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Preparation method of ethylene carbonate

A technology of vinylene carbonate and chloroethylene carbonate, applied in the field of preparation of vinylene carbonate, can solve problems such as high cost and inability to be applied on a large scale, and achieve the effect of reducing adverse effects

Inactive Publication Date: 2019-01-04
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods are too costly to be applied on a large scale

Method used

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Examples

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preparation example Construction

[0029] In order to solve these problems, a specific embodiment of the present invention provides a kind of preparation method of vinylene carbonate, described method comprises: in the presence of catalyst, make described chloroethylene carbonate and organic amine react in organic solvent , generate vinylene carbonate; Wherein, the catalyst is potassium bromide, sodium bromide, sodium iodide, potassium iodide or any combination thereof and 18-crown-6, tetrabutylammonium bromide or a mixture thereof, A mixture of potassium bromide and tetrabutylammonium bromide is preferred.

[0030] In the mixture of the present invention, the ratio of potassium bromide, sodium bromide, sodium iodide, potassium iodide or any combination thereof to 18-crown-6, tetrabutylammonium bromide or their combination is not special limit. For economic considerations, in a specific embodiment, in terms of mass, the potassium bromide, sodium bromide, sodium iodide, potassium iodide or any combination there...

Embodiment 1

[0055] This example illustrates a method of preparing vinylene carbonate comprising:

[0056] (a) Pass dry chlorine into 200kg of ethylene carbonate heated to 60°C, add 60kg of free radical initiator azobisisobutyronitrile in batches to react, and the reaction ends after 6 hours;

[0057] (b) Get 150kg of monochloroethylene carbonate generated by the reaction of step (a), join in dimethyl carbonate, then add polymerization inhibitor 2,6-di-tert-butyl-4-methylphenol 7.5kg, catalyst 7.5kg (the mass ratio of potassium bromide and tetrabutylammonium bromide is 1:3), then triethylamine is added dropwise; the reaction temperature is controlled at 5° C., and the reaction time is 4 hours; and

[0058] (c) filtering and rectifying the reaction product obtained in step (b), and then controlling the temperature to freeze and crystallize within the range of 10-20° C., thereby obtaining vinylene carbonate with a purity greater than 99.5% and a yield of 86%.

Embodiment 2

[0060] This example illustrates a method of preparing vinylene carbonate comprising:

[0061] (a) Pass dry chlorine into 200kg of ethylene carbonate heated to 60°C, add 50kg of free radical initiator azobisisoheptanonitrile in batches to react, and the reaction ends after 6 hours;

[0062] (b) get the monochloroethylene carbonate 150kg that step (a) reacts to generate, join in ethyl acetate, then add polymerization inhibitor 1,4-benzoquinone 6kg, catalyst 6kg (potassium bromide and tetrabutyl bromide The mass ratio of ammonium chloride is 1:2), then piperidine is added dropwise; the reaction temperature is controlled at 2° C., and the reaction time is 1 hour; and

[0063](c) filtering and rectifying the reaction product obtained in step (b), and then controlling the temperature to freeze and crystallize within the range of 10-20° C., thereby obtaining vinylene carbonate with a purity greater than 99.3% and a yield of 85%.

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Abstract

The invention belongs to the field of lithium battery electrolyte additive preparation, and particularly relates to a preparation process of ethylene carbonate. The method comprises: making monochloroethylene carbonate react with organic amine in an organic solvent in the presence of a catalyst; wherein the catalyst is a mixture of potassium bromide, sodium bromide, sodium iodide, potassium iodide, or any combination thereof and 18-crown ethers-6, tetrabutylammonium bromide or a combination thereof. The preparation method of the ethylene carbonate can improve a yield, the reaction condition ismild and environment-friendly.

Description

technical field [0001] The invention belongs to the field of manufacturing electrolyte additives for lithium batteries, and in particular relates to a preparation method of vinylene carbonate. technical background [0002] Vinylene carbonate, also known as 1,3-dioxol-2-one or ethylene carbonate, is a colorless transparent liquid, used as a new type of organic film-forming additive and overcharge protection additive for lithium-ion batteries , It can also be used as a fine chemical intermediate for the preparation of polymer compounds polyvinyl carbonate or aromatic benzils. [0003] At present, the stability and service life of lithium batteries are one of the current research hotspots. Vinylene carbonate is currently one of the most suitable additives to solve the problem of lithium battery safety and stability, and it is also one of the most scientific research and practical use of battery additives. Using about 3% vinylene carbonate as an electrolyte additive can form a...

Claims

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Application Information

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IPC IPC(8): C07D317/40
CPCC07D317/40
Inventor 吴国栋沈鸣李伟峰杨志勇孙昌标袁青海
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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