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A kind of preparation method of vinylene carbonate

A technology of vinylene carbonate and carbonate, which is applied in the field of preparation of vinylene carbonate, can solve the problems of negative impact of safety protection measures required by equipment, high reaction temperature, high difficulty of process operation separation, etc., and achieve controllable yield and The effect of purity, good safety and high economic benefit

Active Publication Date: 2021-11-26
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent avoids the hydrogen chloride, solid waste of salts and coking residues produced during the elimination reaction after the usual use of chlorination, it still produces hydrogen, and the reaction temperature is very high (200°C ~ 600°C), which will Have a great negative impact on the equipment requirements and safety protection measures in the actual production process
[0005] Another example is the Chinese invention CN1290840C, which uses monochloroethylene carbonate and triethylamine to generate dechlorination reaction to synthesize vinylene carbonate. However, this type of reaction has defects such as many by-products, unsatisfactory yield, and large solvent usage, resulting in subsequent process operations. Difficult to separate problems

Method used

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  • A kind of preparation method of vinylene carbonate

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Effect test

Embodiment 1

[0030] The preparation of embodiment 1 vinylene carbonate

[0031] Under the protection of nitrogen, add 130 grams of sodium carbonate and 600 milliliters of deionized water to a 1000 ml four-neck flask (with a condenser), stir and heat up to 40 ° C to completely dissolve, then add 200 grams of 1,2-dibromoethylene and 0.2 grams of potassium iodide, 0.4 g of polyethylene glycol 600, continue to heat up to 90 ° C, keep the reaction for 10 hours, then cool down to room temperature. 100ml of ethyl acetate was added to the reaction solution to extract twice, the combined organic phases were dried through molecular sieves, filtered, and the solvent was removed by distillation under reduced pressure to obtain 86.4 grams of vinylene carbonate crude product with a purity of 91.3% and a pure product yield of 85%.

Embodiment 2

[0032] The preparation of embodiment 2 vinylene carbonate

[0033] Under the protection of nitrogen, add 130 grams of sodium carbonate and 600 milliliters of deionized water to a 1000 ml four-neck flask (with a condenser), stir and heat up to 40 ° C to completely dissolve, then add 200 grams of 1,2-dibromoethylene and 0.2 grams of potassium iodide, 0.4 g of tetrabutylammonium bromide, continue to heat up to 90° C., keep the temperature for 10 hours, and then cool down to room temperature. 100ml of chloroform was added to the reaction solution to extract twice, the combined organic matter was dried through molecular sieves, filtered, and the solvent was removed by distillation under reduced pressure to obtain 90 g of crude vinylene carbonate with a purity of 90.3% and a yield of 88%.

Embodiment 3

[0034] The preparation of embodiment 3 vinylene carbonate

[0035] Under the protection of nitrogen, add 150 grams of potassium carbonate and 600 milliliters of deionized water into a 1000 ml four-necked flask (with a condenser), stir and heat up to 40 ° C, and then add 200 grams of 1,2-dibromoethylene, 0.2 potassium bromide gram, 0.5 grams of benzyltriethylammonium chloride, continue to heat up to 92 ° C, keep the reaction for 12 hours, then cool down to room temperature. 100ml of chloroform was added to the reaction solution to extract twice, the combined organic phases were dried over molecular sieves, filtered, and the solvent was removed by distillation under reduced pressure to obtain 88 g of crude vinylene carbonate with a purity of 90.5% and a yield of 86%.

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Abstract

The invention discloses a preparation method of vinylene carbonate. The preparation method comprises: reacting 1,2-dibromoethylene and basic carbonate in water in the presence of an alkali metal halide salt and a phase transfer catalyst to form Vinylene carbonate; the method of the invention not only has high yield and good purity, but also has controllable reaction process, low cost and simple operation process, and is suitable for industrial application.

Description

technical field [0001] The invention belongs to the field of organic film-forming additives and / or overcharge protection additives for lithium-ion battery electrolytes, and in particular relates to a preparation method of vinylene carbonate. Background technique [0002] Vinylene carbonate (VC, Vinylene Carbonate), colorless and transparent liquid at room temperature, melting point is 21°C, boiling point is 165°C / 760mmHg, density (20°C) is 1.360g / cm 3 In 1953, Newman et al first reported the synthesis method of vinylene carbonate (J.Am.Chem.Soc., 1953, 75(5), pp1263–1264), using chlorine gas and ethylene carbonate to generate free radical substitution synthesis Chloroethylene carbonate, followed by elimination reaction with triethylamine in ether solvent to obtain vinylene carbonate. It is mainly used as a new type of organic film-forming additive and overcharge protection additive for lithium-ion batteries, etc. It has good high and low temperature performance and anti-fla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/40B01J31/26B01J31/06B01J31/02B01J27/08
CPCB01J27/08B01J31/0239B01J31/068B01J31/26B01J35/0006C07D317/40
Inventor 汪许诚管晓东王小龙
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD