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Preparation method of polysiloxane modified silicon-containing arylacetylene resin

A polysiloxane and silicon aryl alkyne technology, which is applied in the field of polysiloxane-modified silicon-containing aryl alkyne resin and its preparation field, can solve the problems of insufficiently low viscosity and insufficient mechanical properties of silicon-containing aryl alkyne resin, and achieves the Improved mechanical properties, improved processability, and stable heat resistance

Active Publication Date: 2017-06-23
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Due to the limitations of the structure of the modified silicon-containing aryne resin, the viscosity of the silicon-containing aryne resin modified by the existing technology is not low enough, and the mechanical properties are insufficient.

Method used

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  • Preparation method of polysiloxane modified silicon-containing arylacetylene resin
  • Preparation method of polysiloxane modified silicon-containing arylacetylene resin
  • Preparation method of polysiloxane modified silicon-containing arylacetylene resin

Examples

Experimental program
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Effect test

Embodiment 1

[0043] Example 1. Two (1,3-ethynylanilino) tetramethyldisiloxane modified silicon-containing aryne resin

[0044] 1. Synthesis of bis(1,3-ethynylanilino)tetramethyldisiloxane

[0045] Under nitrogen protection, 30mL of toluene, 14mL of triethylamine (0.1mol) and 11.3mL of m-aminophenylacetylene (0.1mol ); using an ice-salt bath to cool the above mixed solution to -10°C, and drop the mixed solution of 30mL toluene and 10mL 1,3-dichlorotetramethyldisiloxane (0.05mol) into In the above solution, the rate of addition was controlled so that the temperature of the reaction solution was maintained at -10°C; after the dropwise addition was completed, the reaction was continued for 1 hour, then the temperature was raised to 30°C, and the reaction was continued with stirring for 12 hours to obtain a yellow suspension. Remove the precipitate by filtration, wash the filtrate to neutral with deionized water, and dry it with anhydrous sodium sulfate, then filter and distill off the solvent...

Embodiment 2

[0055] Example 2. Two (1,3-ethynylanilino) tetraphenyldisiloxane modified silicon-containing aryne resin

[0056] 1. Synthesis of bis(1,3-ethynylanilino)tetraphenyldisiloxane

[0057] Under nitrogen protection, 30mL of toluene, 14mL of triethylamine (0.1mol) and 11.3mL of m-aminophenylacetylene (0.1mol ); using an ice-salt bath to cool the above mixed solution to -10°C, and drop the mixed solution of 20mL toluene and 18.8mL 1,3-dichlorotetraphenyldisiloxane (0.05mol) through a constant pressure dropping funnel Add to the above solution, during which the rate of addition is controlled so that the temperature of the reaction solution is maintained at -10°C; after the dropwise addition is complete, the reaction is continued for 1 hour, then the temperature is raised to about 80°C, and the reaction is continued for 48 hours with stirring to obtain a yellow suspension. Remove the precipitate by filtration, wash the filtrate to neutral with deionized water, and dry it with anhydrou...

Embodiment 3

[0061] Example 3. Two (1,5-ethynylanilino) hexamethyltrisiloxane modified silicon-containing aryne resin

[0062] 1. Synthesis of bis(1,5-ethynylanilino)hexamethyltrisiloxane

[0063] Under nitrogen protection, 40mL of toluene, 14mL of triethylamine (0.1mol) and 11.3mL of m-aminophenylacetylene (0.1mol ); Use an ice-salt bath to cool the above mixed solution to -10°C, and drop the mixed solution of 20mL toluene and 13.8mL 1,5-dichlorohexamethyltrisiloxane (0.05mol) through a constant pressure dropping funnel Into the above solution, during which the rate of addition is controlled so that the temperature of the reaction solution is maintained at -10°C; after the dropwise addition is complete, the reaction is continued for 1 hour, then the temperature is raised to 60°C, and the reaction is continued for 20 hours with stirring to obtain a yellow suspension. Remove the precipitate by filtration, wash the filtrate to neutral with deionized water, and dry it with anhydrous sodium s...

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Abstract

The invention discloses polysiloxane modified silicon-containing arylacetylene resin and a preparation method thereof. The preparation method comprises the following steps: under inert gas shielding, stirring 5-30 parts of ethynyl aniline terminated polysiloxane (SO) and 70-95 parts of silicon-containing arylacetylene resin (PSA) by weight part at 100-140 DEG C to carry out reaction for 0.5-3h to obtain redish brown modified silicon-containing arylacetylene resin. As for the obtained ethynyl aniline terminated polysiloxane modified silicon-containing arylacetylene resin, while excellent heat resistance of the silicon-containing arylacetylene resin is kept, the viscosity of the resin is remarkably lowered, the processing properties and the dielectric properties are improved, the mechanical properties are further improved, and the application range of the silicon-containing arylacetylene resin as an ablation resistant material, a high-temperature resistant wave-transparent material, a ceramic precursor, a structure and function integrated material and the like in the aerospace field, the military field, the electronic field and the like is expanded.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and modified resins, in particular to an ethynylaniline-terminated polysiloxane-modified silicon-containing aryne resin and a preparation method thereof. Background technique [0002] Silicon-containing aryne resin (PSA) has broad application prospects in the aerospace field because of its excellent high temperature resistance and dielectric properties. However, silicon-containing aryne resins are brittle after curing and have mediocre mechanical properties, which limit their application range. Therefore, it is imperative to modify silicon-containing aryne resins. In recent years, researchers have made active attempts in the modification of silicon-containing aryne resins and achieved some results. Gao Yu et al. (Gao Yu, Zhou Yan, Huang Farong, et al. Preparation and properties of silicon-containing arylactylene resin / benzoxazines blends. High Performance Polymers. 2013, 25(4): 445–453) used be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/60C08G77/54C08G77/452
CPCC08G77/452C08G77/54C08G77/60C08G77/80
Inventor 周燕黄发荣杨庆涛邓诗峰杜磊
Owner EAST CHINA UNIV OF SCI & TECH
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