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

Inactive Publication Date: 2009-02-18
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a kind of method of producing vinylene carbonate from ethylene carbonate, the two-step synthetic process route principle of this method application is completely consistent with above preparation vinylene carbonate technology, but a kind of technological improvement to aforementioned synthetic method : On the one hand, in the synthesis process of chlorinated ethylene carbonate, different new initiators are selected and quoted, so that the reaction can be completed at a lower temperature and in a shorter time; on the other hand, in the dechlorination process, new Composite antioxidant, instead of the polymerization inhibitor usually added in the prior art, overcomes the shortcomings of easy polymerization and difficult separation of the product in the preparation method of the prior art, and improves the synthetic purity of the final product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The present invention provides a preparation method of vinylene carbonate used in a lithium battery, which is a technical improvement of the prior synthesis method. On one hand, in the synthesis process of chlorinated ethylene carbonate, different novel initiators are used so that the reaction can be completed within a shorter period of time at the lower temperature; on the other hand, a novel composite antioxidant is added in the technical process of dechlorination, instead of adding a common inhibitor in the prior art. Therefore, the present invention overcomes the defects in the prior preparation method that the products can be easily polymerized and can not be easily separated, and has the advantage that the synthesis purity of the final product is enhanced.

Description

technical field [0001] The present invention relates to the production technology of lithium ion battery electrolyte, is a kind of preparation method of vinylene carbonate for lithium battery; It relates to a kind of preparation method of vinylene carbonate from monochloroethylene carbonate. Background technique [0002] Vinylene carbonate is an electrolyte additive for lithium-ion batteries, which can significantly increase the initial capacity of the battery and improve the performance of the SEI film, thereby improving the charge-discharge efficiency and cycle characteristics of lithium-ion secondary batteries. Its unique structure has attracted high attention in the field of lithium-ion batteries are of broad interest to molecular chemists and are therefore receiving increasing attention. [0003] The main principle of the production method of vinylene carbonate is the same, that is, first ethylene carbonate monochlorination, and then dehydrochlorination. The difference...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/40
Inventor 刘锦平赵洪宋晓莉李晓磊
Owner CHINA NAT OFFSHORE OIL CORP
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