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Liquid oxygen compatible phosphorus-containing epoxy resin system and preparation method thereof

An epoxy resin system, liquid oxygen technology, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as damage to epoxy resin properties, and achieve easy operation and preparation. Simple and feasible method

Pending Publication Date: 2022-07-05
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, both of these methods will damage the properties of the epoxy itself, such as thermal stability and mechanical properties

Method used

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  • Liquid oxygen compatible phosphorus-containing epoxy resin system and preparation method thereof
  • Liquid oxygen compatible phosphorus-containing epoxy resin system and preparation method thereof
  • Liquid oxygen compatible phosphorus-containing epoxy resin system and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 250ml three-necked flask equipped with a stirring paddle, a reflux condenser and a nitrogen port, add 32.4g (0.1mol) of 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphorus Heterophenanthrene-10-oxide and 92.5g (1mol) epichlorohydrin, then add 0.01mol tetrabutylammonium bromide, under nitrogen protection, stir and react in an oil bath at 65°C for 6h, until the solution is clear and transparent ; Cool down to 50°C, add 20wt% sodium hydroxide (8g) solution dropwise with a constant pressure dropping funnel, the dropwise addition time is 1h, the reaction is 6h, the solution is clear and transparent; it is cooled to room temperature, and the organic solvent dichloromethane is used. Extraction, and wash with deionized water for 3 times to remove sodium chloride, until the aqueous phase is free of chloride ions (using silver nitrate solution to check); the final product is rotary distilled at 100 ° C to remove excess epichlorohydrin, organic solvent and water, and finally...

Embodiment 2

[0031] In a 250ml three-necked flask equipped with a stirring paddle, a reflux condenser and a nitrogen port, add 32.4g (0.1mol) of 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphorus Heterophenanthrene-10-oxide and 92.5g (1mol) epichlorohydrin, then add 0.005mol of tetrabutylammonium bromide, under nitrogen protection, stir and react in an oil bath at 65°C for 6h, until the solution is clear and transparent ; Cool down to 50°C, add 20wt% sodium hydroxide (8g) solution dropwise with a constant pressure dropping funnel, the dropwise addition time is 1h, the reaction is 6h, the solution is clear and transparent; it is cooled to room temperature, and the organic solvent dichloromethane is used. Extraction, and wash with deionized water for 3 times to remove sodium chloride, until the aqueous phase is free of chloride ions (using silver nitrate solution to check); the final product is rotary distilled at 100 ° C to remove excess epichlorohydrin, organic solvent and water, and fin...

Embodiment 3

[0033] In a 250ml three-necked flask equipped with a stirring paddle, a reflux condenser and a nitrogen port, add 32.4g (0.1mol) of 10-(2,5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphorus Heterophenanthrene-10-oxide and 92.5g (1mol) epichlorohydrin, then add 0.005mol of tetrabutylammonium bromide, under nitrogen protection, stir and react in an oil bath at 65°C for 6h, until the solution is clear and transparent ; Cool to 50°C, add 28wt% sodium hydroxide (8g) solution dropwise using a constant pressure dropping funnel, the dropwise addition time is 1h, the reaction is 6h, the solution is clear and transparent; it is cooled to room temperature, and the organic solvent dichloromethane is used. Extraction, and wash with deionized water for 3 times to remove sodium chloride, until the aqueous phase is free of chloride ions (using silver nitrate solution to check); the final product is rotary distilled at 100 ° C to remove excess epichlorohydrin, organic solvent and water, and finally...

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Abstract

The invention discloses a liquid oxygen compatible phosphorus-containing epoxy resin system and a preparation method thereof, and the preparation method comprises the following steps: carrying out ring opening on 10-(2, 5-dihydroxyphenyl)-10-hydro-9-oxa-10-phosphaphenanthrene-10-oxide and epoxy chloropropane under the action of a quaternary ammonium salt catalyst, and then carrying out epoxidation under the action of a basic catalyst. The prepared epoxy resin has liquid oxygen compatibility, is expected to be used as a matrix material of a composite material, and is applied to a lining-free composite material liquid oxygen storage tank.

Description

technical field [0001] The invention relates to the field of preparation of organic polymer compounds, in particular to a liquid oxygen compatible phosphorus-containing epoxy resin system and a preparation method thereof. Background technique [0002] Reducing the launch cost of spacecraft and improving the carrying capacity are the development trends of future spacecraft and launch vehicles. In order to achieve this goal, the first problem that must be solved is the excessive weight of the aircraft. As one of the main components of the launch vehicle, the propellant tank occupies a large volume and is the main weight reduction component. Traditional propellant storage tanks are mainly made of metal materials. If epoxy resin and composite materials are used, the weight of the storage tank will be reduced by 20-40%. However, when epoxy resin and its composite materials are in contact with liquid oxygen, violent chemical reactions such as explosion and combustion may occur u...

Claims

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Application Information

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IPC IPC(8): C08G59/06C07F9/6571
CPCC08G59/063C07F9/657172
Inventor 严佳李娟子武湛君陈铎李世超
Owner DALIAN UNIV OF TECH
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