Preparation method of bis(fluorosulfonyl)amide alkali metal salt

A technology of bisfluorosulfonimide base and bischlorosulfonimide base, applied in the direction of nitrogen and non-metallic compounds, sulfamic acid, etc., to achieve the effects of simplifying the purification steps, solving the problem of sublimation residues, and reducing the production cost

Active Publication Date: 2019-11-05
刘大凡
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] In view of this, the present invention provides a kind of preparation method of alkali metal salt of bisfluorosulfonimide, solves the problem of how to improve the fluorination effect and the separation of products and by-products after fluorination

Method used

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  • Preparation method of bis(fluorosulfonyl)amide alkali metal salt
  • Preparation method of bis(fluorosulfonyl)amide alkali metal salt
  • Preparation method of bis(fluorosulfonyl)amide alkali metal salt

Examples

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Embodiment 1

[0036] The preparation method of bisfluorosulfonimide alkali metal salt, the steps are as follows:

[0037](1) Under the protection of dry nitrogen, add 0.2L dimethyl carbonate and 115g dichlorosulfonimide potassium salt into a 1L three-necked flask. After stirring and dissolving, 148 g of dried bismuth fluoride was added at room temperature, and stirred at room temperature for 24 hours. After the reaction, the system was moved to a glove box with a water content lower than 1 ppm to filter and remove excess bismuth fluoride. The filtrate was evaporated to dryness with a rotary evaporator to obtain a light yellow solid mixture;

[0038] (2) Under the protection of dry nitrogen, the above-mentioned light yellow solid mixture was dissolved in 120 g of absolute ethanol in a jacketed flask with a cooling device, and the temperature of the solution was kept not higher than 20° C. After stirring and dissolving for 4 hours, it was transferred to a glove box for filtration, and the f...

Embodiment 2

[0040] The preparation method of bisfluorosulfonimide alkali metal salt, the steps are as follows:

[0041] (1) Under the protection of dry nitrogen, 0.2 L of acetonitrile and 117.6 g of lithium dichlorosulfonimide were added to a 1 L three-necked flask. After stirring and dissolving, 64 g of dry antimony fluoride was added at room temperature, and the reaction was stirred at room temperature for 24 hours. After the reaction, the system was moved to a glove box with a moisture content lower than 1 ppm to remove excess antimony fluoride by filtration. The filtrate was evaporated to dryness with a rotary evaporator to obtain a light yellow solid mixture;

[0042] (2) Under the protection of dry nitrogen, the above light yellow solid mixture was dissolved in 200 g of anhydrous toluene in a jacketed flask with a cooling device, and the temperature of the solution was kept not higher than 20° C. After stirring and dissolving for 4 hours, it was transferred to a glove box for filt...

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Abstract

The invention discloses a preparation method of a bis(fluorosulfonyl)amide alkali metal salt. A trivalent metal fluoride is used for fluoridizing a bis(chlorosulfonyl)amide alkali metal salt in an organic solvent into the bis(fluorosulfonyl)amide alkali metal salt, then, a trivalent metal chloride and the bis(fluorosulfonyl)amide alkali metal salt are separated and purified by means of differencesof solubilities of the trivalent metal chloride and the bis(fluorosulfonyl)amide alkali metal salt in different solvents, the method avoids generation of hydrogen chloride gas in the fluorination process, and the fluorination efficiency is high.

Description

technical field [0001] The invention relates to a preparation method of an alkali metal salt of bisfluorosulfonimide, which belongs to the field of fine chemicals. Background technique [0002] Bisfluorosulfonimide HN(SO 2 F) 2 (referred to as HFSI) due to its large anion size and highly delocalized charge, it is a typical "weakly coordinated" anion and has weak electrostatic interaction with cations. Therefore, its alkali metal salts have many distinctive and excellent properties in the field of electrochemistry. For example, LiFSI has higher ionic conductivity than lithium hexafluorophosphate, excellent thermal stability and hydrolysis resistance in lithium ion battery electrolytes, and can effectively improve the high and low temperature performance and cycle life of lithium ion batteries. It is considered to be the next generation of new lithium salts. [0003] At present, the preparation methods of HFSI and its alkali metal salts mainly include the following: [000...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096
CPCC01B21/096
Inventor 刘大凡
Owner 刘大凡
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