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Polymer with backbone chain having silicon-aromatic bispropargyl ether structure and preparation method thereof

A technology of dipropargyl ether and polymer, applied in coatings, adhesives and other directions, can solve the problems of harsh synthesis reaction conditions, affecting popularization and application, and being difficult to obtain, and achieves low price, simple production process, and increased cross-linking. The effect of density

Inactive Publication Date: 2009-03-11
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cost of raw materials for synthesizing this silicon-containing polymer is high, it is not easy to obtain, and the synthesis reaction conditions are harsh, which affects its popularization and application.

Method used

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  • Polymer with backbone chain having silicon-aromatic bispropargyl ether structure and preparation method thereof
  • Polymer with backbone chain having silicon-aromatic bispropargyl ether structure and preparation method thereof
  • Polymer with backbone chain having silicon-aromatic bispropargyl ether structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] A solution of 4.03g (13.25mmol) of dipropargyl bisphenol A ether (aromatic dipropargyl ether compound) and 5ml of diethylene glycol dimethyl ether (solvent) was added to the reaction vessel, and gradually added under stirring 26.60mg (0.70mmol) lithium aluminum hydride LiAlH 4(Catalyst) and 1.43g (13.25mmol) of phenylsilane (silicon-hydrogen compound), after being thoroughly mixed, the temperature is raised to 120°C under the protection of inert gas, and the reaction is carried out under normal pressure for 20h.

[0065] After the reaction is over, add 5ml of toluene and 5ml of 1mol / L hydrochloric acid to the reaction vessel at room temperature, stir well, separate the liquids, remove the lower aqueous phase, add 15ml of deionized water to the upper organic phase, and separate again , Remove the lower aqueous phase, and repeat the operation three times. The obtained organic phase was collected and the solvent was distilled off under reduced pressure to obtain the target pro...

Embodiment 2

[0073] Add a solution of 6.00g (19.75mmol) of dipropargyl bisphenol A ether (aromatic dipropargyl ether compound) and 8ml of diethylene glycol dimethyl ether (solvent) into the reaction vessel, and gradually add under stirring 38.00mg (1mmol) lithium aluminum hydride LiAlH 4 (Catalyst) and 2.19g (20.25mmol) of phenylsilane (silicon hydride compound), after being thoroughly mixed, under the protection of inert gas, the temperature is raised to 110°C and reacted under normal pressure for 20h.

[0074] After the reaction is over, add 8ml of toluene and 8ml of 1mol / L hydrochloric acid to the reaction vessel at room temperature, stir well, separate the liquids, remove the lower aqueous phase, add 20ml of deionized water to the upper organic phase, and then separate the liquids , Remove the lower aqueous phase, and repeat the operation three times. The obtained organic phase was collected and the solvent was distilled off under reduced pressure to obtain the target product with a yield ...

Embodiment 3

[0077] A solution of 5.93g (19.50mmol) of dipropargyl bisphenol A ether (aromatic dipropargyl ether compound) and 44ml of toluene (solvent) was added to the reaction vessel, and 5.50g (137.50mmol) was gradually added under stirring MgO (catalyst) and 2.21g (20.50mmol) of phenylsilane (silicon hydride compound), after stirring uniformly, under the protection of inert gas, the temperature is raised to 80°C, and the reaction is carried out under normal pressure for 18h.

[0078] After the reaction, MgO was removed by filtration. Add 120 ml of n-heptane to the filtrate and stir well. The precipitate was filtered and collected, and dried under vacuum at 60° C. for 50 h to obtain the target product. The yield was 43%.

[0079] The obtained poly(phenylsilane-4,4'-dipropargyl bisphenol A ether) has a weight average molecular weight Mw of 5,473 as measured by gel permeation chromatography.

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Abstract

The invention relates to a polymer containing a silicon-alkyne propyl ether structure on a main chain and a method for preparing the same. The structure of the polymer is shown in the graph, and the polymer is produced from an aromatic diyne propyl ether compound and a silicon hydride compound through dehydrogenation coupling reaction. The polymer can be used as a high temperature resistant polymer and applied to matrix resin, high temperature resistant adhesives and coatings of advanced composite materials, and the preparation of ceramic precursors.

Description

Technical field [0001] The invention relates to a polymer containing a silicon-aromatic dipropargyl ether structure on the main chain and a preparation method thereof. Background technique [0002] Silicon-containing polymers, such as polysiloxanes, polyhydrocarbons, polysilazanes, and polysilicates, have good intrinsic heat resistance, and are usually used as high temperature resistant materials. The silicon-containing polymer poly[(phenylsilylene)-ethynyl-1,3-phenylethynyl] synthesized by MasayoshiItoh et al., because it contains silicon-carbon bonds with larger bond energy in the main chain, and is resistant to Heat and quite active silicon-hydrogen bonds can react with unsaturated alkynyl groups under heated conditions to increase the cross-linking density of the polymer during curing, so the cured product of this polymer has a very high The thermal stability performance. In addition, the polymer can be molded at about 150°C, showing good processability. However, the cost of ...

Claims

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Application Information

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IPC IPC(8): C08G77/60C08L83/16C09J183/16C09D183/16C04B35/634
Inventor 杨光张马宁
Owner BEIHANG UNIV
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