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Novel polycarbosilane and preparation method thereof

A polycarbosilane, a new type of technology, applied in the field of new ceramic materials, can solve the problems of reducing the high temperature stability of pyrolysis products, unfavorable material processing, large heat release, etc., achieve excellent heat resistance, increase ceramic yield, reduce freedom The effect of carbon content

Active Publication Date: 2012-09-19
AEROSPACE RES INST OF MATERIAL & PROCESSING TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the Si / C of the above silikyne polymers is relatively low, and there is more carbon in the product, which reduces the high temperature stability of the pyrolysis product, and the thermal crosslinking process releases a lot of heat, which is not conducive to material processing.

Method used

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  • Novel polycarbosilane and preparation method thereof
  • Novel polycarbosilane and preparation method thereof
  • Novel polycarbosilane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 500ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 8.0g magnesium chips to the reaction flask, add 50ml tetrahydrofuran to the reaction flask with a syringe; add 100ml tetrahydrofuran, 2.0g allyl chloride and 42.3g chloromethyl alkoxy dichlorosilane to the constant pressure dropping funnel, A mixed solution was formed. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 5.0 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0045] Add 100 ml of petroleum ether, 350 ml of deionized water and 10 ml of concentrated hydrochloric acid (commercial standa...

Embodiment 2

[0049] 1000ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 8.0g of magnesium chips into the reaction flask, add 30ml of tetrahydrofuran into the reaction flask with a syringe; add 200ml of tetrahydrofuran, 1.7g of vinyl chloride and 42.3g of chloromethylalkoxydichlorosilane into the constant pressure dropping funnel to form mixture. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 5.0 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0050] Add 100 ml of petroleum ether, 200 ml of deionized water and 10 ml of concentrated hydrochloric acid (commerci...

Embodiment 3

[0054] 1000ml dry three-neck bottle, equipped with N 2 Import piston, condensation tube, nitrogen outlet piston, constant pressure dropping funnel and electromagnetic force stirring, vacuumize, and replace the air in the system with nitrogen gas, and bake with alcohol lamp to remove adsorbed water. Add 8.0g magnesium chips in the reaction flask, add 80ml tetrahydrofuran into the reaction flask with a syringe; add 300ml tetrahydrofuran, 1.6g propargyl chloride and 42.3g chloromethylalkoxydichlorosilane into the constant pressure dropping funnel, A mixed solution was formed. At 60°C, slowly add the mixed solution dropwise into the mixed system of magnesium chips and tetrahydrofuran under stirring, and continue stirring for 10 h after the dropwise addition is completed. Add 5.0 g of granular lithium aluminum hydride and stir at room temperature for 5-20 hours.

[0055] Add 100 ml of petroleum ether, 500 ml of deionized water and 10 ml of concentrated hydrochloric acid (commerci...

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Abstract

The invention relates to novel polycarbosilane and a preparation method thereof. A polycarbosilane ceramic precursor is prepared by adopting a Grignard reagent coupling method; a molecular structure contains unsaturated groups such as a Si-H bond, C=C and the like; the precursor can be crosslinked and cured at a certain temperature, and has low curing weight loss and high manufacturability; the Si / C ratio in the precursor and the process performance of a precursor product can be adjusted effectively by adjusting the functionality and feed ratio of a chlorosilane monomer serving as a reactant and optimizing reaction conditions; and the obtained product has excellent heat resistance, high ceramic yield, low free carbon content in ceramic and high SiC ceramic phase purity, is suitable for serving as a high-performance SiC ceramic precursor, and can be used for preparing an ultrahigh-temperature ceramic-based composite material submerged substrate as well as high-performance materials such as SiC ceramic coatings, fibers and the like.

Description

technical field [0001] The invention relates to the field of new ceramic materials, and relates to a novel polycarbosilane and a preparation method thereof, in particular to a method for preparing a polycarbosilane polymer ceramic precursor by using a Grignard reagent coupling method. Background technique [0002] SiC ceramics have good high temperature stability and high temperature oxidation resistance, so it has great potential as a high temperature resistant structural material in the fields of aviation, aerospace industry and energy industry. At present, the rapid development of new hypersonic technology aircraft requires the development of new ultra-high temperature and oxidation-resistant ceramic matrix composite materials as soon as possible, so as to provide key material support and material technology reserves for the smooth development of near-space aircraft development. Precursor pyrolysis is an effective method for preparing ultra-high temperature oxidation-resi...

Claims

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Application Information

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IPC IPC(8): C08G77/60C04B35/565
Inventor 胡继东陶孟冯志海周延春刘宏瑞李军平
Owner AEROSPACE RES INST OF MATERIAL & PROCESSING TECH
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