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Method for preparing fluoroethylene carbonate by direct fluorination

A technology for fluoroethylene carbonate and ethylene carbonate, which is applied in the field of direct fluorination to prepare fluoroethylene carbonate, can solve the problems of waste of halogen raw materials, harsh process conditions, large environmental pollution, etc. Chroma, cost reduction effect

Active Publication Date: 2018-06-22
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] Step 1: Dissolve 435g of bistrifluoromethanesulfonamide 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 about 370 g of regenerated N-fluorobistrifluoromethanesulfonamide.

[0021] Step 2: Add 100g of ethylene carbonate and 370g of N-fluorobistrifluoromethanesulfonamide into the closed reaction kettle, stir, heat up to 120°C, sample for HPLC analysis until ethylene carbonate is undetectable, the reaction time is 0.9h, The reaction was stopped, and 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.

[0022] The separated fluorinated reagent reaction product was mixed with the incompletely reacted bis-trifluoromethanesulfonamide in step 1 and the reaction in step 1 was repeated to obtain about 368 g of N-fluorobis-trifluoromethanesulfonamide.

[0023] It was used in the same reaction...

Embodiment 2

[0026] Step 1: Replace the bistrifluoromethanesulfonamide in Example 1 with 460g of bisbenzenesulfonamide to obtain about 390g of N-fluorobisbenzenesulfonamide;

[0027] Step 2: Replace the fluorinated reagent of Example 1 with 390 g of N-fluorobisbenzenesulfonamide. Under the same conditions, the complete reaction time is 1.2 hours, the purity is >99.9%, and the yield is 98.2%; the chromaticity is 8 Hazen.

[0028] The fluorinated reagent was regenerated in the same way to obtain 388 g of N-fluorobistrifluoromethanesulfonamide.

[0029] It was used in the same reaction as above for 100 g of ethylene carbonate, the purity was >99.9%, the yield was 98%; the chromaticity was 8 Hazen.

[0030] The above-mentioned product can achieve impurity undetectable by HPLC after simple molecular sieve adsorption treatment, and the chromaticity is 6 Hazen.

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Abstract

The invention relates to a method for preparing fluoroethylene carbonate by direct fluorination. The method comprises the following steps: carrying out a reaction on fluorine gas with a fluorinating agent precursor to prepare a fluorinating agent, and directly fluorinating ethylene carbonate with the prepared fluorinating agent under a condition with a solvent or without a solvent, and without a catalyst to prepare the fluoroethylene carbonate, wherein a product obtained after the reaction of the fluorinating agent is subjected to fluorinating regeneration, and is recycled for a fluorination reaction of ethylene carbonate. According to the method provided by the invention, the problem of excessive fluorine gas activity is overcome, the fluorine gas is indirectly converted into the mild andefficient fluorinating reagent, the utilization rate and the safety of the fluorine gas are improved, and the environmental pollution is reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing fluoroethylene carbonate by direct fluorination. 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, "Summar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/42
CPCC07D317/42
Inventor 苏振东
Owner 张甘泉