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Novel carborane- (siloxane or silane)- ethinyl high temperature resistant polymer and its preparation method

A technology of octacarboryl and carborane, which is applied in the field of organic boron polymers, can solve the problems of crosslinking density affecting the flexibility of Si-O bonds, etc., and achieve easy control of reaction conditions, simple process flow, and simple operation process easy effect

Inactive Publication Date: 2006-12-27
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of polymer has a relatively high acetylene content, and the high crosslink density affects the flexibility of the Si-O bond.

Method used

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  • Novel carborane- (siloxane or silane)- ethinyl high temperature resistant polymer and its preparation method
  • Novel carborane- (siloxane or silane)- ethinyl high temperature resistant polymer and its preparation method
  • Novel carborane- (siloxane or silane)- ethinyl high temperature resistant polymer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: Poly[phenylethynyl-bis(methylsilane)-1,7-carborane]

[0052]

[0053]

[0054] (2)

[0055]

[0056] Dissolve 2mmol of phenylacetylene and 1mmol of 1,7-carborane in 14ml of tetrahydrofuran, and slowly add 4mmol of butyllithium reagent dropwise through a constant pressure funnel. After the dropwise addition, react at -40°C for 2 hours. Then, 2 mmol of methyldichlorosilane was dissolved in 4 ml of tetrahydrofuran and added dropwise to phenylethynyllithium and carborane lithium reagents, and reacted at 20° C. for 12 hours after the addition was completed. After the reaction, 20ml of saturated ammonium chloride solution was added to the reaction solution, fully stirred, separated, and the upper oil phase was taken and washed with 20ml of saturated ammonium chloride solution until the pH value was neutral. The water phase obtained twice was extracted with diethyl ether, separated, and the oil phase obtaine...

Embodiment 2

[0057] Embodiment 2: Preparation of poly[phenylethynyl-bis(methylsilane)-1,7-carborane] cured product and ceramic structural material

[0058] The target polymer obtained in Example 1 was cured at 350° C. and 400° C. for 2 hours under the protection of nitrogen to obtain a black cured product. Td of the cured product in nitrogen atmosphere 5 (The thermal decomposition temperature when the weight loss of the resin is 5%) reaches 762°C; the carbon residue rate at 800°C is 94.2%. Td in air atmosphere 5 Over 800°C; the carbon residue rate at 800°C is 95.6%. The cured product is further heated to 1000°C in nitrogen, and the resulting pyrolysis product has a ceramic structure.

Embodiment 3

[0059] Example 3: Poly[naphthynyl-bis(dimethylsilane)-1,7-carborane]

[0060]

[0061] 1.5 mmol of naphthalene acetylene and 1.5 mmol of 1,7-carborane were dissolved in 14 ml of tetrahydrofuran. Add 4.5 mmol of butyllithium reagent dropwise with a constant pressure funnel for 5 minutes, and react at -20°C for 3 hours after the addition is complete. Then 2.25 mmol of dimethyldichlorosilane was dissolved in 5 ml of tetrahydrofuran and added dropwise to the reagents of lithium naphthynyl and lithium carborane, and reacted at -20°C for 10 hours after the addition was completed. After the reaction, add 20ml of saturated ammonium chloride solution into the reaction solution, fully stir, separate the liquids, take the upper oil phase and wash it once with 20ml of saturated ammonium chloride solution until the pH value is neutral. The water phase obtained twice was extracted by adding diethyl ether solvent, separated, and the oil phase obtained was collected and combined, and the ...

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Abstract

The invention discloses a new kind of carborane- silane- phenylacetylene polymer and the method for preparing the same. Said polymer employs methylchlorosilane, phenylacetylene, carborane and organic lithium agent as raw material, anhydrous tetrahydrofuran (THF) as dissolvent and preparing with protection of nitrogen. The invention moderates molar ratio between simple function group ethynyl compound and carborane to easily control molecular weight of polymer, crosslinking density and carborane content, and realizes purpose of adjustable polymer property. The invention is characterized by simple process and easy operation. The prepared polymer forms thermostable thermosetting material with excellent thermal oxidation performance by heat, light and chemical initiation. Said thermosetting material can be produced to ceramic structure by heating on air or inactive gas. The polymer can be used as base resin and thermo-stable coating for advanced complex material and for preparing ceramic pioneer body.

Description

Technical field: [0001] The invention relates to a high temperature resistant polymer, in particular to an organoboron polymer containing carborane, silane or siloxane and ethynyl in the main chain. Its repeating unit is composed of silane (or siloxane)-carborane-silane (or siloxane), and the monofunctional ethynyl compound caps the polymer. The ethynyl group undergoes cross-linking and curing reactions under the action of light or heat to form a three-dimensional network structure. Under the action of high temperature, a ceramic structure is further formed. Background technique: [0002] In 1963, two research groups in the United States discovered B 10 h 12 (CH 3 EN) 2 Reaction with acetylene gives icosahedral carborane (C 2 B 10 h 12 ). Carborane is a three-dimensional superaromatic polyhedral compound composed of boron, carbon, and hydrogen atoms, and its CH group is weakly acidic [PKa (1,2-isomer)=22.0, PKa (1,7-isomer) conformation)=25.6, PKa (1,12-isomer)=26....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/56C04B35/565C09D183/14C09D5/18
Inventor 周权倪礼忠茅祖菊陈建定
Owner EAST CHINA UNIV OF SCI & TECH
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