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Preparation method of lithium bis (fluorosulfonyl) imide

A technology of bisfluorosulfonimide lithium and bisfluorosulfonimide is applied in the field of preparation of bisfluorosulfonimide lithium, which can solve the problems of inability to complete metathesis reaction, severe reaction and high price, and achieve high reaction Effects of conversion rate and yield, mild reaction conditions and high technical indicators

Active Publication Date: 2021-08-13
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: 1) the metathesis reaction is difficult to complete, and the residual potassium ions in the product are relatively high; 2) lithium tetrafluoroborate and lithium perchlorate, which are used as reaction raw materials, have a large solubility in the reaction organic solvent and are difficult to separate. The products often contain some unreacted or excessive raw materials, and the product purity is not high; 3) The price of organic lithium salts such as lithium tetrafluoroborate or lithium perchlorate is relatively high, resulting in high manufacturing costs; lithium perchlorate is Explosive compounds bring certain safety risks and are not suitable for industrial production
Its main disadvantages are: 1) bisfluorosulfonimide is a proton strong acid, which reacts violently with alkali and generates a lot of heat
The reaction process needs to be controlled by freezing and low temperature, and the energy consumption is high; 2) The essence of the reaction is an acid-base neutralization reaction, and at the same time, equimolar water is generated. It is difficult to completely remove water by thionyl chloride, the reaction time is long, and there are many wastes.
At the same time, the water removal reaction process easily causes partial hydrolysis of the product, resulting in residual water in the product, excessive chloride ions and sulfate ions, and it is difficult to obtain high-quality products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Under a nitrogen atmosphere, add 42 g (1 mol) of anhydrous lithium chloride into a dry three-neck flask equipped with a stirring and condensing reflux device, then add 360 g of dichloromethane, and start stirring. Add 181g (1mol) of bisfluorosulfonimide to the dry constant pressure dropping funnel under nitrogen atmosphere, and drop it into the flask at room temperature. During the dropping process, acidic tail gas escapes, and the tail gas of the condensing return pipe is connected to the lye absorption device. After 1 hour, the dropwise addition was completed, and the temperature was raised to reflux at about 40°C, and the reaction was continued for 1 hour, then stopped, and cooled to room temperature. The pH of the reaction solution was measured to be 1, and triethylamine was slowly added dropwise therein under stirring, and the pH of the reaction solution was continuously checked during the process, and the dropwise addition was stopped when the pH was 6-7, and the ...

Embodiment 2

[0025] Under a nitrogen atmosphere, add 28.6 g (1.1 mol) of anhydrous lithium fluoride into a dry three-neck flask equipped with a stirring and condensing reflux device, then add 181 g of dichloroethane to it, and start stirring. Add 181 g (1 mol) of bisfluorosulfonimide to a dry constant-pressure dropping funnel under nitrogen atmosphere, add dropwise to the flask at room temperature, and connect the tail gas of the condensing reflux tube to the alkali liquor absorption device. After 1 hour, the dropwise addition was completed, and the temperature was raised to 55° C. to 60° C. to continue the reaction for 12 hours, and the temperature was stopped to cool down to room temperature. The pH of the reaction solution was measured to be 1, and dipropylamine was slowly added dropwise therein under stirring, and the pH of the reaction solution was continuously checked during the process, and the dropwise addition was stopped when the pH was 5-6, and the stirring was continued for abou...

Embodiment 3

[0029]Under a nitrogen atmosphere, add 46 g (1.1 mol) of anhydrous lithium chloride into a dry three-neck flask equipped with a stirring and condensing reflux device, then add 540 g of dichloroethane, and start stirring. Add 181g (1mol) of bisfluorosulfonimide to the dry constant pressure dropping funnel under nitrogen atmosphere, and drop it into the flask at room temperature. During the dropping process, acidic tail gas escapes, and the tail gas of the condensing return pipe is connected to the lye absorption device. After 1 hour, the dropwise addition was completed, and the reaction was incubated at 0-8° C. for 12 hours, and the pH of the reaction solution was measured to be 1. Pyridine was slowly added dropwise therein under stirring, and the pH of the reaction solution was continuously checked during the process, until the pH was 7-8, the dropwise addition was stopped, and the stirring was continued for about 30 minutes. Filter under the protection of nitrogen, and rinse...

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Abstract

The invention discloses a preparation method of lithium bis (fluorosulfonyl) imide, which comprises the following steps: dropwise adding bis (fluorosulfonyl) imide under the condition that anhydrous lithium halide salt and a non-polar solvent are mixed and stirred, and absorbing tail gas by adopting alkali liquor; continuously reacting for 1-12 hours at the temperature of 0-60 DEG C after dropwise adding, cooling to room temperature, dropwise adding an organic alkaline compound, and adjusting the pH value of the reaction liquid to 5-8; and filtering, and leaching a filter cake by adopting a non-polar solvent to obtain a lithium bis (fluorosulfonyl) imide crude product. The method has the beneficial effects of mild reaction, simple process and low cost, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of electrolytes in lithium ion battery electrolytes, and in particular relates to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonyl imide (LiFSI) is a lithium salt of lithium ion battery electrolyte. It has high and low temperature resistance, stable structure, and is not easy to be hydrolyzed. It is superior to the currently widely used lithium hexafluorophosphate in terms of application safety and stability. , is expected to replace lithium hexafluorophosphate as an ideal substitute for lithium salt as the main electrolyte in the future. At present, there are two main routes for the preparation of lithium bisfluorosulfonyl imide publicly reported at home and abroad: [0003] One is the metathesis reaction of bisfluorosulfonimide potassium salt and organic lithium salts such as lithium tetrafluoroborate or lithium perchlorate in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086H01M10/0562H01M10/0525
CPCC01B21/086C01P2006/40C01P2006/80H01M10/0525H01M10/0562Y02E60/10
Inventor 杨志勇李伟锋曹娜陆海媛袁青海
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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