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Method for continuously preparing fluoroethylene carbonate and/or vinylene carbonate by gas phase

A technology of fluoroethylene carbonate and vinylene carbonate, which is applied in the field of gas-phase continuous preparation of fluoroethylene carbonate, can solve problems such as environmental pollution, difficult reaction control, and difficult acquisition of organic raw materials, and achieves easy continuous process and easy reaction , easily accessible effects

Pending Publication Date: 2018-07-27
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The above method has the following defects: (1) the first route uses highly toxic fluorine gas, the reaction is difficult to control, there are many by-products, the selectivity is poor, and it is easy to explode; (2) the second route uses intermittent Liquid-phase fluorine-chlorine exchange method, the excess hydrogen fluoride and the generated by-product hydrogen chloride are difficult to be recycled, which is easy to cause serious environmental pollution, and the yield of fluoroethylene carbonate is low; (3) the third route is not only organic raw materials It is difficult to obtain and control the inorganic raw material fluorine gas, and the fragments of pyrolysis are not complete, the conversion rate is low, and it is easy to cause waste of raw materials

Method used

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  • Method for continuously preparing fluoroethylene carbonate and/or vinylene carbonate by gas phase
  • Method for continuously preparing fluoroethylene carbonate and/or vinylene carbonate by gas phase
  • Method for continuously preparing fluoroethylene carbonate and/or vinylene carbonate by gas phase

Examples

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Effect test

Embodiment 1

[0030] 10 ml of commercially available activated carbon (Shirasagi C2x7 / 12 activated carbon, Osaka Gas Chemicals Co. Ltd.) was charged into a tubular reactor made of Inconium alloy with an inner diameter of 1 / 2 inch and a length of 30 cm. The reaction conditions are: the reaction temperature is raised to 160°C, the molar ratio of anhydrous hydrogen fluoride to chloroethylene carbonate is 10:1, the contact time is 10s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was separated by heating to remove HF and HCl, then condensed, and the liquid organic phase was taken for GC analysis. The reaction result is: the conversion rate of chloroethylene carbonate is 97.71%, the selectivity of fluoroethylene carbonate is 55.8%, the selectivity of vinylene carbonate is 15.9%, the rest is fluoroacetaldehyde, chloroacetaldehyde , acetic acid and other by-products.

[0031] The above organic phase was rectified to obtain fluoroethylene carbonate and viny...

Embodiment 2

[0033] Fill 10 milliliters of fluorination catalyst FeF prepared by the above-mentioned method in the tubular reactor made of Incon alloy with internal diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are: the reaction temperature is raised to 160°C, the molar ratio of anhydrous hydrogen fluoride to chloroethylene carbonate is 10:1, the contact time is 10s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was separated by heating to remove HF and HCl, then condensed, and the liquid organic phase was taken for GC analysis. The reaction result is: the conversion rate of chloroethylene carbonate is 100%, the selectivity of fluoroethylene carbonate is 81.0%, the selectivity of vinylene carbonate is 12.7%, the rest is fluoroacetaldehyde, chloroacetaldehyde , acetic acid and other by-products.

[0034] The above organic phase was rectified to obtain fluoroethylene carbonate and vinylene carbonate. The boiling point of fluoroethylene car...

Embodiment 3

[0036] Fill 10 milliliters of fluorination catalyst FeF prepared by the above-mentioned method in the tubular reactor made of Incon alloy with internal diameter 1 / 2 inch, long 30cm 3 . The reaction conditions are: the reaction temperature is raised to 200°C, the molar ratio of anhydrous hydrogen fluoride to chloroethylene carbonate is 10:1, the contact time is 10s, and the reaction pressure is 0.1MPa. After running for 10 hours, the reaction product was separated by heating to remove HF and HCl, then condensed, and the liquid organic phase was taken for GC analysis. The reaction result is: the conversion rate of chloroethylene carbonate is 100%, the selectivity of fluoroethylene carbonate is 56.3%, the selectivity of vinylene carbonate is 32.9%, the rest is fluoroacetaldehyde, chloroacetaldehyde , acetic acid and other by-products.

[0037] The above organic phase was rectified to obtain fluoroethylene carbonate and vinylene carbonate. The boiling point of fluoroethylene car...

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Abstract

The invention relates to a method for continuously preparing fluoroethylene carbonate and / or vinylene carbonate by gas phase. In the reaction, the fluoroethylene carbonate is used as raw materials; inthe hydrogen fluoride atmosphere, under the existence of fluorination catalysts, fluorine-chlorine exchange reaction is taken to obtain the fluoroethylene carbonate and / or vinylene carbonate. The rawmaterials can be easily obtained; the conversion rate is high; the reaction can be easily controlled; the large-scale continuous production of the fluoroethylene carbonate can be easily realized; thevinylene carbonate can be coproduced at the same time; a target product can be prepared through temperature regulation.

Description

technical field [0001] The present invention relates to a method for continuously preparing fluoroethylene carbonate in the gas phase, in particular to a method for preparing fluoroethylene carbonate through the fluorine-chlorine exchange reaction of chloroethylene carbonate under the catalysis of a hydrogen fluoride catalyst. Preparation of vinylene carbonate. Background technique [0002] Fluoroethylene carbonate is a new type of electrolyte additive that can significantly improve the performance of lithium batteries. Fluoroethylene carbonate mainly has the following three synthetic routes: [0003] The first is the direct fluorination route of fluorine gas. The literature [Journal of Fluorine Chemistry 120 (2003) 105-110] reported the direct fluorination of ethylene carbonate with 30% fluorine / nitrogen to obtain fluoroethylene carbonate with a yield of 70%. [0004] [0005] The second is the batch preparation route of the liquid-phase fluorine-chlorine exchange rea...

Claims

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Application Information

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IPC IPC(8): C07D317/36C07D317/40
CPCC07D317/36C07D317/40
Inventor 张呈平胡儒柱贾晓卿权恒道
Owner 泉州宇极新材料科技有限公司
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