Preparation method of phosphate ester compound
A technology for phosphate esters and compounds, applied in the field of phosphate ester compounds, can solve the problems of many by-products, complicated post-processing and high cost, and achieve the effects of reducing the generation of three wastes, simple post-processing and fewer reaction steps.
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Embodiment 1
[0042] Embodiment 1: the synthesis of triethyl phosphate
[0043] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold toluene to form a mixture of toluene and ethyl chloride. Add 6.2 g of benzyltriethylammonium bromide and toluene ethyl chloride mixture to the autoclave in turn. Seal the autoclave, heat up to 110°C with stirring, and keep it warm for 20 hours. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of toluene. All the toluene solutions obtained in the above process were combined and added to a 500mL single-necked round bottom flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distilled under re...
Embodiment 2
[0044] Embodiment 2: the synthesis of triethyl phosphate
[0045] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold xylene to form a mixture of xylene chloride and ethyl chloride. Add 6.2 g of benzyltriethylammonium chloride and xylene chloride into the autoclave in turn. Seal the autoclave, heat up to 130°C with stirring, and keep the temperature for 20 hours. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of xylene. All the xylene solutions obtained in the above process were combined and added into a 500mL single-necked round-bottomed flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distilled und...
Embodiment 3
[0046] Embodiment 3: the synthesis of triethyl phosphate
[0047] Experimental operation: Add 97g of sodium diethyl phosphate obtained from wastewater treatment into a 1000mL autoclave. Add 112g of cold ethyl chloride to 350mL of cold xylene to form a mixture of xylene chloride and ethyl chloride. Add 9.3g of tetrabutylammonium bromide and xylene chloride ethyl ethane mixture to the autoclave in turn. Seal the autoclave, heat up to 130°C with stirring, and keep the temperature for 5h. After the reaction was completed, the autoclave was turned off and heated, and the temperature was naturally lowered to 50° C. under stirring. The reaction system was filtered and separated, and the filter cake was washed 3 times with 70 mL of xylene. All the xylene solutions obtained in the above process were combined and added in a 500mL single-necked round-bottomed flask, concentrated under reduced pressure to obtain the crude product of triethyl phosphate, and the crude product was distille...
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