Novel high-temperature resistant phenylacetylene terminated poly (acetenyl-silane) and preparation method thereof

A phenylacetylene and ethynyl technology, which is applied in the field of new high-temperature-resistant phenylacetylene-terminated poly(ethynyl-silane) and its preparation, can solve the problems of inability to meet the higher requirements of aerospace technology and the decline of thermal oxidation stability, etc. Achieve the effects of easy control of reaction conditions, short reaction time and convenient operation

Inactive Publication Date: 2011-04-13
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Methyldiphenylethynylsilane (abbreviated as MDPES, ZL02151140.3; ZL200510110133.5), methyltriphenylethynylsilane (abbreviated as MTPES, ZL200510110132.0) and tetraphenylethynylsilane (abbreviated as TPES) in a nitrogen atmosphere Td 5 (Decomposition temperature at 5% mass loss rate) are 615°C, 695°C and 710°C respectively; 800°C mass retention rates are 91.1%, 92.9% and 93.3% respectively, however the thermo-oxidative stability of this kind of material in air The significant drop (as shown in Table 1) makes this type of material unable to meet the higher requirements of aerospace technology for high-temperature resistant composite materials

Method used

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  • Novel high-temperature resistant phenylacetylene terminated poly (acetenyl-silane) and preparation method thereof
  • Novel high-temperature resistant phenylacetylene terminated poly (acetenyl-silane) and preparation method thereof
  • Novel high-temperature resistant phenylacetylene terminated poly (acetenyl-silane) and preparation method thereof

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Experimental program
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Embodiment 1

[0027] Dissolve 10mmol of phenylacetylene and 45mmol of trichlorethylene in 45ml of tetrahydrofuran, add 145mmol of butyllithium reagent dropwise with a constant pressure funnel, dropwise for 40 minutes, and react at -30°C for 4 hours after the dropwise addition. Then, 50 mmol of methylhydrogendichlorosilane was dissolved in 20 ml of tetrahydrofuran and added dropwise to the mixture of ethynyl dilithium and phenylethynyl lithium, and reacted at 10° C. for 6 hours after the dropwise addition was completed. After the reaction, add 50ml of saturated ammonium chloride solution into the reaction solution, stir fully, separate the liquids, take the upper oil phase and wash it with 30ml of saturated ammonium chloride solution until the pH value is neutral, add ether to the obtained water phase twice to extract , liquid separation, collecting and merging the resulting oil phase, and decompression distillation to remove the solvent to obtain a brown viscous resin phenylacetylene-termina...

Embodiment 2

[0029] Dissolve 30mmol of phenylacetylene and 35mmol of trichlorethylene in 40ml of tetrahydrofuran, add 135mmol of butyllithium reagent dropwise with a constant pressure funnel, dropwise for 40 minutes, and react at -20°C for 3 hours after the dropwise addition. Then, 50 mmol of dimethyldichlorosilane was dissolved in 20 ml of tetrahydrofuran and added dropwise to the mixture of ethynyl dilithium and phenylethynyl lithium, and reacted at 20° C. for 5 hours after the dropwise addition was completed. After the reaction, add 50ml of saturated ammonium chloride solution into the reaction solution, stir fully, separate the liquids, take the upper oil phase and wash it with 30ml of saturated ammonium chloride solution until the pH value is neutral, add ether to the obtained water phase twice to extract , separated, collected and combined the obtained oil phases, and distilled off the solvent under reduced pressure to obtain a brown-red viscous liquid phenylacetylene-terminated poly(...

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Abstract

The invention discloses a novel phenylacetylene terminated poly (acetenyl-silane) polymer and a preparation method thereof. The polymer is prepared from dihalogenosilane, phenylacetylene, trichloroethylene and organic lithium serving as raw materials and prepared by two-step reaction under the protection of inert gas. The method comprises the following steps of: 1, under the protection of the inert gas, making a mixture of the trichloroethylene and the phenylacetylene react with the organic lithium to obtain acetenyl dilithium and phenylacetylene lithium; and 2, under the protection of the inert gas, performing coupling reaction on the mixture of the acetenyl dilithium and the phenylacetylene lithium generated in the first step and the dihalogenosilane to obtain a final target product. The raw materials used in the polymer are easily obtained, the process flow is simple, and the operation process is feasible. The polymer prepared by the method is subjected to cross-linking reaction under heat or chemical initiation to form a thermosetting material with high-temperature resistance and excellent thermal oxidation resistance, and the thermosetting material is further heated to form a ceramic structure. The polymer prepared by the method can be used as a matrix resin, a high-temperature resistant coating and a ceramic precursor of an advanced composite material.

Description

technical field [0001] The invention relates to a high temperature resistant and thermal oxidation resistant polymer, in particular to an organic-inorganic hybrid polymer whose main chain contains silicon atoms and acetylene groups. The main chain is composed of Si-C and C≡C. The base compound caps the polymer. The ethynyl group undergoes a curing crosslinking reaction under the action of light, heat or an initiator to form a three-dimensional network structure, and further forms a ceramic structure under the action of high temperature. Background technique [0002] Silicone polymers containing π-electron systems and alternating silicon atoms in the molecular backbone have become a new field of materials research. Such polymers can not only be used as functional materials such as semiconductors and optics, but also as high-temperature-resistant matrix resins. And silicon carbide precursor, so it has potential application value in aerospace field. Among them, polycarbosilan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60
Inventor 周权倪礼忠王子昂
Owner EAST CHINA UNIV OF SCI & TECH
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