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Method for synthesizing vinylene carbonate

A technology of vinylene carbonate and ethylene carbonate, which is applied in the field of improved synthesis, can solve unsatisfactory problems and achieve the effects of lowering melting point, lowering cost and reducing loss

Active Publication Date: 2012-02-29
江苏瀚康新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the use of a single solvent is not ideal for this reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In a 2-liter four-neck flask, add 400 g of chloroethylene carbonate, 500 g of methyl acetate, and 500 g of toluene, then add 7 g of polymerization inhibitor BHT, and put it into a heating mantle. Add a stirring device, thermometer, reflux condenser and 500ml constant pressure dropping funnel. Raise the temperature of the raw materials in the flask to 60°C, then drop 320g of triethylamine into the flask at a uniform rate with a dropping funnel, and control the dropping within 4 to 6 hours, and control the temperature at 55 to 65°C. After the dropwise addition, keep the temperature and continue the reaction for 12 hours, then transfer the reaction product to a flat cylindrical filter, pressurize with nitrogen, the maximum pressure is not more than 0.2Mpa, and obtain a black filtrate and filter residue; the weight of the filter residue is 574.7g , 105 ℃ × 3 hours volatile matter content is 32.15%, the content of water-insoluble matter in salt slag is 8.95%. The filtrate w...

Embodiment 2

[0030] In a 2-liter four-neck flask, add 400 g of chloroethylene carbonate, 400 g of ethyl acetate, 500 g of tetrahydrofuran, and 100 g of n-hexane, and then add 7 g of polymerization inhibitor BHT, and put it into a heating mantle. Add a stirring device, thermometer, reflux condenser and 500ml constant pressure dropping funnel. Raise the temperature of the raw materials in the flask to 60°C, then drop 320g of triethylamine into the flask at a uniform rate with a dropping funnel, and control the dropping within 4 to 6 hours, and control the temperature at 55 to 65°C. After the dropwise addition, keep the temperature and continue the reaction for 12 hours, then transfer the reaction product to a flat cylindrical filter, pressurize with nitrogen, the maximum pressure is not more than 0.2Mpa, and obtain a black filtrate and filter residue; the filter residue weighs 477.7g , 105 ℃ × 3 hours volatile matter content is 16.73%, the content of water-insoluble matter in salt slag is 7....

Embodiment 3

[0032]In a 2-liter four-neck flask, add 400g of chloroethylene carbonate, 400g of ethyl propionate, 200g of diethyl carbonate, 200g of n-heptane and 200g of ethylene glycol dimethyl ether, and then add 7g of inhibitor Agent BHT, placed in a heating mantle. Add a stirring device, thermometer, reflux condenser and 500ml constant pressure dropping funnel. Raise the temperature of the raw materials in the flask to 60°C, then drop 320g of triethylamine into the flask at a uniform rate with a dropping funnel, and control the dropping within 4 to 6 hours, and control the temperature at 55 to 65°C. After the dropwise addition, keep this temperature and continue the reaction for 12 hours, then transfer the reaction product to a flat cylindrical filter, pressurize with nitrogen, the maximum pressure is not more than 0.2Mpa, and obtain a black filtrate and filter residue; the filter residue weighs 472g, The volatile matter content at 105°C for 3 hours is 11.91%, and the water-insoluble ...

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Abstract

The invention discloses a method for synthesizing vinylene carbonate, and the method mainly comprises the following steps: (1) chlorine gas is introduced into the raw material of ethylene carbonate in ultraviolet light condition, thus synthesizing chlor-ethylene carbonate; (2) taking mixture of ester, ether and hydrocarbon as the organic solvent, the chlor-ethylene carbonate which is obtained in the step (1) produces elimination reaction with triethylamine, thus eliminating hydrogen chloride and generating the vinylene carbonate; and (3) the mixed product obtained in the step (2) is distilledand purified after filtration. By adopting the mixed solvent of ester, ether and hydrocarbon, the reaction product is easily isolated from triethylamine hydrochloride, thus increasing the yield and the production efficiency; and BHT can be used as a polymerization inhibitor in the reaction process, thus controlling the polymerization of the vinylene carbonate effectively and increasing the yield.

Description

technical field [0001] The invention relates to an improved synthesis method of a non-aqueous electrolyte additive—vinylene carbonate. Background technique [0002] Electrolyte is an important raw material in lithium-ion secondary batteries, which has a very important impact on various performances of batteries. In recent years, with the continuous development of the application of lithium-ion batteries, users have put forward higher and higher requirements for lithium-ion batteries. In order to achieve better performance, the use of additives in Li-ion battery electrolytes is an important solution. At present, among the additives of lithium-ion battery electrolytes, vinylene carbonate (VC for short) is the organic film-forming additive with the most in-depth research, the most ideal effect, the widest application range and the largest dosage. According to reports, VC can undergo free radical polymerization on the surface of the carbon negative electrode to generate polyal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/36C07D317/42
Inventor 傅人俊
Owner 江苏瀚康新材料有限公司
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