Preparation method and device of liquid polycarbosilane ceramic precursor

A technology of ceramic precursors and polycarbosilane, which is applied in pressure vessels used in chemical processes, pressure vessels/vacuum vessels, etc., can solve the problems affecting the mechanical properties of composite materials, low impregnation efficiency, low density, etc., and achieve excellent flow High impregnation efficiency, high impregnation efficiency, and less air bubble effect

Active Publication Date: 2022-07-15
福建立亚化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chloromethyltrichlorosilane is used as raw material to prepare liquid polycarbosilane, which will overflow a large amount of small molecular gas during cross-linking curing and pyrolysis molding, w

Method used

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  • Preparation method and device of liquid polycarbosilane ceramic precursor
  • Preparation method and device of liquid polycarbosilane ceramic precursor
  • Preparation method and device of liquid polycarbosilane ceramic precursor

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preparation example Construction

[0032] The preparation method of a liquid polycarbosilane ceramic precursor provided by the invention comprises the following steps:

[0033] (1) heating the reaction kettle 1 to 100 ℃~110 ℃, vacuuming to -0.08MPa~-0.095MPa, keeping the temperature for 1h~3h, drying the reaction kettle 1 to remove moisture; then open the nitrogen valve 7 to put the nitrogen in the nitrogen tank 4 The nitrogen is passed into the reaction kettle 1 to replace the air in the reaction kettle 1, after repeated operations three times, the nitrogen is introduced and then cooled to 40 ° C ~ 60 ° C, and the reaction kettle 1 is kept in a slightly positive pressure state.

[0034] (2) successively add tetrahydrofuran, metal magnesium and 1,1,3,3-tetrachloro-1,3-disilazane into the reactor 1, keep the temperature of the reactor at 40 ℃~60 ℃, open the condenser and The stirring device of the reaction kettle of the reaction kettle, while stirring, add the first batch of chlorosilanes, control the temperatur...

Embodiment 1

[0040]The preparation method of a liquid polycarbosilane ceramic precursor provided by the invention comprises the following steps:

[0041] (1) reaction kettle 1 is heated to 100° C., evacuated to -0.08MPaMPa, kept for 1 h, and reaction kettle 1 is dried to remove moisture; then open nitrogen valve 7 to pass nitrogen in nitrogen tank 4 into reaction kettle 1 The air in the reaction kettle 1 was replaced, and after the operation was repeated three times, nitrogen was introduced, and then the temperature was lowered to 40° C., and the reaction kettle 1 was kept in a slightly positive pressure state.

[0042] (2) successively add tetrahydrofuran, metallic magnesium and 1,1,3,3-tetrachloro-1,3-disilazane in the reactor 1, keep the reactor temperature at 40 ° C, open the condenser and the reactor The stirring device of the reaction kettle, while stirring, add the first batch of chlorosilanes, control the temperature of the reaction kettle 1 to be lower than 60 ° C, wait for the re...

Embodiment 2

[0046] The preparation method of a liquid polycarbosilane ceramic precursor provided by the invention comprises the following steps:

[0047] (1) heating the reactor 1 to 105°C, vacuuming to -0.095MPa, keeping the temperature for 2h, drying the reactor 1 to remove moisture; then open the nitrogen valve 7 to pass the nitrogen in the nitrogen tank 4 into the reactor 1 The air in the reaction kettle 1 was replaced, and after repeated operations three times, nitrogen was introduced, and then the temperature was lowered to 40°C to 60°C, and the reaction kettle 1 was kept in a slightly positive pressure state.

[0048] (2) in reactor 1, add tetrahydrofuran, metallic magnesium and 1,1,3,3-tetrachloro-1,3-disilazane successively, keep reactor temperature to be 50 ℃, open condenser and reactor The stirring device of the reaction kettle, while stirring, add the first batch of chlorosilanes, control the temperature of the reaction kettle 1 to be lower than 60 ° C, wait for the reaction t...

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Abstract

The invention discloses a preparation method of a liquid polycarbosilane ceramic precursor, which is characterized by comprising the following steps: drying a reaction kettle, introducing nitrogen to replace air in the reaction kettle, and cooling the reaction kettle to keep the reaction kettle in a micro-positive pressure state; the method comprises the following steps: adding tetrahydrofuran, magnesium metal and 1, 1, 3, 3-tetrachloro-1, 3-disilanebutane into a reaction kettle, then starting a condenser and a stirring device of the reaction kettle, then adding a first batch of chlorosilane, cooling to 40-50 DEG C, then adding a second batch of chlorosilane, maintaining the temperature for full reaction, then continuing to add unsaturated chloroalkane, after dropwise adding is finished, adding a second batch of chlorosilane, and after dropwise adding is finished, adding a third batch of chlorosilane into the reaction kettle; raising the temperature of the reaction kettle to 50-65 DEG C, and stirring to react for 3-10 hours; reducing the temperature of the reaction kettle to 40-50 DEG C, then adding a reducing agent, then heating to 50-65 DEG C, and stirring to react for 5-15 hours; and finally, extracting, drying and distilling to obtain the liquid hyperbranched polycarbosilane ceramic precursor.

Description

technical field [0001] The invention relates to the technical field of ceramic precursor materials, in particular to a preparation method and device for a liquid polycarbosilane ceramic precursor. Background technique [0002] The precursor impregnation and pyrolysis (PIP) process is a process in which a ceramic precursor is used to impregnate a fiber preform, and after cross-linking and curing, it is converted into a ceramic matrix composite material at high temperature. The precursor is the key to the preparation of silicon carbide (SiC) ceramic-based materials: (1) The precursor should have good manufacturability. The raw materials of precursors are cheap and readily available, and organic precursors with specific compositions can be synthesized through molecular design. In order to ensure the purity of the components, the precursor should preferably be in a liquid state. (2) The precursor should be cross-linkable, that is, it contains a certain active group. Only the c...

Claims

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Application Information

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IPC IPC(8): C08G77/60B01J3/03C04B35/571C04B35/622
CPCC08G77/60B01J3/03C04B35/571C04B35/622Y02E60/10
Inventor 郑桦贺卫东陈丽滨杨伟凯
Owner 福建立亚化学有限公司
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