Preparation method of spinnable polycarbosilane precursor material

The technology of polycarbosilane and precursor is applied in the field of preparation of spinning-grade polycarbosilane precursor material, which can solve the problems of unstable softening point and low success rate of spinning-grade polycarbosilane, and achieve moderate viscosity and softening effect. The effect of stable point and lower production cost

Inactive Publication Date: 2019-05-31
福建立亚化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polycarbosilane obtained by this method has a low success rate of spinning grade polycarbosilane, and the softening point is relatively unstable. The softening point is from 180°C to 250°C, and the molecular weight is 800 to 2000

Method used

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  • Preparation method of spinnable polycarbosilane precursor material

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Embodiment

[0026] Containers used in the present invention are as figure 1 As shown, the equipment includes a cracking kettle 1 with a heating device and a stirring device, a synthesis kettle 2 with a stirring device and a heating device, a reflux tank 3, an intermediate liquid receiving tank 4, a buffer tank 5, a vacuum pump 6 and a raffinate receiving tank 7 and And finished product receiving tank 8, nitrogen is connected with pyrolysis kettle 1 through cracking kettle nitrogen valve 10 through pipeline, nitrogen is connected with synthesis kettle 2 through pipeline through nitrogen inlet valve 11 of synthesis kettle, synthesis kettle 2 is through pipeline through reflux valve and reflux The tanks 3 are connected, the intermediate liquid receiving tank 4 is connected with the synthesis kettle 2 through the bottom valve 13 through the pipeline, a constant pressure valve 14 is connected above the synthesis kettle 2, a filter 15 is connected between the synthesis kettle 2 and the buffer ta...

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Abstract

The invention discloses a preparation method of a spinnable polycarbosilane precursor material. The preparation method includes the steps: placing polydimethyl silane into a pyrolysis kettle, openinga vacuum valve of the pyrolysis kettle, turning on a vacuum pump, closing the vacuum valve of the pyrolysis kettle when the pyrolysis kettle is vacuumized to be -0.08 to -0.09Mpa, opening a nitrogen valve of the pyrolysis kettle, leading in nitrogen, enabling the internal pressure of the pyrolysis kettle to be 0.04Mpa and maintaining the pressure for 20-24 hours; vacuumizing the pyrolysis kettle to be lower than -0.09Mpa, turning on a stirring device and a heating device of the pyrolysis kettle, heating the inside of the pyrolysis kettle to reach the temperature of 200 DEG C, keeping the temperature for 1-3 hours, continuously stirring the polydimethyl silane in the pyrolysis kettle at high temperature and low pressure to remove residual solvents of the polydimethyl silane, increasing thetemperature for pyrolysis, transferring the polydimethyl silane to a synthesis kettle and performing synthesis at the high temperature and high pressure to obtain polycarbosilane. A molecular chain inthe prepared polycarbosilane is good in linearity, branches on the molecular chain are fewer and less crossed, the polycarbosilane is moderate in viscosity and good in spinnability, the molecular weight of the prepared polycarbosilane is moderately 800-1300, and the polycarbosilane is the most spinnable.

Description

technical field [0001] The invention relates to the technical field of ceramic precursor materials, in particular to a preparation method of a spinning grade polycarbosilane precursor material. Background technique [0002] Precursor ceramic materials are polymers that can be converted into ceramic materials through chemical synthesis. By making full use of the good machinability of polymers, the polymers are processed and shaped, and then heat treated to obtain advanced ceramics that are difficult to obtain by traditional ceramics. Ceramic material. Such as ceramic fibers, ceramic powders, ceramic films, ceramic matrix composites and porous ceramics. [0003] Polycarbosilane (PCS) is a key raw material for silicon carbide fibers. The melt spinning of silicon carbide fiber has high requirements on the molecular weight distribution and softening point of PCS. Polycarbosilane (PCS) is a brittle organic material, so the spinning performance is poor, not as good as other orga...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60D01F9/10
Inventor 贺卫东郑桦庄佳慧张和生
Owner 福建立亚化学有限公司
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