A novel preparation of aluminum diethylphosphinate(AlPi) was carried out with free-radical addition reaction by means of UV-irradiation under atmospheric pressure.A solution of sodium hypophosphite was treated with ...A novel preparation of aluminum diethylphosphinate(AlPi) was carried out with free-radical addition reaction by means of UV-irradiation under atmospheric pressure.A solution of sodium hypophosphite was treated with ethylene and irradiated with ultraviolet light in the presence of an amount of photoinitiator effective to initiate the free-radical reaction between the hypophosphite anion and the double bond of the ethylene molecule.The ethylene was micro-bubbled into the reaction mixture with the addition of the photoinitiator,and the gas-liquid contact surface and the photoinitiator concentration in the gas-liquid interface were increased largely.The yield of the final product could be improved to about 96%.The contents of P,Al in samples were detected by ICP,and the molecular structure of the samples was confirmed by ^(31)P NMR,~1H NMR and FTIR spectroscopic analysis.Thermal stability of the final products was investigated in detail by TG-DTA.展开更多
基金support by Zhenxing Chemistry Co.,Ltd(Tianjin,China)
文摘A novel preparation of aluminum diethylphosphinate(AlPi) was carried out with free-radical addition reaction by means of UV-irradiation under atmospheric pressure.A solution of sodium hypophosphite was treated with ethylene and irradiated with ultraviolet light in the presence of an amount of photoinitiator effective to initiate the free-radical reaction between the hypophosphite anion and the double bond of the ethylene molecule.The ethylene was micro-bubbled into the reaction mixture with the addition of the photoinitiator,and the gas-liquid contact surface and the photoinitiator concentration in the gas-liquid interface were increased largely.The yield of the final product could be improved to about 96%.The contents of P,Al in samples were detected by ICP,and the molecular structure of the samples was confirmed by ^(31)P NMR,~1H NMR and FTIR spectroscopic analysis.Thermal stability of the final products was investigated in detail by TG-DTA.