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Preparation method of fluoroethylene carbonate

A technology for fluoroethylene carbonate and ethylene carbonate, applied in the field of organic synthesis, can solve the problems of large environmental pollution, waste of halogen raw materials, harsh process conditions, etc., and achieve the effects of reducing cost, improving utilization rate, and improving system safety.

Active Publication Date: 2018-05-15
张甘泉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of synthetic method of the fluorinated ethylene carbonate that overcomes prior art deficiency, and this method should at least overcome the cost and processing that the process of halogen exchange method is loaded down with trivial details, the waste of halogen raw material, use additional catalyst or solvent etc. Difficulty, at least to overcome the difficulty of controlling the reaction process of direct fluorination, high requirements on equipment, harsh process conditions, complicated purification treatment in the later stage, and large environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 100g of ethylene carbonate and 370g of N-fluorobistrifluoromethanesulfonamide into the closed reaction kettle, stir, heat up to 120°C, take a sample for HPLC analysis until the reaction time is 0.9h when ethylene carbonate is undetectable, stop the reaction, The fluoroethylene carbonate product was separated by rectification with a purity of >99.9% and a yield of 97.8%; the chromaticity was 8 Hazen.

[0021] After dissolving the residue (the product after the reaction of the fluorinated reagent) in 1L of acetonitrile, add 50g of sodium fluoride, and bubble 10% F at -10°C 2 / N 2 After the reaction is complete, filter and rectify to obtain 326 g of regenerated N-fluorobistrifluoromethanesulfonamide (contains some unfluorinated substances, which are not strictly treated, and purification is not necessary). Exhaust gas recovery and circulation.

[0022] The regenerated fluorinated reagent was used in the same reaction as above for 100 g of ethylene carbonate to obtain...

Embodiment 2

[0025] The above-mentioned fluorinated reagent was replaced with 390g N-fluorobisbenzenesulfonamide. Under the same conditions, the complete reaction time was 1.2h, the purity was >99.9%, and the yield was 98.2%; the chromaticity was 8 Hazen.

[0026] The fluorinated reagent was regenerated in the same way to obtain 334 g of N-fluorobistrifluoromethanesulfonamide.

[0027] It was used in the same reaction as above for 100 g of ethylene carbonate, the purity was >99.9%, the yield was 97.7%; the chroma was 8 Hazen.

[0028] The above products are collected and subjected to simple 4A molecular sieve adsorption treatment to achieve undetectable impurities by HPLC and a chromaticity of 6 Hazen.

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Abstract

The invention relates to a direct fluorination synthesis method of fluoroethylene carbonate, which includes steps of performing direct fluorination to ethylene carbonate and a fluorination reagent inthe presence / absence of a solvent and in the absence of a catalyst to prepare the fluoroethylene carbonate, performing fluorination regeneration to a product of the fluorination reagent after reaction, thus recycling the fluorination reagent for the direct fluorination of the ethylene carbonate. Being different from indirect fluorination, the method can efficiently produce the fluoroethylene carbonate through a direct one-step reaction, thus reducing reaction process. The product can reach high level in purity, chromaticity and yield of the product. The method is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a direct fluorination synthesis method of fluoroethylene carbonate. Background technique [0002] Fluoroethylene Carbonate (Fluoroethylene Carbonate, FEC; 4-fluoro-1,3-dioxolan-2-one; CAS Registry No. 114435-02-8) began to attract people's attention and attention because of its role as a lithium battery electrolytic The use of liquid additives, and people's lives in modern life are inseparable from lithium batteries, which are widely used in mobile phones, automobiles, electronics, aviation, military and other fields. In addition to lithium batteries, there are also potential uses of fluoroethylene carbonate in the fields of pesticides and chemicals. [0003] At present, the synthesis of fluoroethylene carbonate is mainly through the halogen exchange method and the direct fluorination method; among them, the halogen exchange method has been studied more, for example,...

Claims

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Application Information

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IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 苏振东
Owner 张甘泉