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ChemicalBook CAS DataBase List Chloroethylene carbonate
3967-54-2

Chloroethylene carbonate synthesis

7synthesis methods
-

Yield:3967-54-2 93.2%

Reaction Conditions:

with iron(III) chloride;3,6-dimethyl-3,6-dihydroperoxy-4,5-dioxaoctane at 60; for 0.5 h;Inert atmosphere;Reagent/catalyst;

Steps:

3
1) in the material of stainless steel packed tower reactor, along the tower height, every 1 meter for a packing layer, the installation of a bracket for supporting the filler, the filler for the transparent polyester material, each bracket at the bottom of the installation A first mercury leachate lamp in which a liquid distributor and a second mercury leachate lamp are respectively installed above each packing, the liquid distributor is fixed to the support for liquid dispersion, the second mercury infusion The first mercury immersion lamp and the second mercury immersion lamp are both used for light irradiation filler, the total filling height is 12 meters, and the first mercury immersion lamp and the second mercury leaching Liquid lamps are explosion-proof, power 800W;2) 1000 kg of ethylene carbonate preheated to 60 ° C, the ethylene carbonate from the solid into a liquid, then add 1 kg of methyl ethyl ketone peroxide and 5 kg of ferric chloride, stir well, heated to 60 ° C, containing methyl ethyl ketone peroxide and Ferric chloride liquid of ferric chloride;3) from the bottom of the bottom of the nitrogen for 30 minutes, replace the tower air, nitrogen exhaust vent;4) After drying and dehydration, the chlorine gas is heated to 65 ° C. At the bottom of the column and the middle of the column are passed with chlorine gas, the volume of chlorine gas is passed from the bottom of the column: the volume of chlorine gas is passed from the middle of the column = 1: 2, Peristaltic pump added 2) obtained by the methyl ethyl ketone peroxide and ferric chloride vinyl carbonate liquid, the control of chlorine and ethylene carbonate molar ratio of 1.03: 1, gas-liquid counter-current contact reaction, keep the tower temperature of 60-70 And the liquid monochlorocarbonate was collected at the bottom of the column. The yield of vinyl chlorocarbonate was 93.2% and the purity was 99.9%.

References:

Tangshan Hanbai Chemical Co. Ltd.;Zhang, Jiansheng;Wang, YiMin;Zhang, Jinzong;Yan, Qingshan;Guo, LianWu CN105859677, 2016, A Location in patent:Paragraph 0039-0043

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