Vinylene carbonate preparation method
A technology of vinylene carbonate and ethylene carbonate, which is applied in the field of preparation of vinylene carbonate, can solve the problems of unavailable, unstable results, difficult to repeat, etc., to facilitate removal, stable reaction results, and prevent polymerization Effect
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[0021] (1) Synthesis of monochloroethylene carbonate:
[0022] Take 400g of ethylene carbonate and put it into a cylindrical reactor (diameter 400mm, height 1000mm), add CCl 4 Solvent 800ml, use pure nitrogen to remove the air, under the irradiation of 20W ultraviolet light, in 65 ℃ water bath, pass chlorine gas for 6 hours, consume 400g of chlorine gas in total, and pass pure nitrogen gas at the same time to stir (flow rate 2 liters / min·400g sulfite Vinyl ester) After the reaction was completed, the solvent was reclaimed by atmospheric distillation to obtain 588g of crude product, gas chromatography analysis results: monochloride content 77.12%, dichloride 8.66, ethylene carbonate 8.84%, solvent 4.65%, the crude product was decompressed (20mmHg) distillation, get the front cut (70~90 ℃) 48g, gas chromatography analysis result: monochloride content 42.61%, dichloride 49.58%, ethylene carbonate 2.98%, solvent 4.43%; Get back cut ( 95°C) 499g.
[0023] Gas chromatography analy...
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