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Method for preparing vinylene carbonate

A technology of vinylene carbonate and ethylene carbonate, which is applied in the field of preparing vinylene carbonate, can solve problems such as not suitable for industrial production, achieve the effect of reducing equipment requirements and process conditions, and improving safety

Inactive Publication Date: 2012-07-04
HUBEI DEZHOU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This reaction uses toluene as a solvent and is carried out under sealed conditions. High temperature produces high pressure, which is not suitable for industrial production.

Method used

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  • Method for preparing vinylene carbonate
  • Method for preparing vinylene carbonate
  • Method for preparing vinylene carbonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Ethylene carbonate reacts with chlorine to produce chloroethylene carbonate: Under the irradiation of an ultraviolet lamp (45 watts), chlorine is passed into a solution (500 ml) of freshly distilled ethylene carbonate (44 g). The reaction temperature is 55-60°C, and the reaction is carried out for 10 hours under stirring. After the reaction is over, chloroethylene carbonate (72%, B.p. 106-107°C / 10-11mmHg) and ethylene carbonate are obtained by distillation under reduced pressure.

[0035] Add chloroethylene carbonate to 250ml of toluene, that is, toluene is used as the solvent of chloroethylene carbonate, and then add 10g of quaternary ammonium ion exchange resin, and stir and react for 8 hours at a temperature of 50-55°C. The solid was removed by filtration, 5 g of sodium carbonate was added, stirred for 15 minutes, and then filtered. The filtrate was treated with molecular sieve and rectified under reduced pressure to 29g VC (85%, B.p. 62-63°C / 20mmHg).

Embodiment 2

[0037] Ethylene carbonate reacts with chlorine to produce chloroethylene carbonate: Under ultraviolet light (40 watts), chlorine is passed into a solution (800 ml) of freshly distilled ethylene carbonate (52.8 g). The reaction temperature is 50-55°C, and the reaction is carried out for 8 hours under stirring. After the reaction, the crude product was distilled under reduced pressure to obtain 50 g of chloroethylene carbonate (68%, B.p. 106-107°C / 10-11 mmHg).

[0038] Add chloroethylene carbonate (50g) to petroleum ether (500ml), that is, petroleum ether is used as the solvent of chloroethylene carbonate, keep the temperature below 45°C, and add 10g of quaternary ammonium ion exchange resin under stirring. The entire reaction system was stirred at this temperature for 5 hours, and then filtered to remove solids. Add 6 g of sodium carbonate to the obtained liquid, stir for half an hour and then filter; add 10 g of molecular sieve and distill under reduced pressure to obtain 41 g o...

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Abstract

The invention provides a method for preparing vinylene carbonate, which comprises the following steps: (1) adopting ethylene carbonate as raw material, introducing chlorine gas under a condition of ultraviolet irradiation, and allowing substitution reaction to obtain chloroethylene carbonate; allowing elimination reaction of chloroethylene carbonate obtained in the step (1) and quaternary ammonium ion exchange resin in the presence of an organic solvent for dehydrochlorination to obtain vinylene carbonate; and performing distillation purification on a mixed product obtained in the step (2). The method in the invention employs the organic solvent as a solvent of chloroethylene carbonate and the quaternary ammonium ion exchange resin as a dechlorination agent, prevents using a high-temperature cracking process, highly flammable diethyl ether as a solvent and malodorous organic amines, and improves the production safety, carries out the reaction at a relatively low temperature, realizes the purification of the product by distillation, greatly reduces the requirements for equipment and process conditions, and is suitable for industrial production.

Description

Technical field [0001] The invention relates to a method for preparing vinylene carbonate. Background technique [0002] Vinylene carbonate (VC) is an important organic compound. [0003] VC can be applied to the electrolyte of lithium batteries, which can effectively inhibit battery swelling caused by the gas generated when lithium batteries are stored at high temperatures or repeated charging and discharging cycles, and can improve the conductivity of the electrolyte, thereby making lithium ion doping, Dedoping is smoothly performed, reducing the internal resistance of the battery. The gel electrolyte prepared by VC exhibits excellent chemical stability, strength and liquid retention rate, and can prepare a gel electrolyte battery with satisfactory capacity, cycle performance, load performance and low temperature performance. Adding VC to the non-aqueous electrolyte can make it have good high-temperature cycle characteristics and high-temperature storage resistance, which can b...

Claims

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Application Information

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IPC IPC(8): C07D317/40
Inventor 张静
Owner HUBEI DEZHOU TECH DEV