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 polluting the environment, declining mechanical properties, affecting human and animal health, 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 2 mol of phosphorus trichloride 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 hydroquinone dropwise for 30 minutes under stirring, continue to react at room temperature for 60 minutes, and then add 4 mol of ethylene dichloride dropwise Disodium mercaptide, continue to react at room temperature for 120min, add 2L of 1mol / L hydrochloric acid dropwise, wash with water until neutral after 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 206.92g.
[0074] 1 H NMR (CDCl 3 ,500MHz): δ6.98~6.74(m, 4H, Ar-H), 2.54~2.36(m, 16H, CH 2 ), 2.32-2.25 (t, 4H, SH).
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 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 ethanedithiol dropwise, continue the reaction at room temperature for 120 minutes, add 4L 1mol / L hydrochloric acid dropwise, after the reaction, use physical methods to remove impurities and water in the system, and distill off the solvent in the system to obtain the reactivity of the above structure Flame retardant 245.54g.
[0080] 1 H NMR (CDCl 3 ,500MHz): δ4.52~4.46(t, 8H, CH 2 ), 3.95~3.88(m, 2H, CH), 2.54~2.36(m, 8H, CH 2 ), 2.32~2.25(t, 4H, SH), 1.45~1.32(m, 8H, CH ...
Embodiment 3
[0082] The structure of the reactive flame retardant of the present embodiment is as follows:
[0083]
[0084] Put 2mol tert-butyl dichlorophosphoric acid, 200mL ethanol, 1mol 1,4-butylene diamine, 0.1mol sodium hydroxide, 0.1g DMAP into a three-port 2000ml glass reactor with stirring device, heat up to ethanol reflux, and react for 8h under stirring , then add 2mol 2-aminothiophenol, continue the reaction at room temperature 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 flame retardant with the above structure 242.17g.
[0085] 1 H NMR (CDCl 3 ,500MHz): δ7.77~7.61(m, 4H, PONH), 7.07~6.92(m, 8H, Ar-H), 4.61~4.55(s, 2H, Ar-SH), 4.51~4.45(m, 4H , CH 2 ), 1.53~1.42 (m, 4H, CH 2 ), 0.95~0.89 (s, 18H, CH 3 ).
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