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Synthetic method of polycarbosilane

A technology of polycarbosilane and synthesis method, which is applied in the field of preparing polycarbosilane, can solve the problems of low yield and poor thermal stability of polycarbosilane synthesis, and achieve the effect of mild conditions and simple post-treatment method

Inactive Publication Date: 2016-05-11
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a synthesis method of polycarbosilane in order to solve the technical problems of low yield and poor thermal stability of existing synthetic polycarbosilane

Method used

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  • Synthetic method of polycarbosilane
  • Synthetic method of polycarbosilane
  • Synthetic method of polycarbosilane

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specific Embodiment approach 1

[0018] Specific embodiment one: the synthetic method of a kind of polycarbosilane of this embodiment is carried out according to the following steps:

[0019] 1. In the autoclave, add 50g of polydimethylsilane and 0.5g of 100-200-mesh iron powder, replace the autoclave with carbon dioxide gas 3-6 times, start heating, and raise the temperature to 260°C-270°C within 1 hour, and Keep warm for 3 to 3.5 hours until the pressure in the autoclave is 1MPa, then cool down to 50°C to 60°C, release the gas in the autoclave, and then reheat, within 4 hours to 480°C to 560°C, at a pressure of 4.8 MPa~6MPa, temperature 480℃~560℃, keep warm for 9h~11h, then cool to room temperature;

[0020] 2. Dissolve the reaction product obtained in step 1 in 100ml of xylene, filter to obtain a clear and transparent solution, add 100ml of ethanol solution, and precipitate a brown-yellow solid product to obtain polycarbosilane.

specific Embodiment approach 2

[0021] Specific embodiment two: the difference between this embodiment and specific embodiment one is that in step one, the temperature is raised to 515° C. within 4 hours. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0022] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in Step 1, the temperature is raised to 500° C. within 4 hours. Others are the same as those in the first or second embodiment.

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Abstract

The invention discloses a synthetic method of polycarbosilane, and relates to a method for preparing polycarbosilane by using polydimethylsilane as a raw material. The invention aims to solve the technical problems that the yield of polycarbosilane is low and the heat stability is poor in the prior art. The method comprises a first step of adding polydimethylsilane and iron powder into an autoclave, replacing carbon dioxide gas 3 to 6 times in the autoclave, heating, raising the temperature within one hour and maintaining the temperature, heating again after reducing the temperature, maintaining the temperature, and cooling to a room temperature; a second step of dissolving a product obtained in the first step into a certain amount of xylene, filtering to obtain a clear and transparent solution, adding the same volume of ethanol solution, separating out a claybank solid product so as to obtain the polycarbosilane. According to the method disclosed by the invention, the polydimethylsilane is transformed into polycarbosilane at a high temperature and high pressure; the obtained polycarbosilane is narrow in molecular weight distribution and good in heat stability. The yield of the polycarbosilane can reach 52.8 percent. The invention belongs to the synthetic field of polycarbosilane.

Description

technical field [0001] The invention relates to a method for preparing polycarbosilane from polydimethylsilane. Background technique [0002] With the rapid development of science and technology, more and more new materials have entered various fields of people's lives. Silicon carbide fiber is a new type of ceramic fiber. Compared with carbon fiber, it has better performance in high temperature resistance and oxidation resistance. It has broad application prospects in some high-tech fields such as aerospace, aviation, weapons, ships and nuclear industries. . [0003] The synthesis methods of silicon carbide fibers include chemical vapor deposition method, micropowder sintering method, carbon fiber thermal reduction method, and precursor method. Among them, the precursor method has two outstanding advantages: 1. The production process is relatively simple and has been industrialized; 2. The fiber performance is good, and the performance improvement potential through modifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 徐虹李博弘王超曹先启杨杰陈泽明李淑辉李猛梅立鑫单雯妍吕宏飞白雪峰
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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