Method for catalytically synthesizing triethyl phosphate by phase transfer
A technology of triethyl phosphate and phase transfer catalysis, which is applied in the direction of chemical instruments and methods, physical/chemical process catalysts, compounds of Group 5/15 elements of the periodic table, etc., and can solve difficult-to-handle and pollution caused by sodium diethyl phosphate Environmental, triethyl phosphate yield reduction and other issues, to achieve the effect of simple operation, lower synthesis cost, and easy industrial production
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Embodiment 1
[0026] Get 176.0g of diethyl phosphate sodium salt, 12.89g of tetrabutylammonium bromide, 400ml of mixed solvent toluene and 30ml of water and join in the reactor equipped with reflux condenser, feeding funnel, stirring device and thermometer, heat and stir to make phosphoric acid Dissolve diethyl ester sodium salt and tetrabutylammonium bromide, raise the temperature to reflux, add 154.18g diethyl sulfate, keep the reflux reaction for 6h, cool, and filter with suction to obtain a yellow solution, then wash with saturated sodium bicarbonate until neutral , washed twice with water and once with saturated sodium chloride, dried over anhydrous magnesium sulfate, and finally the solvent was rotary evaporated to obtain crude triethyl phosphate, a yellow transparent liquid with a yield of 63.61% to 91.30% and a content of 95%. Distill under reduced pressure to obtain pure triethyl phosphate, a colorless transparent liquid with a refractive index n=1.4055 and a content of 99%.
Embodiment 2
[0028] Get 176.0g of diethyl phosphate sodium salt, 14.58g of cetyltrimethylammonium bromide, 500ml of mixed solvent xylene and 80ml of water, and add them to the reactor equipped with reflux condenser, feeding funnel, stirring device and thermometer , heat and stir to dissolve diethyl phosphate sodium salt and catalyst, raise the temperature to reflux, add 154.18 g of diethyl sulfate, keep reflux reaction for 4 hours, cool, filter with suction to obtain a yellow solution, and then wash with saturated sodium bicarbonate to medium Then wash twice with water and once with saturated sodium chloride, dry over anhydrous magnesium sulfate, and finally spin the solvent to obtain crude triethyl phosphate, a yellow transparent liquid, with a yield of 62.70% to 91.65% and a content of 95%. Distill under reduced pressure to obtain pure triethyl phosphate, a colorless transparent liquid with a refractive index n=1.4055 and a content of 99%.
Embodiment 3
[0030] Get diethyl phosphate sodium salt 176.0g, benzyltriethylammonium chloride 9.09g, mixed solvent chlorobenzene 600ml and water 100ml, join in the reactor that reflux condenser, addition funnel, stirring device and thermometer are housed, Heat and stir to dissolve diethyl phosphate sodium salt and catalyst, raise the temperature to reflux, add 77.09 g of diethyl sulfate, keep reflux reaction for 7 hours, cool, filter with suction to obtain a yellow solution, then wash with saturated sodium bicarbonate until neutral, Wash twice with water and once with saturated sodium chloride, dry over anhydrous magnesium sulfate, and finally spin evaporate the solvent to obtain crude triethyl phosphate, a yellow transparent liquid, with a yield of 53.69% to 91.30% and a content of 95%. Distill under reduced pressure to obtain pure triethyl phosphate, a colorless transparent liquid with a refractive index n=1.4055 and a content of 99%.
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