Preparation method of vinylene carbonate for lithium cell
A technology of vinylene carbonate and ethylene carbonate is applied in the field of preparation of vinylene carbonate for lithium batteries, and can solve problems such as difficult separation
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Embodiment 1
[0024] 0.05g of diisopropyl peroxydicarbonate was fully dissolved in 100ml of solvent for subsequent use. 500 g of raw material ethylene carbonate (99% purity) was first melted in an oven at 80° C., and then added to the reactor. Nitrogen was passed through the reactor so that the entire reaction was carried out under a nitrogen atmosphere. When the material temperature in the reactor reached 20° C., 80 ml of initiator solution was added, and simultaneously, 881.6 g of sulfuryl chloride (purity 95%) was added dropwise, which was continuously added dropwise. After the sulfuryl chloride has been added completely, get 20ml of previously prepared initiator solution and add, and stop after another 4 hours of reaction to obtain monochloroethylene carbonate. As a result of gas chromatography analysis, the purity of vinyl monochloride is 65.7%, and the yield can reach 73%.
Embodiment 2
[0026] 0.05g of diisopropyl peroxydicarbonate was fully dissolved in 100ml of solvent for later use. 500 g of raw material ethylene carbonate (99% purity) was first melted in an oven at 80° C., and then added to the reactor. Nitrogen was passed through the reactor so that the entire reaction was carried out under a nitrogen atmosphere. When the material temperature in the reactor reached 30° C., 80 ml of initiator solution was added, and 881.6 g of sulfuryl chloride (purity 95%) was added dropwise at the same time, which was continuously added dropwise. After the sulfuryl chloride has been added completely, get 20ml of previously prepared initiator solution and add, and stop after another 4 hours of reaction to obtain monochloroethylene carbonate. As a result of gas chromatography analysis, the purity of vinyl chloride was 74.2%, and the yield could reach 76%.
Embodiment 3
[0028] 0.05g of diisopropyl peroxydicarbonate was fully dissolved in 100ml of solvent for later use. 500 g of raw material ethylene carbonate (99% purity) was first melted in an oven at 80° C., and then added to the reactor. Nitrogen was passed through the reactor so that the entire reaction was carried out under a nitrogen atmosphere. When the material temperature in the reactor reached 40° C., 80 ml of initiator solution was added, and 881.6 g of sulfuryl chloride (purity 95%) was added dropwise at the same time, which was continuously added dropwise. After the sulfuryl chloride has been added completely, get 20ml of previously prepared initiator solution and add, and stop after another 4 hours of reaction to obtain monochloroethylene carbonate. As a result of gas chromatography analysis, the purity of vinyl chloride was 51.4%, and the yield was 56%.
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