Aryne resin containing silicone

An arylalkyne resin and siloxane technology, applied in the field of siloxane-containing arylalkyne resins, can solve the problems of poor material performance, difficult processing and molding, and high reaction temperature, and achieves convenient application, easy curing, and low curing temperature. Effect

Inactive Publication Date: 2005-12-21
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this resin is not suitable as a material, because the curing and crosslinking reaction temperature of the resin with phenylacetylene as the terminal group is very high

Method used

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  • Aryne resin containing silicone
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  • Aryne resin containing silicone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030]

[0031]Soak the magnesium powder with 5% dilute hydrochloric acid for 2-3 minutes, and then filter with suction; then wash with deionized water three times, and filter with suction; wash with absolute ethanol for three times, and filter with suction; finally wash with petroleum ether for three times, and filter with suction After drying, the magnesium powder that can be used can be obtained. The 500ml four-necked round-bottomed flask equipped with constant pressure funnel, spherical condenser, ventilation tube / thermometer and stirrer was evacuated and filled with nitrogen, and replaced like this three times; under nitrogen protection, 3.0g (0.12 mol) magnesium powder and a small amount of iodine crystals, and then add 30ml of tetrahydrofuran (treated with sodium metal to remove water and oxygen), and stir evenly. Add 10.9g (0.10mol) bromoethane and 30ml tetrahydrofuran (THF, dried over sodium metal) mixed solution into the constant pressure funnel, start to drop bro...

Embodiment 2

[0036]

[0037] The 500ml four-neck round-bottomed flask equipped with a 100ml constant pressure funnel, spherical condenser, vent tube / thermometer and stirrer was vacuumized and filled with nitrogen, and replaced like this three times; under nitrogen protection, 3.0g ( 0.12mol) of magnesium powder and a small amount of iodine crystals treated (same as in Example 1), and then 30ml of tetrahydrofuran (dried over sodium metal) was added, and stirred evenly. Add 0.10 mol ethyl bromide and 30 ml tetrahydrofuran (THF, treated with sodium metal to remove water and oxygen) mixture into the constant pressure funnel, start adding bromide / THF mixture dropwise to the flask, and stir rapidly, during which you can see The reaction system changed from light brownish yellow to iron gray, and gradually became turbid. After the dropwise addition, react under heating in an oil bath at 60-66°C for 2 hours to obtain the Grignard reagent of ethyl bromide.

[0038] Add 30ml tetrahydrofuran and ...

Embodiment 3

[0042]

[0043] Vacuumize a 500ml four-necked round-bottomed flask equipped with a 100ml constant pressure funnel, spherical condenser, vent tube / thermometer and stirrer, then fill it with nitrogen to dehumidify and deoxygenate, and add 0.12mol of magnesium powder to the four-necked flask under nitrogen protection and a small amount of iodine crystals, and then add 30ml of tetrahydrofuran (dried over sodium metal), and stir evenly. Add 0.10 mol of bromoethane and 30 ml of tetrahydrofuran mixture dropwise through a constant pressure funnel, and cool with an ice-water bath while dropping. During the period, it can be seen that the reaction system changes from the original light brown yellow to iron gray, and gradually becomes turbid. After the dropwise addition, react under heating in an oil bath at 60-66°C for 2 hours to obtain the Grignard reagent of ethyl bromide.

[0044] Add 30ml of tetrahydrofuran and 0.0633mol of 1,3-diethynylbenzene into a four-neck round-bottomed fl...

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Abstract

The invention relates to a kind of arylenealkyne resin containing siloxanes. The said resin makes diethynylene benzene (DEB) and silicon alkyl chloride as raw materials, firstly make use of the reaction of magnesium and alkyl bromide to produce Grignard reagentú¼then react with DEB to produce alkyne Grignard reagent; then react with silicon alkyl chloride, finally hydrolyze and condense in alkaline water liquor, or extend chain with siloxanes chloride, to form a kind of arylenealkyne resin containing siloxanes of new-style structure. The resin designed and synthesized by the invention has good processing property, and can be solidified into crosslinked resin of good thermostability under heat, light or radiative condition. Besides it has good machine capability, electric insulation capability and ceramic performance. So it can be used as the base material of high performance compound material resin, insulation material, the ceramic precursors and so on, and also has wide application prospect in such high technology fields as spaceflight, aviation, navigation and so on.

Description

technical field [0001] The present invention relates to a thermosetting resin, in particular to a silicone-containing aryne resin. Background technique [0002] Alkyne-containing resin (especially aryne resin) is a kind of heat-resistant resin developed and used in recent years. It does not need solvent during the molding process, and no small molecules escape during the curing process. It can be molded under normal or low pressure. The pyrolysis temperature of the cured resin is above 500°C, and the pyrolysis carbonization rate is as high as 80-86%. 50-60% of the currently used phenolic resin composite material, and has a compact structure and excellent ablation resistance. However, the rigidity of the cured resin is too high, resulting in unsatisfactory mechanical properties. Therefore, the modification of alkyne-containing resins (especially aryne resins) has become a research hotspot. [0003] In the 1980s, Naval Research Laboratory T.M.Keller and others began to stud...

Claims

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Application Information

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IPC IPC(8): C08F138/00
Inventor 黄发荣杜磊王帆高飞周燕齐会民沈学宁扈燕红
Owner EAST CHINA UNIV OF SCI & TECH
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