Heat-resisting reaction type phosphorate containing flame retardant with maleimide structure and preparation method thereof

A technology of maleimide and maleimide-based phenol, which is applied in the field of heat-resistant reactive maleimide structure phosphorus-containing flame retardants and its preparation, and can solve the problem of material heat resistance degradation and purification The problem of cumbersome process and low flame retardant efficiency can overcome the damage of heat resistance, the post-processing process is simple, and it is not easy to migrate

Active Publication Date: 2014-02-19
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing reactive flame retardants have the disadvantages of cumbersome reaction and purification process and low flame retardant efficiency. In addition, the low thermal decomposition temperature of organophosphorus flame retardants leads to a decrease in the heat resistance of the material, which limits its application.

Method used

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  • Heat-resisting reaction type phosphorate containing flame retardant with maleimide structure and preparation method thereof
  • Heat-resisting reaction type phosphorate containing flame retardant with maleimide structure and preparation method thereof
  • Heat-resisting reaction type phosphorate containing flame retardant with maleimide structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 37.8g (0.2mol) of maleimidophenol, 250ml of anhydrous tetrahydrofuran and 29.7g (0.1mol) of pentaerythritol diphosphate diphosphoryl chloride into a 500ml three-necked flask equipped with a stirrer, nitrogen inlet and condenser , feed nitrogen, and heat the material in the reactor to 70 ° C, while heating and stirring continuously, after constant temperature, continue to stir until no HCl gas is released, cool to room temperature, and remove the reaction solvent by distillation under reduced pressure, the obtained orange product is heat-resistant Phosphorus-containing flame retardant with reactive maleimide structure, the yield is 90%.

[0030] The proton nuclear magnetic resonance spectrum analysis of the resulting product, the peak position of the chemical shift at 6.80-6.85ppm is the hydrogen vibration signal on the double bond on the nitrogen-containing five-membered ring, and the chemical shift is between 7.05-7.11ppm and 7.12-7.14ppm The peaks between are the ...

Embodiment 2

[0034] Add 18.9g (0.1mol) of maleimidophenol, 150ml of anhydrous acetonitrile and 18.5g (0.1mol) of neopentyl glycol phosphorus oxychloride into a 500ml three-neck flask equipped with a stirrer, an argon inlet and a condenser , feed argon, and heat the material in the reactor to 85 ° C, while heating, continue to stir, after constant temperature, continue to stir until no HCl gas is released, cool to room temperature, and remove the reaction solvent by distillation under reduced pressure, the obtained orange-yellow product is resistant to Phosphorus-containing flame retardant with heat-reactive maleimide structure, the yield is 92%.

[0035]The proton nuclear magnetic resonance spectrum analysis of the resulting product, the peak position of the chemical shift at 6.80-6.86ppm is the hydrogen vibration signal on the double bond on the nitrogen-containing five-membered ring, and the chemical shift is between 7.06-7.11ppm and 7.11-7.14ppm The peaks between are the hydrogen vibrat...

Embodiment 3

[0039] Add 37.8g (0.2mol) of maleimidophenol, 250ml of anhydrous toluene and 21.1g (0.1mol) of phenyl dichlorophosphate into a 500ml three-necked flask equipped with a stirrer, a helium inlet and a condenser , feed helium, and heat the material in the reactor to 100 ° C, while heating and stirring continuously, after constant temperature, continue stirring until no HCl gas is released, cool to room temperature, and distill off the reaction solvent under reduced pressure, the obtained orange-yellow product is resistant Phosphorus-containing flame retardant with heat-reactive maleimide structure, the yield is 88%.

[0040] The proton nuclear magnetic resonance spectrum analysis of the resulting product, the peak position of the chemical shift at 6.80-6.86ppm is the hydrogen vibration signal on the double bond on the nitrogen-containing five-membered ring, and the chemical shift is between 7.05-7.11ppm and 7.12-7.14ppm The peaks between are the hydrogen vibration signals on the b...

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Abstract

The invention discloses a heat-resisting reaction type phosphorate containing flame retardant with a maleimide structure and a preparation method thereof. The preparation method is characterized in that maleimide based phenol and phosphoryl chloride or phosphoryl bromide are added into a reactor, a reaction solvent is added into the reactor, then an inert gas is fed into the reactor, and materials in the reactor are heated to 70-100 DEG C; continuous stirring is performed during heating, and stirring is continued during a constant temperature reaction until no hydrogen halide gas is released; the materials are cooled to a room temperature, distillation under reduced pressure is performed to remove the reaction solvent, and an obtained orange-yellow product is the heat-resisting reaction type phosphorate containing flame retardant with the maleimide structure. The prepared heat-resisting reaction type phosphorate containing flame retardant with the maleimide structure can serve as a reaction type flame retardant to react with a polymer resin matrix, is not prone to movement and has superior service durability and good flame-retardant effect, and the heat resistance of a material can be improved simultaneously.

Description

technical field [0001] The invention belongs to the technical field of halogen-free phosphorus-containing flame retardants, and in particular relates to a phosphorus-containing flame retardant with a heat-resistant reactive maleimide structure and a preparation method thereof. Background technique [0002] At present, polymer-based composite materials are becoming an increasingly important class of new materials due to their light weight and excellent performance, replacing traditional materials and being widely used in all aspects of life and production. Thermosetting resins such as epoxy resins and unsaturated polyesters are widely used in the field of reinforced composite materials. Reinforced composite materials have excellent properties such as low price, high tensile strength, light weight, and chemical resistance, and are used in construction, chemical industry, transportation, shipbuilding, electrical and other fields. However, thermosetting resins are mostly compos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/527C08K5/5397C08K5/5313C07F9/6574C07F9/572C08L67/06
Inventor 胡源白志满宋磊台启龙
Owner UNIV OF SCI & TECH OF CHINA
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