon carbide ceramic fibers, or preparing a carbon / carbon - silicon carbide composite material to improve the oxidation of carbon / carbon composite material performance. However, as the polysilane composite impregnating agent, on the one hand it requires a potentially reactive groups to increase the ceramic yield, on the other hand it is desirable to hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 齐会民王帆朱亚平郭康康石俊慧
Owner EAST CHINA UNIV OF SCI & TECH