MarkIII type polycarbosilane and preparation method thereof

A polycarbosilane and polysilane technology, applied in the field of MarkIII type polycarbosilane and its preparation, can solve the problems of unfavorable product performance uniformity, uneven heat transfer in the reaction system, high environmental requirements, and avoid toxicity and environmental pollution. , High synthesis yield, uniform heat transfer effect

Active Publication Date: 2021-09-17
CHANGSHA DAFEI NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following defects in this route: 1, when synthesizing sendon, with dichlorodiphenylsilane and boric acid as starting raw material, reaction process can produce acid hydrogen chloride gas, is unfavorable for environmental protection, simultaneously dichlorodiphenylsilane is easy to hydrolyze , the storage and operation process has relatively high environmental requirements
2. When synthesizing MarkIII PCS, mix and heat Paisone and polydimethylsilane. Since Paisone and polydimethylsilane are both solids, the mixing of solids and solids is not conducive to heat transfer, and it is easy to cause poor heat transfer in the reaction system. Uniformity, which is not conducive to the control of the reaction and the uniformity of product properties

Method used

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  • MarkIII type polycarbosilane and preparation method thereof
  • MarkIII type polycarbosilane and preparation method thereof
  • MarkIII type polycarbosilane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Put diphenylsilanediol and boric acid in a molar ratio of 3:2 into a metal reaction kettle with n-butyl ether added in advance, blow nitrogen, start stirring, heat up to 90°C, carry out reflux reaction for 15 hours, and then close the reflux. Reaction by-product water and solvent n-butyl ether were distilled off, the temperature was raised to 300° C., kept for 1 hour, and the temperature was lowered to obtain polyborondiphenylsiloxane.

[0031] 2. Add the polydimethylsilane powder into the metal reaction kettle, vacuumize the reaction kettle and fill it with nitrogen, repeat at least three times, and finally keep the nitrogen flow at normal pressure, then start stirring, raise the temperature of the system to 400°C, keep it for 2 hours, and get Pyrolysis product liquid polysilane.

[0032] 3. Add polyborondiphenylsiloxane to liquid polysilane at a ratio of 2% by weight, raise the temperature to 350°C in an inert atmosphere, keep it warm for 6 hours, and then cool dow...

Embodiment 2

[0034] 1. Put diphenylsilanediol and boric acid in a molar ratio of 3:2 into the reaction kettle with n-butyl ether added in advance, blow nitrogen, start stirring, heat up to 95°C, carry out reflux reaction for 18 hours, then close the reflux, and distill Remove the reaction by-product water and the solvent n-butyl ether, raise the temperature to 350° C., keep it warm for 1 hour, and cool down to obtain polyboron diphenylsiloxane.

[0035] 2. Add polydimethylsilane powder into the reaction kettle, vacuumize and fill the reaction kettle with nitrogen, repeat at least three times, and finally keep the nitrogen flow at normal pressure, then start stirring, raise the temperature of the system to 420°C, keep it warm for 3 hours, and obtain heat The hydrolysis product is liquid polysilane.

[0036] 3. Add polyborondiphenylsiloxane to liquid polysilane in a proportion of 3% by weight, raise the temperature to 360°C in an inert atmosphere, keep it warm for 7 hours, and then cool down...

Embodiment 3

[0038] 1. Put diphenylsilanediol and boric acid in a molar ratio of 3:2 into the reaction kettle with n-butyl ether added in advance, blow nitrogen, start stirring, heat up to 100°C, carry out reflux reaction for 20 hours, then close the reflux, and distill Remove the reaction by-product water and the solvent n-butyl ether, raise the temperature to 350° C., keep it under vacuum for 1 hour, and cool down to obtain polyborondiphenylsiloxane.

[0039] 2. Add the polydimethylsilane powder into the reaction kettle, vacuumize the reaction kettle and fill it with nitrogen, repeat at least three times, and finally keep the nitrogen flow at normal pressure, then start stirring, raise the temperature of the system to 420°C, keep it for 2 hours, and get the heat The hydrolysis product is liquid polysilane.

[0040]3. Add polyborondiphenylsiloxane to liquid polysilane at a ratio of 3% by weight, raise the temperature to 370°C in an inert atmosphere, keep it warm for 6 hours, and then lowe...

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Abstract

The invention discloses a markIII type polycarbosilane and a preparation method thereof. The preparation method comprises the following steps: adding diphenyl silanediol and boric acid into an organic solvent, carrying out a reflux reaction at 80-110 DEG C in a protective atmosphere for 15-25 h, then distilling to remove water and the organic solvent, heating to 300-400 DEG C, carrying out heat preservation for 0.5-3 h, and cooling to obtain polyboron diphenyl siloxane; adding polydimethylsilane powder into a reaction kettle, heating to 380-450 DEG C in a nitrogen atmosphere, and keeping the temperature for 1-10 hours to pyrolyze the polydimethylsilane powder to obtain liquid polysilane; and then adding the polyboron diphenyl siloxane into the liquid polysilane, and carrying out pyrolysis rearrangement reaction so as to obtain the MarkIII type polycarbosilane. The preparation method is simple, controllable, environment-friendly, pollution-free and safe, the synthesized product is good in quality, required equipment is simple, and the preparation method is completely compatible with an existing process device.

Description

technical field [0001] The invention relates to a MarkIII type polycarbosilane and a preparation method thereof, belonging to the technical field of preparation of ceramic precursors. Background technique [0002] Silicon carbide-based composite materials have a series of advantages such as high temperature resistance, high strength, high modulus, low density, and small thermal expansion coefficient, and have become a new generation of strategic thermal structural materials. It has key and extensive applications in the fields of aviation, aerospace, weapons, ships, armor protection and high-speed braking. The precursor conversion method is the mainstream method for preparing silicon carbide fibers, which mainly includes four steps: precursor synthesis, spinning, non-melting treatment and high-temperature firing. There are mainly two types of continuous silicon carbide fibers prepared at present, namely doped fibers and undoped fibers. The doping path uses the thinking of m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 唐云黄小忠王春齐薛金根刘鹏段世同
Owner CHANGSHA DAFEI NEW MATERIAL TECH CO LTD
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