Preparation method of vinylene carbonate
A technology of vinylene carbonate and ethylene carbonate, which is applied in the field of preparation of vinylene carbonate, can solve the problems of hydrogen generation, high reaction temperature, and negative impact of safety protection measures required by equipment, and achieve high yield and simple separation and purification , to overcome the effect of bad influence
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Embodiment 1
[0025] Vacuumize the 1L four-necked bottle connected with the water separator, and replace it with nitrogen for 3 times. Under nitrogen atmosphere, add 352g of benzene, 176g of ethylene carbonate, and 333g of selenium dioxide; then heat to reflux and divide water for 36 hours, and the reaction ends After cooling to room temperature, suction filtration under reduced pressure, the filter cake was washed with a small amount of benzene, the filtrate and washing liquid were combined, then the benzene was evaporated at normal pressure, and the product vinylene carbonate was obtained by rectification under reduced pressure, with a yield of 43.4%, a purity of 99.93%.
Embodiment 2
[0027] Vacuumize the 1L four-necked bottle connected with the water separator, and replace it with nitrogen for 3 times. Under nitrogen atmosphere, add 352g of benzene, 176g of ethylene carbonate, 333g of selenium dioxide and 0.24g of glacial acetic acid, heat to reflux and divide water for 30 hour, after the end of the reaction, cool to room temperature, filter under reduced pressure, wash the filter cake with a small amount of benzene, combine the filtrate and washing liquid, then steam the benzene at normal pressure, and rectify under reduced pressure to obtain the product vinylene carbonate, the yield 44.1%, purity 99.95%.
Embodiment 3
[0029] Vacuumize the 1L four-necked bottle connected with the water separator, and replace it with nitrogen three times. Under nitrogen atmosphere, add 352g of benzene, 176g of ethylene carbonate, 333g of selenium dioxide and 0.3g of glacial acetic acid, and heat to reflux for 24 hour, after the end of the reaction, cool to room temperature, filter under reduced pressure, wash the filter cake with a small amount of benzene to combine the filtrate and washing liquid, then steam the benzene under normal pressure, and rectify under reduced pressure to obtain the product vinylene carbonate, the yield is 45.1 %, purity 99.95%.
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