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Silica-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: 2017-09-08
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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  • Silica-based carborane polymer and preparation method thereof
  • Silica-based carborane polymer and preparation method thereof
  • Silica-based carborane polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0080] 1. Synthesis of 1,1'-bisphenylsilylmethylene-2,2'-bis(dimethylhydroxysilyl)biscarborane

[0081] Add 135 grams of dehydrated tetrahydrofuran and 13.2 grams of diphenyldichlorosilane to a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and then add 25 grams of water through a constant pressure dropping funnel. Ethynyl magnesium bromide Grignard reagent, dripping time is 30 minutes, set the reaction temperature to 40℃, and the reaction time is 4 hours. At the same time, configure a mixed solution of 6.2 grams of decaborane, 78 grams of acetonitrile and 178 grams of tetrahydrofuran, reaction 4 After hours, the same was dripped through a constant pressure dropping funnel, and the dripping time was 30 minutes. After the dripping, the reaction temperature was adjusted to 80°C, and the reaction time was 48 hours.

[0082] After the reaction is over, add a prepared mixed solution of 110 grams of acetonitrile,...

Embodiment 2

[0106] 1. Synthesis of 1,1'-bisphenylsilylmethylene-2,2'-bis(dimethylhydroxysilyl)biscarborane

[0107] Add 135 grams of dehydrated tetrahydrofuran and 13.2 grams of diphenyldichlorosilane to a 1000ml three-necked flask. After setting up the experimental device, first pass nitrogen to remove the air in the device, and then add 25 grams of water through a constant pressure dropping funnel. Ethynyl magnesium bromide Grignard reagent, dripping time is 30 minutes, set the reaction temperature to 40℃, and the reaction time is 4 hours. At the same time, configure a mixed solution of 6.2 grams of decaborane, 78 grams of acetonitrile and 178 grams of tetrahydrofuran, reaction 4 After hours, the same was dripped through a constant pressure dropping funnel, and the dripping 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 over, add a prepared mixed solution of 110 grams of aceto...

Embodiment 3

[0126] 1. Synthesis of 1,1'-bisphenylsilylene-2,2'-bis(dimethylhydroxysilyl)biscarborane

[0127] The synthesis of bisphenylsilylmethylene biscarborane is the same as in Example 1.

[0128] Add 71.28 grams of dry tetrahydrofuran and 9.55 grams of bisphenylsilylene dicarborane to 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 ice bath conditions. The temperature was lowered to 0°C, and then 25.50 g of 1.6M n-butyl lithium 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 g of dimethylchlorosilane and 35.75 g of dry tetrahydrofuran was added dropwise under the same ice bath. The dropping process lasted for 30 minutes. After reacting for 2 hours, it was trans...

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Abstract

The invention discloses a silica-based carborane polymer and a preparation method thereof. The preparation method specifically comprises the following steps: preparing 1,1'-alkylsilylidene-2,2'-bis(hydroxydimethylsilyl)bicyclaborane from a reaction raw material, namely 1,1'-alkylsilylidene-2,2'-bis(dimethylsilyl)bicyclaborane; and reacting by virtue of trivinyl trimethyl cyclotrisilazane as an initial raw material and dimethylchlorosilane, so as to obtain 1,3,5-trimethyl-1,3,5-tris[beta-(dimethylsilyl)ethyl]cyclotrisilazane, carrying out condensation polymerization so as to obtain a polymer with reactivity, and coating the surface of carbon fiber with the polymer so as to obtain a silica-based carborane cross-linked polymer protected carbon fiber material. Prepared carborane has very excellent heat resistance and anti-oxidation function. A preparation process of the silica-based carborane polymer is simple and convenient, reaction conditions are mild, and the raw materials are easily available; and the preparation process is suitable for enlarged production.

Description

Technical field [0001] The invention relates to a silicon-based carborane polymer and a preparation method thereof, and belongs to the technical field of fine chemicals and high temperature resistant polymer synthesis. [0002] technical background [0003] SiBCN ceramics, as a new type of high-performance ceramic material, is better than SiC, Si 3 N 4 , BN and other binary system ceramics and SiCN, SiCO and other ternary system ceramics have more excellent high temperature stability and oxidation resistance, some SiBCN ceramics high temperature stability can even reach 2000 ℃. Because of this, SiBCN ceramics have been used as ceramic coatings, ceramic fibers, and ceramic matrix composite materials for decades. In addition, it can 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 high temperature cracking of organic-inorga...

Claims

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Application Information

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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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