Synthetic method of spinning grade polyaluminocarbosilane precursor

A technology of polyaluminocarbosilane and polycarbosilane, which is applied in the direction of textiles, papermaking, fiber chemical characteristics, etc., can solve the problems of poor spinning performance, increase the reaction rate, avoid easy breakage, and improve the effect of effective length and toughness

Active Publication Date: 2016-03-09
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a synthetic method of spinning grade polyaluminocarbosilane p...

Method used

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  • Synthetic method of spinning grade polyaluminocarbosilane precursor
  • Synthetic method of spinning grade polyaluminocarbosilane precursor
  • Synthetic method of spinning grade polyaluminocarbosilane precursor

Examples

Experimental program
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Effect test

Embodiment 1

[0044] (1) Put 2.0kg of polydimethylsilane and 2.0L of xylene in a high-pressure reactor, evacuate, replace with nitrogen, repeat three times, then pre-fill 0.5MPa of nitrogen in the kettle, raise the temperature to 420°C, and keep warm After 8 hours, stop the reaction when the final pressure rises to 9MPa, cool to room temperature, filter and distill under reduced pressure after the reaction is completed, to obtain polycarbosilane-1.

[0045] (2) Dissolve 1320g of polycarbosilane in xylene, place the solution in an autoclave, and then add 79.2g of aluminum acetylacetonate. Vacuumize and replace nitrogen three times, then pre-fill nitrogen in the kettle to 1.0MPa, then heat to 300°C for reaction, keep warm for 2 hours, and the pressure at the end of keep warm is 4.3MPa. After the reaction, the mixture was filtered to remove insoluble matter.

[0046] (3) Put the filtrate in a three-necked flask, vacuumize and replace nitrogen three times, then heat to 390°C under the protecti...

Embodiment 2

[0054] (1) Put 2.3kg of polydimethylsilane and 1.5L of toluene in a high-pressure reactor, vacuumize, replace with nitrogen, repeat three times, then pre-fill 0.2MPa of nitrogen in the kettle, raise the temperature to 440°C, and keep warm for reaction After 15 hours, the reaction was stopped when the final pressure rose to 11 MPa, cooled to room temperature, filtered and distilled under reduced pressure after the reaction was completed to obtain polycarbosilane-2.

[0055] (2) Dissolve 1120 g of polycarbosilane in xylene, place the solution in an autoclave, and then add 33.6 g of aluminum acetylacetonate. Vacuumize and replace nitrogen three times, then pre-fill nitrogen in the kettle to 1.5MPa, then heat to 280°C for reaction, keep warm for 5h, and the pressure is 3MPa at the end of keep warm. After the reaction, the mixture was filtered to remove insoluble matter.

[0056] (3) Put the filtrate in a three-necked flask, vacuumize and replace nitrogen three times, then heat to...

Embodiment 3

[0059] (1) Put 1.2kg of polydimethylsilane and 1.5L of xylene in a high-pressure reactor, vacuumize, replace with nitrogen, repeat three times, then pre-fill 2MPa nitrogen in the kettle, raise the temperature to 480°C, and keep it warm for 5h , stop the reaction when the final pressure rises to 15MPa, cool to room temperature, filter after the reaction, and distill under reduced pressure to obtain polycarbosilane-3.

[0060] (2) Dissolve 1140g of polycarbosilane in xylene, place the solution in an autoclave, and then add 91.2g of aluminum acetylacetonate. Vacuumize and replace nitrogen three times, then pre-fill nitrogen in the kettle to 3MPa, then heat to 320°C for reaction, keep warm for 4 hours, and the pressure at the end of keep warm is 5.2MPa. After the reaction, the mixture was filtered to remove insoluble matter.

[0061] (3) Put the filtrate in a three-necked flask, vacuumize and replace nitrogen three times, then heat to 410°C under the protection of nitrogen to rea...

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Abstract

The invention provides a synthetic method of a spinning grade polyaluminocarbosilane precursor. The method is characterized in that polycarbosilane with suitable molecular weight and molecular weight distribution, adopted as a raw material, reacts with aluminum acetylacetonate to prepare the precursor with excellent spinnability.

Description

technical field [0001] The invention relates to the technical field of polyaluminocarbosilane, in particular to a method for synthesizing a spinning grade polyaluminocarbosilane precursor. Background technique [0002] As a high-performance ceramic fiber, SiC fiber has a series of excellent properties such as high temperature resistance, oxidation resistance, wear resistance, corrosion resistance, creep resistance, high tensile strength and good compatibility with ceramic matrix. It is a very The ideal composite reinforcement fiber has broad application prospects in aerospace, aviation, high-performance weaponry and other fields. Due to the introduction of aluminum elements, SiC fibers can be densified during high-temperature sintering. Therefore, the third-generation continuous SiC fibers containing aluminum contain lower content of impurity elements oxygen and free carbon in composition, and have a near-stoichiometric Compared with the elemental composition, it has higher...

Claims

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Application Information

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IPC IPC(8): C08G77/60D01F9/10C04B35/565
CPCC04B35/571C08G77/60D01F9/10
Inventor 苟燕子宋永才王应德王浩王军谢征芳简科
Owner NAT UNIV OF DEFENSE TECH
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