Method for preparing monochloroethylene carbonate

A technology of monochloroethylene carbonate and ethylene carbonate, which is applied in the field of preparation of monochloroethylene carbonate, can solve the problem of low yield of monochloroethylene carbonate products, low yield of monochloroethylene carbonate, and the inability to enter industrial production and other problems, to achieve the effect of low equipment requirements, improved cycle performance, and fast response speed

Active Publication Date: 2008-02-20
BYD CO LTD
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AI Technical Summary

Problems solved by technology

[0004] Later, there was also a process research report on the preparation of chloroethylene carbonate by chlorination of ethylene carbonate powder directly under ultraviolet light catalysis without solvent, but it was found that in the absence of solvent, due to uneven reaction, resulting in monochlorocarbonic acid The yield of vinyl ester is very low and there is no prospect of industrial application
About using other solvents such as solvents such as ether, ethanol to replace carbon tetrachloride as the research of chlorination reaction solvent, also someone has carried out the research of this respect, but all can not enter industrial production because of the low yield of chloroethylene carbonate product
[0005] In addition, Sun Hao and Cai Chun of Nanjing University of Science and Technology disclosed a preparation method of monochloroethylene carbonate in "Petrochemical Industry", 2005, 34 (10), 977-979. Nitrile is used as an initiator to react ethylene carbonate and sulfuryl chloride at a temperature of 90°C for 1-1.5 hours. The molar ratio of ethylene carbonate, sulfuryl chloride and azobisisobutyronitrile is 1:1.25:0.002, and chloroethylene carbonate The yield is lower, only 65%

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  • Method for preparing monochloroethylene carbonate
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  • Method for preparing monochloroethylene carbonate

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preparation example Construction

[0015] The method for preparing chloroethylene carbonate of the present invention can be represented by following chemical reaction formula (III):

[0016]

[0017] In the above reaction, there is no special limitation on the amount of the initiator added, which can be the amount of conventional initiators. Sulfuryl chloride and ethylene carbonate can be added according to the stoichiometric ratio, and excessive sulfuryl chloride can also be added, and excessive ethylene carbonate can also be added. In order to make the reaction more thorough, one of them is usually excessive. Considering that the sulfuryl chloride raw material is easy to get And it is easy to remove from the product after the reaction, so sulfuryl chloride is preferably in excess. Preferably, the weight ratio of the 2,4,2,4-tetrachlorobenzoyl peroxide, sulfuryl chloride and ethylene carbonate is (0.001-0.05): (1-2): 1, more preferably ( 0.001-0.0075):(1-2):1.

[0018] The present invention does not have ...

Embodiment 1

[0034] This embodiment is used to illustrate the preparation method of chloroethylene carbonate provided by the present invention.

[0035] Add 100 grams of ethylene carbonate to a 500 ml four-necked round-bottomed flask equipped with a stirrer, put the round-bottomed flask in a water bath, then slowly feed dry nitrogen into the device for 10 minutes, heat the water bath to make the temperature in the flask When rising to 50°C, start to add 158.5 grams of sulfuryl chloride dropwise under stirring, then add 1.08 grams of DCBP dissolved in 50 milliliters of benzene into the four-necked round-bottomed flask at the same time after adding 20 milliliters of sulfuryl chloride dropwise. After 3 hours of reaction, the above reaction solution was transferred to a 500 ml single-necked flask for vacuum distillation, and 140 grams of colorless fractions with a system pressure of 3 mm Hg and a temperature of 88-92° C. were collected. 140 g of the colorless fraction obtained were subjected t...

Embodiment 2

[0037] This embodiment is used to illustrate the preparation method of chloroethylene carbonate provided by the present invention.

[0038] Add 100 grams of ethylene carbonate to a 500 ml four-necked round-bottomed flask equipped with a stirrer, put the round-bottomed flask into a water bath, then slowly feed dry argon into the device for 10 minutes, heat the water bath to make the When the temperature rose to 90°C, 288.5 grams of sulfuryl chloride began to be added dropwise under stirring, and then 0.88 grams of DCBP dissolved in 50 milliliters of benzene was added dropwise to the four-necked round-bottomed flask after adding 20 milliliters of sulfuryl chloride dropwise. Both were 4.5 ml / min. After 3 hours of reaction, the above reaction solution was transferred to a 500 ml single-necked flask for vacuum distillation, and 141 grams of colorless fractions with a system pressure of 3 mmHg and a temperature of 88-92°C were collected. The resulting 141 g colorless fraction was su...

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Abstract

An ethylene carbonate chloride preparation method is that ethylene carbonate and sulfuryl chloride are contacted and reacted with the existing of an initiator of 2, 4, 2, 4-tetrachlorobenzoyl peroxide. The yield of ethylene carbonate chloride provided by the invention is as high as 93 percent or over, and the product is easily separated and purified, with the purity rate being 98 percent. Besides, as the toxicity of suffuryl chloride is much lower than the toxicity of carbon tetrachloride, the requirement to equipment is comparatively lower, and the operation is safer, thus being suitable for the requirements of industrial mass production.

Description

technical field [0001] The present invention relates to a preparation method of chloroethylene carbonate, in particular to a method for preparing monochloroethylene carbonate with ethylene carbonate as raw material. technical background [0002] Lithium-ion secondary battery is a newly developed green energy in the 1990s. It is favored by the world for its high reversible capacity, high voltage, high cycle performance and high energy density. It is called the leading power source in the 20th century. , and its application fields continue to expand. Cycle performance is an important index to measure lithium-ion secondary batteries. Adding a certain amount of chloroethylene carbonate, vinylene carbonate and other substances to the electrolyte can promote the formation of SEI film and enhance the cycle performance of lithium-ion secondary batteries. . [0003] J.Am.Chem.Soc., 1955,77,3789-3793 and CN 1733756A all disclose a kind of preparation method of monochloroethylene car...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42C07D317/40
Inventor 史国强先雪峰刘会权
Owner BYD CO LTD
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