Polyphenylacetylene silicon oxide borane and preparation method thereof

A technology of polyphenylethynylsiloxaborane and alkylboronic acid, which is applied in the field of polyphenylethynylsiloxaborane and its preparation, can solve problems such as difficult molding of high temperature resistant materials, achieve improved thermal oxidation performance, good resistance Thermal oxidation performance, effect of improving thermal oxidation resistance

Active Publication Date: 2011-11-09
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The curing and molding of this material does not require the use of catalysts or initiators. Under heated conditions, the acetylene group in the polymer can undergo a polymerization reaction to solidify the material, which solves the problem of difficult molding of high temperature resistant materials.

Method used

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  • Polyphenylacetylene silicon oxide borane and preparation method thereof
  • Polyphenylacetylene silicon oxide borane and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1: prepare polyphenylethynylsiloxaborane (wherein, R 1 , R 2 C respectively 6 h 5 、C 6 h 5 )

[0021] Under the protection of nitrogen, add 0.025mol phenylboronic acid (3.05g) and 15ml N,N-dimethylformamide to a 100ml three-necked flask, and heat up to 40°C under stirring to completely dissolve phenylboronic acid in the solvent; mol phenyltrichlorosilane (5.3g) and 20ml N, N-dimethylformamide mixed solution dropwise into the solution of phenylboronic acid, the temperature of the system is kept at 100°C ± 5°C; after the dropwise addition, the temperature of the system is controlled at 150℃±5℃, react for 48h. Add a mixed solution of 0.025mol phenylethynyllithium and tetrahydrofuran (the volume ratio of phenylethynyllithium to tetrahydrofuran is 1:5) dropwise into the reaction system, the dropping temperature is controlled at 0°C ± 5°C, and the dropwise addition is completed. The temperature of the system was controlled at 20°C±5°C, and the reaction was c...

Embodiment 2

[0022] Embodiment 2: Preparation of boron-containing phenylethynyl siloxane (wherein, R 1 , R 2 C respectively 6 h 5 、CH 3 )

[0023] Under nitrogen protection, add 0.025mol phenylboronic acid (3.05g) and 15ml n-butyl ether into a 100ml three-necked flask, and heat up to 40°C under stirring to completely dissolve phenylboronic acid in the solvent; 0.03mol methyltrichlorosilane (4.5g) and 25ml of butyl ether mixed solution was dropped into the phenylboronic acid solution, and the system temperature was kept at 90°C±5°C; after the addition, the system temperature was controlled at 65°C±5°C, and the reaction was carried out for 60 hours. Add a mixed solution of 0.04mol phenylethynyllithium and tetrahydrofuran (the volume ratio of phenylethynyllithium to tetrahydrofuran is 1:5) dropwise into the reaction system, and the dropping temperature is controlled at 0°C ± 5°C. After the addition is complete, The temperature of the system was controlled at 20°C±5°C, and the reaction wa...

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Abstract

The invention discloses polyphenylacetylene silicon oxide borane and a preparation method thereof. The structure of the prepared polyphenylacetylene silicon oxide borane is shown as a formula I, wherein R1 and R2 refer to CH3, C6H5, and n is 1-100. The preparation method comprises the following steps of: performing hydrogen chloride removal reaction on trichlorosilane and alkyl boric acid to obtain polychlorosilicon oxide borane; and reacting the polychlorosilicon oxide borane with phenylacetylenelithium to obtain the polyphenylacetylene silicon oxide borane. In the polymer, a repeat unit contains polyphenylacetylene, so the magnitude of the polymerization degree cannot influence the crosslinking density of the polymer. The molecular weight of the polymer can be controlled by proportioning raw materials. In high temperature environment, the surface of a material is vitrified, and a ceramic layer such as a silicon carbide layer or a boron carbide layer is formed, so that the inner material is isolated from heat and oxygen; therefore, the thermal oxidation performance of the structural material is improved. The polyphenylacetylene silicon oxide borane is applied to preparing ceramic precursors, high-performance composite material matrixes, ablation resistant materials, high temperature resistant coatings and the like. The formula I is shown in the specifications.

Description

technical field [0001] The invention belongs to a polyphenylethynylsiloxaborane and a preparation method thereof. Background technique [0002] Silicon-containing polymers, such as polysilane, polycarbosilane, polynitrosilane and polycarbosilazane, have unique physical and chemical properties and are widely used in aviation, aerospace and other fields. Silicon-containing polymers with carbon-carbon triple bonds in the molecular chain have become a research hotspot in recent years because of their excellent high temperature resistance and molding process performance. Japan's Itoh synthesized a silicon-containing polymer with a carbon-carbon triple bond in the molecular chain [-Si(Ph)H-C≡C-C 6 h 4 -C≡C-] (referred to as MSP), the study found that the Td of its cured product under argon and air 5 (The temperature when the mass loss reaches 5%) is 860°C and 567°C respectively; Chinese patent CN1421446A "Phenylethynylsilane and its preparation method" and CN1763053A "New Synth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G79/08
Inventor 宋宁倪礼忠朱依丽周权陈建定
Owner EAST CHINA UNIV OF SCI & TECH
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