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Preparation method of difluoroethylene carbonate

A technology of difluoroethylene carbonate and dichloroethylene carbonate, applied in the field of preparation of difluoroethylene carbonate, can solve the problem of difficult large-scale preparation of high-purity difluoroethylene carbonate, the effect is not very satisfactory, The conversion rate is not high, and the reaction time is shortened, the reaction conditions are mild, and the selectivity is improved.

Inactive Publication Date: 2012-11-07
SUZHOU HUAYI NEW ENERGY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction time of this method is long, and the conversion rate is not high, the effect is not very ideal, it is difficult to prepare high-purity difluoroethylene carbonate product on a large scale

Method used

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  • Preparation method of difluoroethylene carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Under the protection of nitrogen, add 1Kg anhydrous potassium fluoride, 1.6L acetonitrile, 20g tetrakis (diethylamino) phosphorus bromide to the 5000ml tetrafluoro reactor, after connecting the condenser vent pipe and other devices, start stirring, Stir vigorously, turn on the heating, raise the temperature to 70°C, then add 800g of dichloroethylene carbonate dropwise with a constant pressure funnel for 2 hours, after the addition, keep warm for 3 hours, cool down and filter, and wash the filter residue twice with 400ml of acetonitrile , Obtain filtrate 1.98Kg. Neutralize the filtrate with a saturated sodium bicarbonate solution, separate the organic phase, dry with anhydrous magnesium sulfate for 24 hours, filter, and transfer the resulting filtrate to a distillation apparatus for distillation under reduced pressure. After the distillation ends, 525 g of the product difluoroethylene carbonate is obtained. , GC content is 88.65%. Further rectification and purification ...

Embodiment 2

[0028] Under the protection of nitrogen, add 1Kg anhydrous potassium fluoride, 1.6L α-pyrrolidone, 30g tetrakis(diethylamino)phosphorus bromide into the 5000ml tetrafluoro reactor, and after connecting the condenser vent pipe and other devices, open the Stir, turn on the heating, raise the temperature to 90°C, then add 800g of dichloroethylene carbonate dropwise with a constant pressure funnel for 2 hours, after the dropwise addition, keep warm for 2.5 hours, cool down and filter, and wash the filter residue with 400ml α-pyrrolidone 2 times, the filtrate 2.2Kg was obtained. Neutralize the filtrate with a saturated sodium bicarbonate solution, separate the organic phase, dry with anhydrous magnesium sulfate for 24 hours, filter, and transfer the resulting filtrate to a distillation apparatus for distillation under reduced pressure. After the distillation ends, 485g of the product difluoroethylene carbonate is obtained. , the GC content is 86.87%.

Embodiment 3

[0030] Under nitrogen protection, add 1Kg of anhydrous potassium fluoride, 1.6L of γ-butyrolactone, and 35g of tetrakis(diethylamino)phosphorus bromide into a 5000ml tetrafluoro reactor, and connect the condenser vent pipe and other devices. , start stirring, turn on heating, heat up to 85°C, then add 800g of dichloroethylene carbonate dropwise with a constant pressure funnel, dropwise for 2 hours, after the addition, heat up to 100°C, keep warm for 2.5 hours, cool down and filter and use 400ml of γ-butyrolactone washed the filter residue twice to obtain 2.3Kg of filtrate. Neutralize the filtrate with a saturated sodium bicarbonate solution, separate the organic phase, dry with anhydrous magnesium sulfate for 24 hours, filter, and transfer the resulting filtrate to a distillation apparatus for vacuum distillation. After the distillation ends, 468g of the product difluoroethylene carbonate is obtained. , GC content is 87.05%.

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Abstract

The invention relates to a preparation method of difluoroethylene carbonate. According to the method, replacement reaction is carried out on dichloroethylene carbonate to generate the difluoroethylene carbonate. The replacement reaction is implemented by the steps of: dripping the dichloroethylene carbonate into a mixed system of anhydrous fluoride, catalyst and organic solvent at the temperature which is controlled within a range of 40-100 DEG C to react; after the reaction, sequentially carrying out solid-liquid separating, alkali washing and neutralizing, and distilling to obtain the difluoroethylene carbonate, wherein the fluoride is potassium fluoride or sodium fluoride or a mixture of the potassium fluoride and the sodium fluoride, and the adding mol ratio of the dichloroethylene carbonate to the fluoride is 1: (2-10); and the catalyst is tetra(diethylin)phosphorus bromide and the adding amount of the catalyst is 0.001-0.1 time as much as the total mass of the dichloroethylene carbonate and the fluoride. The preparation method disclosed by the invention has the advantages of moderate reaction conditions, simplicity and safety, high reaction selectivity, greatly-shortened reaction time and obvious economic benefits, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of difluoroethylene carbonate. Background technique [0002] Difluoroethylene carbonate (DFEC) has two isomers, cis and trans, and its structural formula is as follows: [0003] [0004] cis trans [0005] At present, difluoroethylene carbonate is mainly used as medicine, pesticide intermediate and lithium-ion battery electrolyte additive. The use of difluoroethylene carbonate determines that there is a higher requirement for its purity. [0006] In the prior art, in order to prepare high-purity difluoroethylene carbonate, the usual method is to synthesize fluorine and ethylene carbonate as raw materials. For example, Japanese Patent JP 200034476 introduces the use of a mixed gas of fluorine and nitrogen and carbonic acid Vinyl ester reaction to prepare fluoroethylene carbonate derivatives. Using fluorine gas as a raw material, on the one hand, fluorine gas has high toxicity and high activity, and th...

Claims

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Application Information

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IPC IPC(8): C07D317/42
Inventor 汪许诚顾乃刚陶有祥王小龙王振一
Owner SUZHOU HUAYI NEW ENERGY TECH CO LTD
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