Method for preparing hexyl-dioctyl phosphorus oxide

[0025] Add 2g of dioctylphosphine oxide (0.007mol), 1.52g of 1-hexene (0.018mol), 10ml of acetic acid, 0.2g of di-tert-butyl peroxide into a 25ml PTFE reactor, mix a small amount of decene, and stir to dissolve , heated up to 140°C, and reacted for 12 hours. 31 P-NMR detection reaction is complete. Add 5 wt% dilute hydrochloric acid to the reaction solution to break the emulsion and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 81.5%.

[0027] Add 2g of dioctylphosphine oxide (0.007mol), 1.52g of 1-hexene (0.018mol), 10ml of acetic acid, 0.4g of di-tert-butyl peroxide into a 25ml PTFE reactor, mix a small amount of decene, and stir to dissolve , heated up to 130°C, and reacted for 36 hours. 31 P-NMR detection reaction is complete. Add 15wt% dilute hydrochloric acid to the reaction solution to break the emulsion and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 81.8%.

[0029] Add 2g of dioctylphosphine oxide (0.007mol), 1.52g of 1-hexene (0.018mol), 10ml of acetic acid, 0.3g of di-tert-butyl peroxide into a 25ml PTFE reactor, mix a small amount of decene, and stir to dissolve , heated up to 135°C, and reacted for 24 hours. 31 P-NMR detection reaction is complete. Add 10wt% dilute hydrochloric acid to the reaction solution to break the emulsification and wash it, and extract it with chloroform. The organic layer is washed with water until neutral, and the chloroform and unreacted olefins are evaporated by a rotary evaporator. Recrystallization from ethanol, filtration, and vacuum drying afforded a white solid. Yield 83%.