Preparation method of phosphorus oxime-containing flame retardant
A flame retardant and solvent technology, applied in the field of organic chemistry and polymer material synthesis, can solve the problems of insufficient improvement of flame retardancy and heat resistance, easy hydrolysis, etc., to achieve safe escape and fire fighting time, flame retardant Performance Hydrolysis resistance, loss reduction effect
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Embodiment 1
[0033] Add 30 parts of 4,4'-dihydroxybenzophenone, 350 parts of xylene, and 12.5 parts of triethylamine into a reaction vessel equipped with a mechanical stirring and temperature control device. Blow nitrogen, stir for 30 minutes, add 82.5 parts of diphenyl chlorophosphate, and stir at 20-30°C for 1 hour after the addition, the system turns from cloudy to clear, add water to quench the reaction, evaporate the solvent under reduced pressure, and extract 3 times with dichloromethane, The organic phase was washed 3 times with deionized water, dichloromethane was evaporated to dryness under reduced pressure to obtain a colorless liquid, and the product was separated and purified by column chromatography (petroleum ether: ethyl acetate=5:1, V / V) to obtain a white solid DHPP .
Embodiment 2
[0035] Add 132 parts of DHPP, 180 parts of ethanol, 20.4 parts of hydroxylamine hydrochloride and 39.6 parts of sodium acetate trihydrate into a reaction vessel equipped with a mechanical stirring and temperature control device. After the addition was complete, stir at 20-30°C for 4 h; evaporate the solvent to dryness under reduced pressure, then extract 3 times with dichloromethane, wash the organic phase 3 times with deionized water, evaporate the dichloromethane to dryness under reduced pressure, and use column chromatography (PE:EA =4:1, V / V) separation and purification to obtain DHPP-NOH.
Embodiment 3
[0037] Add 253.6 parts of DHPP-NOH, 220 parts of toluene, 7.2 parts of triethylamine, and 26.4 parts of p-phenylene diisocyanate into a reaction vessel equipped with a reflux device, a temperature control device, and a mechanical stirring device, and stir at 110°C for 6 hours under reflux; The solvent was dried, the system was extracted 3 times with dichloromethane, and the organic phase was washed 3 times with deionized water. Dichloromethane was evaporated to dryness under reduced pressure. DHPP-NOH-NCO was obtained by separation and purification by column chromatography (petroleum ether: ethyl acetate = 3:1, V / V).
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