Preparation method of polycarbosilane ceramic precursor material

A technology of ceramic precursor and polycarbosilane, which is applied in the direction of additive processing, textile and papermaking, fiber chemical characteristics, etc., can solve problems such as difficult to guarantee polycarbosilane, achieve high pass rate of process, reduce production cost, and equipment and the effect of low process requirements

Active Publication Date: 2020-12-11
福建立亚化学有限公司
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Problems solved by technology

[0011] To sum up: Manufacture polycarbosilane according to the usual synthesis process to control the reaction temperature and holding time, it is difficult to ensure that the content o

Method used

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  • Preparation method of polycarbosilane ceramic precursor material
  • Preparation method of polycarbosilane ceramic precursor material
  • Preparation method of polycarbosilane ceramic precursor material

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Embodiment

[0043] refer to Figure 4 , Figure 5 , Figure 6 and Figure 7 , a polycarbosilane ceramic precursor material preparation method, comprising the following steps:

[0044] (1) Put polydimethylsilane in a high-pressure synthesis kettle, repeatedly evacuate and replace the gas in the kettle with high-purity nitrogen, and circulate nitrogen, control the temperature at 380°C±5°C, and keep the polydimethylsilane under normal pressure. Carbosilane cracking for 2 hours, then add nitrogen to keep the pressure at 0.5Mpa, continue to heat up to 440°C, react for 6 hours, control the pressure at (0.44-0.50)Mpa, and cool to obtain a polycarbonate with a softening point of 190-195°C Crude silane. Wherein, the obtained polycarbosilane crude product has a high molecular weight part of 6% to 8%, and a medium molecular weight part of 68% to 71%; the molecular weight distribution of the polycarbosilane crude product is shown in Figure 6 .

[0045] (2) Grinding the crude polycarbosilane, a...

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Abstract

The invention discloses a preparation method of a polycarbosilane ceramic precursor material. The method comprises the following steps: putting polydimethylsilane into a high-pressure synthesis kettle, repeatedly vacuumizing, replacing gas in the kettle with high-purity nitrogen, introducing nitrogen, controlling the temperature, cracking polycarbosilane under normal pressure, adding nitrogen to maintain the pressure, continuing heating to react, controlling a certain pressure, and cooling to obtain a polycarbosilane crude product; grinding and screening the polycarbosilane crude product to form polycarbosilane powder; soaking the screened polycarbosilane powder with absolute ethyl alcohol, fully stirring and filtering to collect polycarbosilane insoluble in the absolute ethyl alcohol; dissolving polycarbosilane which is insoluble in n-propanol by using xylene, introducing nitrogen during reaction, and fully stirring to obtain a mixed solution; heating the mixed solution under the protection of nitrogen, and cooling to obtain a polycarbosilane finished product of which the softening point is 200-210 DEG C, the high molecular weight part is 8-12% and the medium molecular weight partis more than 70%.

Description

technical field [0001] The invention relates to the technical field of ceramic precursor materials, in particular to a method for preparing a polycarbosilane ceramic precursor material. Background technique [0002] Polycarbosilane (PCS) is the key raw material for 3D printing of silicon carbide fibers and silicon carbide components. Melt spinning of silicon carbide fibers and 3D printing of silicon carbide components have high requirements on the molecular weight distribution and softening point of PCS. The increase of PCS softening point is basically linear with the increase of polymer content. With the increase of polymer content, the softening point of PCS increases, which is mainly due to the increase of PCS molecular weight due to the condensation between molecules. Since the PCS molecules are in the shape of oblate spheroids, the condensation between molecules will inevitably lead to the increase of branched and cross-linked structures in the molecules, resulting in t...

Claims

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Application Information

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IPC IPC(8): C08G77/60D01F9/10C04B35/571B33Y70/00
CPCC08G77/60D01F9/10C04B35/571B33Y70/00Y02E60/10
Inventor 贺卫东陈福来陈柏林肖美敏张佚林张宗清刘燕鹏
Owner 福建立亚化学有限公司
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