Difluoro-sulfonyl imine preparation method and method for preparing difluoro-sulfonyl imine alkali metal salt by using prepared difluoro-sulfonyl imine

A technology of bisfluorosulfonimide base and bisfluorosulfonimide, which is applied in the field of fluorine chemical industry, can solve the problem of hindering the large-scale application of bisfluorosulfonimide and its alkali metal salts, mainstream electrolyte materials, and production processes Long process and other issues, to achieve the effect of reducing material consumption and waste generation, simple reaction equipment, and low raw material cost

Inactive Publication Date: 2017-11-24
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method reported in this patent has the following disadvantages: the reaction steps are too long, the price of antimony trifluoride is high, and it is difficult to scale up industrially; the consumption of raw materials is large and a large amount of waste is generated, and the product has many impurities, and it is difficult to purify to meet the application standards
However, the production process of the methods reported in these patents is too long, the consumption of raw materials is too large, and the waste production is too much, so it is difficult to scale up industrially.
If the above problems are not solved, it will hinder the large-scale application of bisfluorosulfonimide and its alkali metal salts, especially hinder its becoming the mainstream electrolyte material in new energy devices such as lithium-ion batteries and supercapacitors.

Method used

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  • Difluoro-sulfonyl imine preparation method and method for preparing difluoro-sulfonyl imine alkali metal salt by using prepared difluoro-sulfonyl imine
  • Difluoro-sulfonyl imine preparation method and method for preparing difluoro-sulfonyl imine alkali metal salt by using prepared difluoro-sulfonyl imine
  • Difluoro-sulfonyl imine preparation method and method for preparing difluoro-sulfonyl imine alkali metal salt by using prepared difluoro-sulfonyl imine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1 Preparation of polystyrene-supported antimony pentafluoride, bischlorosulfonimide and bisfluorosulfonimide, and activation of polystyrene-supported antimony pentafluoride

[0033] After 100g of polystyrene was dried under vacuum at 60°C for 6h, it was added to 1000g of dichloromethane to swell for 4h, then 400g of antimony pentafluoride was added, and the reaction was stirred at 30°C. The polystyrene microspheres gradually turned red and ended after 12h. reaction. Suction filtration, washing with dichloromethane, toluene and acetone respectively, and vacuum drying to obtain 400 g gray polystyrene antimony pentafluoride microspheres.

[0034] Under agitation, add 580g chlorosulfonic acid (5mol) and 721g chlorosulfonyl isocyanate successively in a dry 2L reaction vessel, then heat the mixed solution to 120°C for reaction, and use a carbon dioxide gas detector to detect that the carbon dioxide concentration is less than 500ppm. The reaction was stopped, and the ...

Embodiment 2

[0038]Example 2: Preparation of lithium bisfluorosulfonyl imide Under stirring, 580 g of chlorosulfonic acid (5 mol) and 721 g of chlorosulfonyl isocyanate were successively added to a dry 2L reaction vessel, and then the mixture was heated to 120°C for reaction, using After the carbon dioxide gas detector detects that the carbon dioxide concentration is less than 500ppm, stop the reaction, carry out vacuum distillation to the obtained brownish yellow liquid crude product, collect the cut of 80-85 ℃ / 30Pa, obtain 856g (yield 80%) dichlorosulfonyl Amine is a colorless liquid.

[0039] Under constant temperature stirring at 25°C, add 400g of polystyrene-loaded antimony pentafluoride, 600g of acetonitrile, and 42.4g of anhydrous lithium chloride into a 2L three-neck flask, and then slowly add 214g of dichlorosulfonimide (1mol) for fluorination Reaction, after adding dichlorosulfonimide dropwise, keep the constant temperature of 25°C to continue the reaction for 6 hours, and then f...

Embodiment 3

[0040] The preparation of embodiment 3 bisfluorosulfonimide lithium

[0041] Under constant temperature stirring at 25°C, add 400g of polystyrene-loaded antimony pentafluoride and 600g of acetonitrile into a 2L three-neck flask, then slowly add 214g of dichlorosulfonimide (1mol) for fluorination reaction, and dropwise add dichlorosulfonimide After the imide, add 42.4g of anhydrous lithium chloride to the system, keep a constant temperature of 25°C to continue the reaction for 6 hours, and then filter with suction. The filter cake is polystyrene-supported antimony pentafluoride, which is used after activation, and the filtrate is rotary evaporated After removing the solvent, 160 g (yield 85.6%) of lithium bisfluorosulfonyl imide remained. The obtained crude lithium bisfluorosulfonyl imide was recrystallized using a mixed solvent of acetonitrile and dichloromethane at a mass ratio of 1:1 to obtain 146 g of a white powdery solid with a yield of 78.1%.

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Abstract

The invention belongs to the technical field of fluorine chemical industry, and especially relates to a difluoro-sulfonyl imine preparation method and a method for preparing difluoro-sulfonyl imine alkali metal salt by using prepared difluoro-sulfonyl imine. The difluoro-sulfonyl imine preparation method comprises the following steps: polystyrene and antimony pentalfluoride are added in a solvent and are subjected to reaction to obtain polystyrene-loaded antimony pentalfluoride, difluoro-sulfonyl imin liquid is added for a reaction, after the reaction is completed, pumping filtration and underpressure distillation are carried out to obtain the difluoro-sulfonyl imin; the method for preparing difluoro-sulfonyl imine alkali metal salt by using the prepared difluoro-sulfonyl imine comprises the following steps: adding difluoro-sulfonyl imine, an alkali metal compound and polystyrene-loaded antimony pentalfluoride in a reaction solvent, reacting the materials for 6-10 h under the reaction temperature of 0-100 DEG C, filtering the materials after the reaction is completed to obtain a difluoro-sulfonyl imine alkali metal salt crude product, and re-crystallizing the difluoro-sulfonyl imine alkali metal salt crude product to obtain a difluoro-sulfonyl imine alkali metal salt fine product. The method has the advantages of controllable reaction, safety, high efficiency, and high yield, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, and in particular relates to a method for preparing bisfluorosulfonimide and a method for preparing alkali metal salt of bisfluorosulfonimide by using the prepared bisfluorosulfonimide. Background technique [0002] Bisfluorosulfonimide and bisfluorosulfonimide alkali metal salts, especially lithium salts, are important fluorine-containing compounds. They are used as key high-performance electrolyte materials in new energy devices such as lithium-ion batteries and supercapacitors. High industrial application value. [0003] The chemical structural formula of bisfluorosulfonimide and alkali metal salt of bisfluorosulfonimide is as follows: [0004] [0005] In the patent CN101747242A, firstly, dichlorosulfonimide is obtained by reacting sulfonamide with thionyl chloride and chlorosulfonic acid, then reacted with antimony trifluoride to obtain bisfluorosulfonimide, and then r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086
Inventor 石宇林存生邢宗仁胡葆华迟鹏利周勇
Owner VALIANT CO LTD
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