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Preparation method for bis(fluorosulfonyl)imide

A fluorosulfonyl and imine technology, applied in the field of preparation of bis-imine, can solve problems such as long reaction time, and achieve the effects of simple operation and mild reaction conditions

Active Publication Date: 2015-10-07
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

long reaction time

Method used

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  • Preparation method for bis(fluorosulfonyl)imide
  • Preparation method for bis(fluorosulfonyl)imide
  • Preparation method for bis(fluorosulfonyl)imide

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preparation example Construction

[0026] A preparation method of bis(fluorosulfonyl)imide, specifically comprising the steps of:

[0027] Step 1. Using bis(fluorosulfonyl)imide alkali metal salt as the solute, prepare a solution with a concentration of 0.05 to 0.5 mol / L, stir vigorously and blow hydrogen chloride gas into the solution at a rate of 0.1 to 0.1 mol / L. 0.5L / min. Keep normal pressure and react for 30-90 minutes.

[0028] The solvent in the solution described in step 1 is an aprotic solvent, which is one or more of ethyl acetate, butyl acetate, and acetonitrile; when the solvent in the described solution is a mixed solvent, its mixing ratio is any Proportion;

[0029] The general formula of the chemical formula of described alkali metal salt is MN(SO 2 F) 2 , wherein M represents lithium, sodium or potassium.

[0030] The gas discharged during the reaction process is absorbed with alkaline solution.

[0031] Step 2, after the reaction, filter the reaction mixture to remove the precipitate to o...

Embodiment 1

[0036] In a 250ml three-neck flask equipped with a gas inlet, stirring, and gas outlet, add 150ml of ethyl acetate solution of lithium bis(fluorosulfonyl)imide with a concentration of 0.05mol / L. With vigorous stirring, hydrogen chloride was introduced into it at a rate of 0.1 L / min, and the introduction of hydrogen chloride was stopped after 90 minutes. The gas outlet must be connected to an absorption bottle, and lye is used to absorb the exhaust gas. After the reaction, the mixture was filtered, and the precipitate was removed to obtain the filtrate, which was distilled at 77° C. for 6 h to obtain bis(fluorosulfonyl)imide with a yield of about 80%.

Embodiment 2

[0038] In a 250ml three-neck flask equipped with a gas inlet, stirring, and gas outlet, add 150ml of a butyl acetate solution of sodium bis(fluorosulfonyl)imide with a concentration of 0.05mol / L. With vigorous stirring, hydrogen chloride was introduced into it at a rate of 0.1 L / min, and the introduction of hydrogen chloride was stopped after 90 minutes. The gas outlet must be connected to an absorption bottle, and lye is used to absorb the exhaust gas. After the reaction, the mixture was filtered, and the precipitate was removed to obtain the filtrate, which was distilled at 127° C. for 6 h to obtain bis(fluorosulfonyl)imide with a yield of about 83%.

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Abstract

The invention discloses a preparation method for bis(fluorosulfonyl)imide. The preparation method comprises the following concrete steps: 1, with bis(fluorosulfonyl)imide alkali metal salt as a solute, preparing a solution with a concentration of 0.05 to 0.5 mol / L, carrying out violent stirring, blowing in hydrogen chloride gas into the solution at a blowing speed of 0.1 to 0.5 L / min and carrying out a reaction for 30 to 90 min at normal pressure; 2, subjecting a reaction mixture obtained after the reaction to filtering to remove a precipitate so as to obtain a solution of bis(fluorosulfonyl)imide; and 3, according to the boiling point of a solvent in the solution, distilling the obtained solution of bis(fluorosulfonyl)imide so as to remove the solvent, thereby obtaining bis(fluorosulfonyl)imide. The chemical formula of bis(fluorosulfonyl)imide is HN(SO2F)2. According to the invention, strong acid with great danger such as hydrogen fluoride and concentrated sulfuric acid is not used as an acidifying raw material. The preparation method in the invention has mild reaction conditions, does not need heating, can be carried out at normal pressure and is simple to operate.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry and aims to provide a preparation method of bis(fluorosulfonyl)imide. Background technique [0002] Bis(fluorosulfonyl)imide, HN(SO 2 F) 2 It is an important nitrogen-containing strong acid and has very high practical value in chemistry. In organic chemistry, it is mainly used for acid-catalyzed reactions or for the preparation of other catalysts; in electrochemistry, it can be used as an important synthetic raw material for lithium-ion battery electrolytes. For example, lithium bis(fluorosulfonyl)imide has become an important type of lithium-ion battery electrolyte because of its good electrochemical performance. It has the advantages of high stability, hydrolytic stability, and environmental friendliness, which is obviously better than Lithium hexafluorophosphate (LiPF 6 ) and other electrolyte materials currently in use; rare earth metal salts of bis(fluorosulfonyl)imides show stro...

Claims

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Application Information

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IPC IPC(8): C01B21/093
Inventor 詹晓力何逸波张庆华陈丰秋
Owner ZHEJIANG UNIV
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