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A kind of synthetic method of thermally curable crosslinked polycarbosilane

A technology of polycarbosilane and synthesis method, which is applied in the field of polycarbosilane synthesis, can solve problems such as difficulty in obtaining pyrolysis ceramic product properties, excellent polycarbosilane, etc., and achieve easy implementation, improved ceramic yield, and simple synthesis method Effect

Active Publication Date: 2017-06-23
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that thermal crosslinking treatment of PCS by introducing crosslinking agent DVB, or endowing PCS with self-curing properties by introducing vinyl groups into PCS, can effectively improve the ceramic yield of pyrolysis products and reduce the impact on the impregnation process. The outflow of the PCS melt is very beneficial, but it is difficult to obtain polycarbosilane with thermal curing crosslinking properties and excellent performance of pyrolytic ceramic products in the existing technology

Method used

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  • A kind of synthetic method of thermally curable crosslinked polycarbosilane
  • A kind of synthetic method of thermally curable crosslinked polycarbosilane
  • A kind of synthetic method of thermally curable crosslinked polycarbosilane

Examples

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Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of PVCS-1 from PCS-1 and Dimethyldivinylsilane (DVS)

[0025] Add PCS-1 and DVS to the autoclave at a weight ratio of 1:0.3, add xylene at a ratio of 10ml / g to xylene / PCS-1 for uniform miscibility, and then add xylene at a ratio of 100ppm (weight of PCS-1 is Calculation basis) Add chloroplatinic acid catalyst, vacuumize and replace high-purity nitrogen, pre-fill nitrogen pressure to 10MPa, heat to 120°C, keep warm for 20 hours, stop the reaction, cool to room temperature, and place the product solution in a distillation device , under the protection of high-purity nitrogen, after heating to 160 ° C to distill off the solvent and unreacted DVS, the light yellow solid product PVCS-1 was obtained.

[0026] The light yellow solid product PVCS-1 of present embodiment gained, record its number average molecular weight In 1951, its molecular weight distribution coefficient The gel permeation chromatography (GPC) figure of raw material PCS-1 and product PVCS-1 is ...

Embodiment 2

[0028] Synthesis of PVCS-2 from PCS-2 and DVS

[0029] Using substantially the same method as in Example 1, LPCS-2 and DVS were co-dissolved in xylene at a ratio of 1:0.4 and then mixed into the autoclave. The reaction conditions different from Example 1 and the characteristics of the product PVCS-2 are shown in the table. 1 and Table 2.

Embodiment 3

[0031] Synthesis of PVCS-3 from PCS-2 and DVS

[0032] Using substantially the same method as in Example 1, LPCS-2 and DVS were co-dissolved in xylene at a ratio of 1:0.5 and then mixed into the autoclave. The reaction conditions different from Example 1 and the characteristics of the product PVCS-3 are shown in the table. 1 and Table 2.

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Abstract

A synthesis method of polycarbosilane capable of being used for thermosetting crosslinking comprises the following steps: taking polycarbosilane used for preparing a composite material as a raw material; placing the polycarbosilane used for preparing the composite material and an organosilan compound containing 2 to 3 -C=C- groups into a reaction vessel; adding dimethyl benzene; mixing uniformly for dissolving; adding a Si-H additive reaction catalyst; vacuumizing; carrying out replacing with high-purity nitrogen; carrying out an Si-H additive reaction under a normal-pressure or high-pressure heating condition and the protection of the high-purity nitrogen. The synthesis method is simple and convenient, and easy to implement; the product PVCS can be used for self-setting crosslinking under an inert atmosphere after being treated at 400 DEG C; the smelting outflow of PCS during heat treatment can be avoided; the ceramic yield can be improved remarkably; the polycarbosilane synthesized according to the synthesize method can be used as a precursor polymer of ceramic-based composite materials such as Cf / SiC, and SiCf / SiC.

Description

technical field [0001] The invention relates to a synthesis method of polycarbosilane, a precursor for preparing silicon carbide-based composite materials, in particular to a synthesis method of thermally curable polycarbosilane. Background technique [0002] Continuous fiber-reinforced ceramic matrix composites are a type of high-tech structural materials that have been developed in recent years and have received much attention. They have the advantages of high temperature resistance, corrosion resistance, high strength and high toughness. Among them, silicon carbide (SiC)-based composite materials such as carbon fiber reinforced silicon carbide (Cf / SiC) and silicon carbide fiber reinforced silicon carbide (SiCf / SiC) composite materials are the most studied, which are mainly used in aerospace nuclear industry and other fields. The main preparation method is the precursor impregnation pyrolysis method (PrecursorInfiltration and Pyrolysis, PIP), which has the advantages of lo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/60C04B35/565
Inventor 宋永才顾喜双苟燕子邵长伟简科王军
Owner NAT UNIV OF DEFENSE TECH
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