A kind of silicon-based carborane polymer and preparation method thereof

The technology of silicon-based carborane and polymer is applied in the field of silicon-based carborane polymer and its preparation, which can solve the problems of high synthesis cost and toxic raw materials in the preparation process, achieve high ceramic yield, and facilitate popularization and application , the effect of excellent heat resistance and oxidation resistance

Active Publication Date: 2020-04-03
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a new type of silicon-based carborane polymer and its preparation method in view of the existing polyborosilazane ceramic precursor preparation process or complex or use of toxic raw materials, and high synthesis costs.

Method used

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  • A kind of silicon-based carborane polymer and preparation method thereof
  • A kind of silicon-based carborane polymer and preparation method thereof
  • A kind of silicon-based carborane polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0081] 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.

[0082] After the reaction is finished...

Embodiment 2

[0106] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0107] 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 86° C., and the reaction time was 48 hours.

[0108] After the reaction is finished...

Embodiment 3

[0126] 1. Synthesis of 1,1′-bisphenylsilyl-2,2′-bis(dimethylhydroxysilyl)biscarborane

[0127] Synthesis of bisphenylsilyl methylene biscarborane is the same as in Example 1.

[0128] Add 71.28 grams of dry tetrahydrofuran and 9.55 grams of bisphenylsiliconyl biscarborane into a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and wait for the solution in the three-necked flask under the condition of an ice bath. The temperature was lowered to 0°C and then 25.50 grams of 1.6M n-butyllithium hexane solution was added dropwise through a constant pressure dropping funnel, the dropping time was 60 minutes, the reaction time was 8 hours, and the reaction temperature was kept below zero. After 8 hours of reaction, a mixed solution of 3.95 grams of dimethylchlorosilane and 35.75 grams of dry tetrahydrofuran was also added dropwise under the condition of an ice bath. The dropwise addition process was 30 minutes, ...

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Abstract

The invention discloses a silicon-based carborane polymer and a preparation method thereof. Specifically, 1,1'-hydrocarbylsilyl-2,2'-bis(dimethylsilyl)biscarborane is used as the reaction raw material to prepare 1,1'-hydrocarbylsilyl-2,2'- Bis(hydroxydimethylsilyl)biscarborane; starting from trivinyltrimethylcyclotrisilazane, reacted with dimethylchlorosilane to obtain 1,3,5‑trimethyl ‑1,3,5‑three[ β ‑(Dimethylchlorosilyl)ethyl]cyclotrisilazane, through polycondensation, the obtained copolymer is reactive, and the polymer can be coated on the surface of carbon fiber to obtain the protection of silicon-based carborane crosslinked polymer Carbon fiber material, the prepared carborane has very excellent heat resistance and oxidation resistance. The silicon-based carborane polymer provided by the invention has simple and convenient preparation process, mild preparation reaction conditions, easy-to-obtain raw materials, and is suitable for industrial scale-up production.

Description

technical field [0001] The invention relates to a silicon-based carborane polymer and a preparation method thereof, belonging to the technical field of fine chemicals and high-temperature-resistant polymer synthesis. [0002] technical background [0003] As a new type of high-performance ceramic material, SiBCN ceramics are better than SiC and Si 3 N 4 , BN and other binary system ceramics and SiCN, SiCO and other ternary system ceramics have better high temperature stability and oxidation resistance, and the high temperature stability of some SiBCN ceramics can even reach 2000 °C. Because of this, the research on SiBCN ceramics as ceramic coatings, ceramic fibers, and ceramic matrix composites has been in the ascendant for decades. In addition, it can also be used as an adhesive for ceramics, multi-layer connection of computer chips, etc., so it is widely used in information, electronics, aerospace and military fields. [0004] SiBCN ceramics are mainly obtained by pyrol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/54C04B35/58C07F7/21C07F7/08
CPCC04B35/58C04B2235/483C04B2235/486C07F7/0836C07F7/21C08G77/54
Inventor 童德进李战雄褚吉成周莹杨录新阎四海戴礼王海朋
Owner SUZHOU UNIV
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