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A kind of multi-temperature zone control method of high molecular weight polycarbosilane bridge synthesis

A polycarbosilane bridge and high molecular weight technology is applied in the multi-temperature zone control field of high molecular weight polycarbosilane bridge combination, can solve the problems of complex process, low actual production efficiency, low cost, etc., and achieves simple process flow, Reduce time cost and economic cost, the effect of short time

Active Publication Date: 2021-06-11
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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  • A kind of multi-temperature zone control method of high molecular weight polycarbosilane bridge synthesis
  • A kind of multi-temperature zone control method of high molecular weight polycarbosilane bridge synthesis
  • A kind of multi-temperature zone control method of high molecular weight polycarbosilane bridge synthesis

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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 high-molecular-weight polycarbosilane bridging synthesis. The method includes synthesis device pretreatment, charging, setting temperature zones, one-time bridging, multiple bridging and obtaining high-molecular-weight polycarbosilane Wait six steps. Compared with the existing preparation method of high molecular weight polycarbosilane, the bridging synthesis method of high molecular weight polycarbosilane provided by the invention has a simple process flow, does not need to use an autoclave, does not need to use a catalyst; at the same time, the multi-temperature polycarbosilane provided by the invention The zone control method can also directly remove low molecules and directly bridge to obtain high-molecular-weight polycarbosilane, which improves production efficiency, and the softening point of the high-molecular-weight polycarbosilane obtained is 250-280°C, and the weight-average molecular weight is 2500-3500 , PDI is 2.0-4.0, and the ceramic yield rate is 60-70% when heated to 1000 ° C in nitrogen, and can be used as a raw material for preparing high-performance silicon carbide fibers.

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 Patents(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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