Carborane ceramic precursor system and preparation method and application thereof

A ceramic precursor, carborane technology, applied in the fields of carbon fiber, textile and papermaking, fiber processing, etc., can solve the problems of poor operability, difficult industrialization, and highly toxic intermediate organoborane.

Active Publication Date: 2017-08-11
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when this method is used to prepare precursor compounds, the intermediate organobor

Method used

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  • Carborane ceramic precursor system and preparation method and application thereof
  • Carborane ceramic precursor system and preparation method and application thereof
  • Carborane ceramic precursor system and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0093] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0094]Add 135 grams of dehydrated tetrahydrofuran and 13.2 grams of diphenyldichlorosilane into a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and then drop 25 grams of diphenyl dichlorosilane through a constant pressure dropping funnel. Ethynylmagnesium bromide Grignard reagent, the dropping time is 30 minutes, the setting reaction temperature is 40°C, and the reaction time is 4 hours. At the same time, a mixed solution of 6.2 grams of decaborane, 78 grams of acetonitrile and 178 grams of tetrahydrofuran is prepared, and reaction 4 Hours later, it was also added dropwise through a constant pressure dropping funnel, and the dropwise addition time was 30 minutes. After the dropwise addition, the reaction temperature was adjusted to 80° C., and the reaction time was 48 hours. After the reaction is finished, add a pr...

Embodiment 2

[0119] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0120] Add 135 grams of dehydrated tetrahydrofuran and 13.2 grams of diphenyldichlorosilane into a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and then drop 25 grams of diphenyl dichlorosilane through a constant pressure dropping funnel. Ethynylmagnesium bromide Grignard reagent, the dropping time is 30 minutes, the setting reaction temperature is 40°C, and the reaction time is 4 hours, simultaneously configure 6.2 grams of decaborane, a mixed solution of 78 grams of acetonitrile and 178 grams of tetrahydrofuran, react After 4 hours, it was also added dropwise through a constant pressure dropping funnel, and the dropwise addition time was 30 minutes. After the dropwise addition, the reaction temperature was adjusted to 86° C., and the reaction time was 48 hours. After the reaction is finished, add a prepared mixe...

Embodiment 3

[0137] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0138] Add 135 grams of dehydrated tetrahydrofuran and 13.2 grams of diphenyldichlorosilane into a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and then drop 25 grams of diphenyl dichlorosilane through a constant pressure dropping funnel. Ethynylmagnesium bromide Grignard reagent, the dropping time is 30 minutes, the setting reaction temperature is 40°C, and the reaction time is 4 hours, simultaneously configure 6.2 grams of decaborane, a mixed solution of 78 grams of acetonitrile and 178 grams of tetrahydrofuran, react After 4 hours, it was also added dropwise through a constant pressure dropping funnel, and the dropwise addition time was 30 minutes. After the dropwise addition, the reaction temperature was adjusted to 80° C., and the reaction time was 48 hours. After the reaction is finished, add a prepared mixe...

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Abstract

The invention discloses a carborane ceramic precursor system and a preparation method and application thereof. Particularly, 1, 1'-silicon alkyl methylene-2, 2'-bis(silicon dimethyl) biscarborane is used as a reaction raw material, and 1, 1'-silicon alkyl methylene-2, 2'-bis(hydroxyl silicon dimethyl) biscarborane is prepared; triethylene trimethyl ring trisilazane is used as an initial raw material and reacted with dimethyl chlorosilane to obtain 1, 3, 5-trimethyl-1, 3, 5-tri[(i)beta(/i)-( dimethyl chlorine silicon) ethyl] cyclotrisiloxane is obtained; then the novel carborane ceramic precursor is prepared. The precursor takes cyclo-silazane as a framework support, and is provided with a cross-linked network structure; thus the precursor has very good ceramic yield in further crosslinking process; therefore, a compact ceramic coating can be formed on the surface of the carbon fiber. The preparation method has the advantages of simple preparation technique, mild reaction condition, and easily-obtained raw materials; the carborane ceramic precursor system is applicable to the industrial amplifying production. The heat resistance and the oxidization resistance of the carbon fiber after coating treatment are very excellent.

Description

technical field [0001] The invention relates to a carborane ceramic precursor system and its preparation method and application, and belongs to the field of preparation and application of high temperature resistant polymers and composite materials. Background technique [0002] Carbon fiber has high specific strength, high specific stiffness, good chemical stability, and excellent thermal performance, so it is widely used as a reinforcing material in ceramic matrix composites. However, carbon fibers will be oxidized by air above 400 °C and have poor interface bonding with the ceramic matrix, which limits the application of carbon fiber reinforced ceramic matrix composites. In order to solve these problems, it is generally necessary to modify the surface of carbon fiber, and the common method is to prepare a coating on its surface. [0003] The methods for preparing carbon fiber surface coatings mainly include chemical vapor deposition, in-situ reaction, electroplating, and ...

Claims

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Application Information

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IPC IPC(8): C08G77/54C08G77/06C08G77/08D06M15/643C04B35/515D06M101/40
CPCC04B35/515C08G77/06C08G77/08C08G77/54D06M15/643D06M2101/40
Inventor 童德进李战雄周莹杨录新赵卓安阎四海戴礼王海朋
Owner SUZHOU UNIV
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