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Preparation method of bis(fluorosulfonyl)imide salt

A technology of bisfluorosulfonimide salt and bisfluorosulfonimide, which is applied in the field of preparation of bisfluorosulfonimide salt, and can solve problems such as increased risk

Active Publication Date: 2017-10-03
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The raw material metal hydroxide, onium hydroxide and HF used in the above method are very active, which increases the danger of the reaction

Method used

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  • Preparation method of bis(fluorosulfonyl)imide salt
  • Preparation method of bis(fluorosulfonyl)imide salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 200ml of butyl acetate and 10.92g (0.13mol) of aluminum fluoride to a 500ml three-necked flask A, add 40.67g (0.19mol) of dichlorosulfonimide dropwise in an ice-water bath, and react 6 at room temperature after the dropwise addition is complete. Hour.

[0022] Add 130g of 30wt% lithium nitrilotriacetate aqueous solution in the 500ml three-necked bottle B, gradually add the reaction solution in the above-mentioned three-necked bottle A dropwise, react at room temperature for 3 hours after the dropwise addition, then separate the liquids, and use butyl acetate for the aqueous phase The ester was extracted twice, the extract was combined with the organic phase, most of the solvent butyl acetate was distilled off, dichloromethane was added to precipitate, and filtered to obtain 24.04 g of white powdery lithium bisfluorosulfonyl imide. The yield of lithium bisfluorosulfonyl imide is 82%, and the content of aluminum ion in lithium bisfluorosulfonyl imide is 7ppm.

Embodiment 2

[0024] Add 200ml of butyl acetate and 15.96g (0.19mol) of aluminum fluoride to a 500ml three-necked flask A, add 40.67g (0.19mol) of dichlorosulfonimide dropwise in an ice-water bath, and react at room temperature for 8 Hour.

[0025] Add 115.56g of 50wt% dilithium ethylenediaminetetraacetic acid salt (Mw=304.109) aqueous solution in the 500ml three-necked bottle B, gradually add the reaction solution in the above-mentioned three-necked bottle A dropwise, and react at room temperature for 5 hours after the dropwise addition is completed. Then separate the liquids, extract the aqueous phase twice with butyl acetate, combine the extract with the upper organic phase, distill off most of the solvent butyl acetate, add dichloromethane to precipitate, filter to obtain white powdery lithium bisfluorosulfonimide 29.19 g. The yield of lithium bisfluorosulfonyl imide is 89%, and the content of aluminum ion in lithium bisfluorosulfonyl imide is 15ppm.

Embodiment 3

[0027] Add 500ml of butyl acetate to a 1000ml three-necked bottle A, add dropwise 85.62g (0.4mol) of dichlorosulfonimide, and add 29.39g (0.35mol) of aluminum fluoride (Mw=83.98) after the dropwise addition, at room temperature React for 5 hours.

[0028] Add 115g of 30wt% lithium metaphosphate (Mw=85.91) aqueous solution in 1000ml three-necked bottle B, gradually add dropwise the reaction solution in the above-mentioned three-necked bottle A, react at room temperature for 6 hours after the dropwise addition, then separate the liquid, the water phase Extracted twice with butyl acetate, combined the extract with the upper organic phase, distilled off most of the solvent butyl acetate, added dichloromethane to precipitate, and filtered to obtain 43.38 g of white powdery lithium bisfluorosulfonyl imide. The yield of lithium bisfluorosulfonyl imide is 80%, and the content of aluminum ion in lithium bisfluorosulfonyl imide is 17ppm.

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Abstract

The invention discloses a method for preparing bis(fluorosulfonyl)imide salt. The method comprises the following steps: reacting bis(chlorosulfonyl)imide and a fluorination reagent to obtain bis(fluorosulfonyl)imide; and reacting the bis(fluorosulfonyl)imide and an alkali metal salt chelator to obtain the corresponding bis(fluorosulfonyl)imide salt. The method provided by the invention does not need the use HF and other high-activity compounds, and is simple and safe in preparation process, thereby being suitable for industrialization application.

Description

technical field [0001] The invention relates to a preparation method of bisfluorosulfonimide salt. Background technique [0002] Bisfluorosulfonimide salt has the characteristics of good electrochemical stability, good hydrolysis resistance and high conductivity, and can be widely used in electrolytes, especially in power batteries, which can improve the cycle performance and rate performance of power batteries. [0003] For the preparation method of bisfluorosulfonimide salt, the prior art has the following reports: [0004] Chinese patent CN103384641B discloses a preparation method of bisfluorosulfonimide salt, which is obtained by using bisfluorosulfonimide ammonium salt as a raw material and performing ion exchange reaction with metal hydroxide or onium hydroxide. [0005] Chinese patent CN103347811B discloses a two-step method for preparing bisfluorosulfonimide salts. The first step is to obtain bisfluorosulfonimide ammonium salt by reacting bischlorosulfonimide ammoni...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086
Inventor 王传水陈慧闯肖恒侨徐卫国
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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