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Multi-temperature-zone control method for bridging synthesis of high-molecular-weight polycarbosilane

A technology of polycarbosilane bridge and high molecular weight, which is applied in the multi-temperature zone control field of high molecular weight polycarbosilane bridge combination, can solve the problems of low cost, complicated process, and low actual production efficiency, and achieve short time and atom economy The effect of good performance, reducing time cost and economic cost

Active Publication Date: 2019-06-11
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a multi-temperature zone control method of high molecular weight polycarbosilane bridge synthesis, which is used to overcome the defects of complex process and low actual production efficiency in the prior art, and realize simple process, high actual production efficiency and low cost

Method used

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  • Multi-temperature-zone control method for bridging synthesis of high-molecular-weight polycarbosilane
  • Multi-temperature-zone control method for bridging synthesis of high-molecular-weight polycarbosilane
  • Multi-temperature-zone control method for bridging synthesis of high-molecular-weight polycarbosilane

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Embodiment 1

[0055] This embodiment provides a multi-temperature zone control method for high molecular weight polycarbosilane bridging synthesis, comprising the following steps:

[0056] S1: Replace the air in the synthesis unit including the gasification temperature zone, rearrangement temperature zone, liquefaction temperature zone, blending temperature zone and bridging temperature zone with nitrogen with a purity ≥ 99.99%;

[0057] S2: Take 100kg of liquid silane and place it in the vaporization temperature zone, and add 5kg of dimethyldivinylsilane into the mixing temperature zone;

[0058] S3: Heating and controlling the temperature in the five temperature zones respectively to realize vaporization of low molecular weight liquid silane, rearrangement of low molecular weight liquid silane, liquefaction of low molecular weight liquid silane, blending of low molecular weight liquid silane and bridging agent and low molecular weight liquid silane The purpose of bridging; the temperature...

Embodiment 2

[0068] This embodiment provides a multi-temperature zone control method for high molecular weight polycarbosilane bridging synthesis, comprising the following steps:

[0069] S1: Replace the air in the synthesis device including the gasification temperature zone, rearrangement temperature zone, liquefaction temperature zone, blending temperature zone and bridging temperature zone with argon with a purity ≥ 99.99%;

[0070] S2: Take 100kg of liquid silane and place it in the vaporization temperature zone, and add 7kg of divinylsilane into the mixing temperature zone;

[0071] S3: Heating and controlling the temperature in the five temperature zones respectively to realize vaporization of low molecular weight liquid silane, rearrangement of low molecular weight liquid silane, liquefaction of low molecular weight liquid silane, blending of low molecular weight liquid silane and bridging agent and low molecular weight liquid silane The purpose of bridging; the temperatures in the ...

Embodiment 3

[0078] This embodiment provides a multi-temperature zone control method for high molecular weight polycarbosilane bridging synthesis, comprising the following steps:

[0079] S1: Replace the air in the synthesis device including the gasification temperature zone, rearrangement temperature zone, liquefaction temperature zone, blending temperature zone and bridging temperature zone with argon with a purity ≥ 99.99%;

[0080] S2: Take 100kg of liquid silane and place it in the vaporization temperature zone, and add 8kg of methyldivinylsilane into the mixing temperature zone;

[0081] S3: Heating and controlling the temperature in the five temperature zones respectively to realize vaporization of low molecular weight liquid silane, rearrangement of low molecular weight liquid silane, liquefaction of low molecular weight liquid silane, blending of low molecular weight liquid silane and bridging agent and low molecular weight liquid silane The purpose of bridging; the temperature in...

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Abstract

The invention discloses a multi-temperature-zone control method for bridging synthesis of high-molecular-weight polycarbosilane. The method comprises the six steps: synthesis device pretreatment, charging, temperature zone setting, one-time bridging, multiple bridging and high-molecular-weight polycarbosilane obtaining. Compared with an existing preparation method of high-molecular-weight polycarbosilane, a bridging synthesis method of high-molecular-weight polycarbosilane, provided by the invention, is simple in process flow and free of a high-pressure autoclave and a catalyst; and meanwhile,by using the multi-temperature-zone control method provided by the invention, low molecules can also be directly removed, high-molecular-weight polycarbosilane can be obtained by direct bridging, theproduction efficiency is increased, and the obtained high-molecular-weight polycarbosilane has the softening point being 250-280 DEG C, the weight-average molecular weight being 2500-3500 DEG C, thePDI being 2.0-4.0 and the ceramic yield being 60-70% when being heated to 1000 DEG C in nitrogen and can be used as a raw material for preparing high-performance silicon nitride fiber.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymer synthesis, in particular to a multi-temperature zone control method for high molecular weight polycarbosilane bridge synthesis. Background technique [0002] Continuous silicon carbide ceramic fibers are key materials in high-tech fields such as aviation, spaceflight and nuclear energy. Polycarbosilane is the main raw material of silicon carbide fiber, which is made into continuous silicon carbide fiber through melt spinning, non-melting and inorganicization. In order to improve production efficiency and reduce costs, the most important thing is to improve the efficiency of non-melting. High-molecular-weight polycarbosilane itself has a relatively large molecular weight. In thermochemical crosslinking, the heat treatment temperature can be increased to improve the non-melting efficiency. The radiation dose can be reduced and the non-melting efficiency can be improved in the irradiat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 邵长伟王军王浩王兵
Owner NAT UNIV OF DEFENSE TECH
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