Reactive flame retardant, preparation method and application thereof
A flame retardant, reactive technology, applied in the field of reactive flame retardants and their preparation, can solve the problems of low temperature resistance level, low flame retardant level, decreased mechanical properties, etc.
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Embodiment 1
[0070] The structure of the reactive flame retardant of the present embodiment is as follows:
[0071]
[0072] The preparation method of this reactive flame retardant is as follows:
[0073] Put 2mol trimethyl phosphate, 200mL ethanol, 1mol p-xylylenediamine, 0.1mol sodium hydroxide, 0.1g DMAP into a three-port 2000ml glass reactor with stirring device, heat up to ethanol reflux, react for 4 hours under stirring, then add 2mol Sodium hydroquinone, reacted for 2 hours, added hydrochloric acid to neutralize the reaction system until the pH was 7, removed impurities and water in the system by physical methods, and distilled off the solvent in the system to obtain 422.37 g of the reactive flame retardant with the above structure.
[0074] 1 H NMR (CDCl 3 ,500MHz): δ7.86~7.82(t, 2H, PONH), 6.98~6.74(m, 4H, Ar-H), 6.66~6.56(m, 8H, Ar-H), 4.72~4.76(s, 2H , Ar-OH), 4.42~4.32 (d, 4H, CH 2 ), 3.34~3.28 (d, 6H, CH 3 ).
Embodiment 2
[0076] The structure of the reactive flame retardant of the present embodiment is as follows:
[0077]
[0078] The preparation method of this reactive flame retardant is as follows:
[0079] Put 2 mol of dichlorophenylphosphine and 200 mL of acetone into a three-port 2000 ml glass reactor with a stirring device, pass in nitrogen gas, add 1 mol of disodium ethylene glycol dropwise for 30 minutes under stirring, continue to react at room temperature for 60 minutes, and then add 2 mol of p-phenylene Sodium diphenolate, continue to react at room temperature for 120min, add 2L 1mol / L hydrochloric acid dropwise for 120min, wash with water until neutral after the reaction, remove impurities and water in the system by physical methods, and distill off the solvent in the system to obtain the reactive barrier compound of the above structure. Fuel agent 177.31g.
[0080] 1 H NMR (CDCl 3 ,500MHz): δ7.32~7.16(m, 10H, Ar-H), 6.81~6.72(m, 8H, Ar-H), 4.75~4.71(s, 2H, Ar-OH), 3.81~3.75(...
Embodiment 3
[0082] The structure of the reactive flame retardant of the present embodiment is as follows:
[0083]
[0084] The preparation method of this reactive flame retardant is as follows:
[0085] Put 2 mol of phosphorus oxychloride and 200 mL of acetone into a three-port 2000 ml glass reactor with a stirring device, pass in nitrogen gas, add 1 mol of p-1,4-cyclohexanediol disodium dropwise for 30 minutes under stirring, continue the reaction at room temperature for 60 minutes, and then Add 4 mol disodium methylhydroquinone dropwise, continue the reaction at room temperature for 120 min, add 4L 1mol / L hydrochloric acid dropwise, wash with water until neutral after the reaction, remove impurities and water in the system by physical methods, and distill off the solvent in the system to obtain the above Structured reactive flame retardant 251.76g.
[0086] 1 H NMR (CDCl 3 ,500MHz): δ6.92~6.83(m, 12H, Ar-H), 4.78~4.72(s, 4H, Ar-OH), 4.12~4.06(m, 2H, CH), 2.38~2.33(s, 12H , CH 3...
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