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Siliceous aromatic ether and aryne polymer and preparation method thereof

A polymer and aryl ether technology, applied in the field of silicon-containing aryl ether aryne polymers and their preparation, can solve the problems of poor toughness, poor overall mechanical properties, and high viscosity of silicon-containing aryl alkyne resins, and achieves good performance, Excellent thermal stability and mechanical properties, easy to store

Inactive Publication Date: 2011-04-20
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Silicon-containing aryne resin has excellent heat resistance and oxidation resistance, and can be used as a precursor of ceramic materials. It has broad application prospects in the fields of electronics and aerospace, but the viscosity of silicon-containing aryne resin is relatively high The material is brittle, the toughness is poor, and the overall mechanical properties are not good, which limits the application of silicon-containing aryne resin to a certain extent

Method used

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  • Siliceous aromatic ether and aryne polymer and preparation method thereof
  • Siliceous aromatic ether and aryne polymer and preparation method thereof
  • Siliceous aromatic ether and aryne polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In an anhydrous, oxygen-free nitrogen atmosphere, add 6.18g (0.26mol) of magnesium powder and THF (50ml) into a four-necked flask, and drop about 1 / 3 of ethyl chloride 26.16g (0.24mol) / THF at one time (50ml) solution in the system, after triggering, add the remaining ethyl chloride (0.16mol) dropwise after cooling in an ice-water bath, and keep warm at 40-60°C for 1-2h. Cool to room temperature, dropwise add bisphenol A (4.56g, 0.02mol) / THF (40ml) solution and diethynylbenzene (12.6g, 0.10mol) / THF (60ml) solution successively, control the dropping rate, 60~70℃ Under the reaction 1 ~ 3h. Cool down to room temperature, add dimethyldichlorosilane (12.9g, 0.10mol) / THF (50ml) dropwise, and react at 60-70°C for 2-5h. Acetic acid / THF solution terminated the reaction, precipitated after suction filtration, and stood overnight to desalt by suction filtration and rotary evaporation to remove the solvent to obtain a brown-yellow viscous liquid. Its infrared spectrum is as figur...

Embodiment 2

[0032] In an anhydrous, oxygen-free nitrogen atmosphere, add 3.09g (0.13mol) of magnesium powder and THF (20ml) into a four-necked flask, and drop about 1 / 3 of the amount of ethyl chloride 7.80g (0.12mol) / THF (50ml) solution in the system, after being triggered, drop the remaining ethyl chloride (0.08mol) after cooling down in an ice-water bath, and keep warm at 40-60°C for 1-3h. Cool to room temperature, successively add bisphenol A (2.28g, 0.01mol) / THF (50ml) solution and diethynylbenzene (6.3g, 0.05mol) / THF (50ml) solution dropwise, control the dropping rate, 60~70℃ The reaction time is 1-2 hours. Cool down to room temperature, add dimethyldichlorosilane (10.35g, 0.09mol) / THF (50ml) dropwise, and react at 60-70°C for 2-5 hours. Acetic acid / THF solution terminated the reaction, precipitated after suction filtration, stood overnight to remove salt by suction filtration, and removed the solvent by rotary evaporation to obtain a brown-yellow viscous liquid. It has a molecular...

Embodiment

[0034] In an anhydrous, oxygen-free nitrogen atmosphere, add magnesium powder 6.18g (0.26mol) / THF (50ml) to the four-necked flask; drop about 1 / 3 of the amount of vinyl chloride 15.00g (0.24mol) / THF (50ml) ) solution in the system, after being triggered, drop the remaining vinyl chloride (0.16mol) after cooling down in an ice-water bath, and keep warm at 40-50°C for 1-2h. After cooling to room temperature, 4,4'-dihydroxydiphenyl ether (4.04g, 0.02mol) / THF (50ml) solution and diethynylbenzene (12.6g, 0.10mol) / THF (50ml) solution were added dropwise successively, controlling Dropping rate, 60~70°C reaction time 1~2h. Cool down to room temperature, add methylhydrogendichlorosilane (11.50g, 0.10mol) / THF (50ml) dropwise, and react at 60-70°C for 2-5 hours. Acetic acid / THF solution terminated the reaction, precipitated after suction filtration, stood overnight to remove salt by suction filtration, and removed the solvent by rotary evaporation to obtain a brown-yellow viscous liquid...

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Abstract

The invention relates to a siliceous aromatic ether and aryne polymer and a preparation method thereof. The polymer is structurally characterized by comprising silicon atoms, aryne groups and an aromatic ether structure on a main chain. The siliceous aromatic ether and aryne polymer is polymerized from diacetylene-benzene or a dyhydroxy aromatic compound and dichlorosilane by Grignard reaction under an inert atmosphere. The preparation method of the polymer comprises the following steps of: firstly reacting haloalkane with magnesium powder to produce an alkyl magnesium halide Grignard reagent; and then reacting with the dyhydroxy aromatic compound to obtain an alkyl magnesium halide Grignard reagent of the dyhydroxy aromatic compound or reacting with diacetylene-benzene to obtain an alkyl magnesium halide Grignard reagent of diacetylene-benzene; and finally reacting with dichlorosilane to obtain the siliceous aromatic ether and aryne polymer. The invention has the advantages of simple process, short reaction time, easily controlled process condition and simple subsequent processing and is convenient to operate; in addition. The product of the method is stable at room temperature and easy to store, the condensate of the polymer has excellent heat-resisting stability and mechanical property and is a high-performance thermosetting resin with good heat-resisting property.

Description

technical field [0001] The invention relates to a heat-resistant and stable silicon-containing aryl ether aryne polymer and a preparation method thereof. Background technique [0002] Silicon-containing aryne resin has excellent heat resistance and oxidation resistance, and can be used as a precursor of ceramic materials. It has broad application prospects in the fields of electronics and aerospace, but the viscosity of silicon-containing aryne resin is relatively high The substance is brittle, the toughness is poor, and the overall mechanical properties are not good, which limits the application of silicon-containing aryne resin to a certain extent. The polymer molecular chains containing ether bonds in the structure are flexible, and the existence of the flexible structure endows the material with excellent toughness and impact resistance. At the same time, the polymer containing the flexible structure in the structure has relatively low viscosity and better processing per...

Claims

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Application Information

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IPC IPC(8): C08G77/52
Inventor 齐会民杜磊黄发荣张玲玲娜清冯之瑶李慧澄
Owner EAST CHINA UNIV OF SCI & TECH
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