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Preparation method of polyborocarbosilane

A technology of carbosilane and polyboron, which is applied in the field of preparation of polyborocarbosilane, which can solve the problems of limited boron element, high corrosion resistance requirements, and inability to obtain polyborosilane with high boron content.

Active Publication Date: 2021-01-22
浙江华茂航天科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Sylramic fiber is a typical boron-containing fiber, and its preparation process is varied. First, boron is introduced through a boron-containing atmosphere without melting during the preparation process. The disadvantages are obvious: the boron-containing atmosphere requires high corrosion resistance of equipment, and the treatment of toxic waste is also a problem
The second preparation process uses a boron-containing precursor, which has obvious disadvantages: the polyborosilazane precursor itself is extremely easy to hydrolyze and oxidize, and the synthesis of the precursor and the entire fiber preparation process must be completed in an anhydrous and oxygen-free environment. Its platform construction and production costs are extremely high
The disadvantages are obvious: boron is introduced through the dehydrogenation reaction of silicon-hydrogen bonds and boron-hydrogen, silicon-hydrogen bonds are consumed to obtain silicon-boron bonds, and the boron-containing polycarbosilane has a low silicon-hydrogen content. In the final analysis, it is due to the silicon-hydrogen content of polycarbosilane Low (0.58mol / 100g), this method is limited by the silicon hydrogen content, the boron element introduced is limited, and high boron content polyborosilane cannot be obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] A preparation method of polyborocarbosilane, comprising the following steps:

[0060] Step 1, synthesize the first raw material,

[0061] Carried out in an autoclave, the reaction pressure is 12Mpa, the liquid polycarbosilane with a molecular weight of 300 and a silicon-hydrogen bond content of 0.7mol / 100g is miscible with 48.96g of tetravinylsilane, and after reacting at 90°C for 300h, 8.16g is removed by vacuum distillation Tetravinylsilane, wherein the catalyst is 880ppm of chloroplatinic acid to obtain the first raw material containing silane of -C=C, the molecular weight of the first raw material is 368, and the vinyl content in the first raw material is 0.9mol .

[0062] Step 2, synthesizing the first intermediate product;

[0063] Obtain the first intermediate product through olefin metathesis reaction with 100g of the first raw material and the second raw material;

[0064] In the olefin metathesis reaction, the reaction temperature is 30°C, and the reaction ...

Embodiment 2

[0073] A preparation method of polyborocarbosilane, comprising the following steps:

[0074] Step 1, synthesize the first raw material,

[0075] Carried out in an autoclave, the reaction pressure is 12Mpa, the liquid polycarbosilane with a molecular weight of 300 and a silicon-hydrogen bond content of 0.7mol / 100g is miscible with 114.24g of tetravinylsilane, and after reacting at 90°C for 600h, 19.04g is removed by vacuum distillation Tetravinylsilane, wherein the catalyst is 10000ppm of chloroplatinic acid to obtain a first raw material containing -C=C, the molecular weight of the first raw material is 434, and the vinyl content in the first raw material is 2.1mol.

[0076] Step 2, synthesizing the first intermediate product;

[0077] Obtain the first intermediate product through olefin metathesis reaction with 100g of the first raw material and the second raw material;

[0078] The olefin metathesis reaction was carried out in an autoclave at a reaction temperature of 160° C...

Embodiment 3

[0087] A preparation method of polyborocarbosilane, comprising the following steps:

[0088] Step 1, synthesize the first raw material,

[0089] 100g of liquid polycarbosilane with a molecular weight of 380 and a viscosity of 32cp and a silicon-hydrogen bond content of 0.7mol / 100g (polydimethylsilane pyrolyzed, can refer to: Wang Yanqiao, Song Yongcai. Vinyl-containing liquid polycarbosilane The structure and performance characterization of [J]. Silicone materials, 2010 (02): 20-23.) After reacting with 11.2g dimethyldivinylsilane at 20°C for 50h, the unreacted dimethyldivinylsilane was distilled off under reduced pressure to remove the unreacted dimethyldivinylsilane 0.2 g of vinyl silane, wherein the catalyst is 1 ppm of chloroplatinic acid to obtain the first raw material of silane containing -C=C, the molecular weight of the first raw material is 405, and the viscosity is 35 cp;

[0090] Step 2, synthesizing the first intermediate product;

[0091] Obtaining the first in...

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Abstract

The invention provides a preparation method of polyborocarbosilane. The method comprises the steps of firstly, synthesizing a first raw material of silane containing -C=C; adding a certain amount of catalyst into the first raw material and a second raw material, and performing olefin metathesis reaction to obtain a first intermediate product, wherein the second raw material contains (X)nSi(Y)m, wherein X is CH2=CH-CH2- or CH2=CH-, and Y is at least one of Cl, Br, I and alkoxy; adding a reducing agent into the first intermediate product, reducing Y into hydrogen atoms by the reducing agent, andremoving solids in the first intermediate product to obtain a second intermediate product; and finally, reacting the second intermediate product with a boron-containing compound to obtain the polyborocarbosilane. The polyborocarbosilane prepared by adopting the method disclosed by the invention is high in boron content, and the boron content can be regulated and controlled.

Description

technical field [0001] The invention relates to a method for preparing silane, in particular to a method for preparing polyborocarbosilane. Background technique [0002] Boron-containing silicon carbide fiber has shown great application potential because of its outstanding high temperature resistance (Li Wenhua, Wang Jun, Wang Hao, etc. Research progress of boron-containing continuous SiC fiber by precursor conversion method, Aerospace Materials Technology, 2007, 4:5 -7.). [0003] Sylramic fiber is a typical boron-containing fiber, and its preparation process is varied. First, boron is introduced through a boron-containing atmosphere without melting during the preparation process. The disadvantages are obvious: the boron-containing atmosphere requires high corrosion resistance of equipment, and the treatment of toxic waste It is also a problem. The second preparation process uses a boron-containing precursor, which has obvious disadvantages: the polyborosilazane precursor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
CPCC08G77/60
Inventor 顾喜双周永江郏保琪曹义张雄军尚来东蒋博
Owner 浙江华茂航天科技股份有限公司
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