Method for preparing bis(trifluoromethanesulfonyl)imide metal salt

A bistrifluoromethanesulfonimide and trifluoromethanesulfonimide technology, which is applied in the field of preparing bistrifluoromethanesulfonimide metal salts, can solve complex post-treatment procedures, excessive intermediate raw materials, and process steps Long-term problems, to achieve the effect of cheap raw materials, simple process route, and easy-to-obtain raw materials

Inactive Publication Date: 2009-06-17
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been reported abroad that the trifluorosulfonyl halide reacts with liquid ammonia to generate trifluorosulfonamide ammonium salt, which is acidified with hydrochloric acid to obtain trifluorosulfonamide, which is reacted with sodium methoxide under the protection of hexamethyldisilazane to prepare A method for preparing bistrifluoromethanesulfonimide metal salt, but the process steps are long, the yield is low, only 30%, and it involves too many intermediate raw materials and complicated post-treatment procedures.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 362.5g of dichloromethane and 202g of triethylamine into a special stainless steel reaction vessel. After cooling to -20°C, 8.5g of anhydrous liquid ammonia and 152g of trifluoromethanesulfonyl fluoride are introduced under stirring, and then React for 4 hours at 20°C. After the reaction is complete, cool and filter to remove the triethylamine hydrogen fluoride salt generated by the reaction. The obtained filtrate is distilled to remove the solvent dichloromethane and excess triethylamine at 40°C / 10Pa. The filtrate is evaporated to dryness. It is solid bistrifluoromethanesulfonimide triethylamine salt, weighed to obtain 184g. The obtained bis(trifluoromethanesulfonimide) triethylamine salt, 40g of lithium hydroxide and 360g of aqueous solution were stirred and mixed at room temperature (25°C) and reacted for 2 hours. After the reaction was completed, the resulting solution was heated at 40°C / The water and the triethylamine produced were distilled off at 10Pa to obtain ...

Embodiment 2

[0022] Add 785.5g of dichloroethane and 600g of pyrimidine into a special stainless steel reaction vessel. After cooling to -10°C, add 17g of anhydrous ammonia gas and 168.5g of trifluoromethanesulfonyl chloride with stirring, and then increase to 40 ℃, react for 4 hours. After the reaction is complete, cool and filter to remove the pyrimidine hydrochloride produced by the reaction. The obtained filtrate is distilled to remove the solvent dichloroethane and excess pyrimidine under the condition of 80 ℃ / 100 Pa. The filtrate is evaporated to dryness, which is a solid bis The trifluoromethanesulfonimide pyrimidine salt was weighed to obtain 160 g. The obtained bis(trifluoromethanesulfonimide) pyrimidine salt, 100g of sodium carbonate, 900g of water, stirred and mixed at room temperature (25°C), reacted for 2 hours, after the reaction was completed, the resulting solution was distilled off at 100°C / 100Pa Water and the generated pyrimidine, the solution was evaporated to dryness, dried...

Embodiment 3

[0024] Add 500g of trichloroethane and 395g of pyridine into a special stainless steel reaction vessel. After cooling to 40°C, 12.8g of anhydrous ammonia gas and 152g of trifluoromethanesulfonyl fluoride are introduced with stirring, and then heated to 60°C After 4 hours of reaction, after the reaction is complete, cool and filter to remove the pyridine hydrogen fluoride salt generated by the reaction. The obtained filtrate is distilled to remove the solvent trichloroethane and excess pyridine under the condition of 60℃ / 50Pa. The filtrate is evaporated to dryness, and it is solid bistrifluoride Methanesulfonimide tripyridine salt, weighed to obtain 178 g. The obtained bis(trifluoromethanesulfonimide) pyridinium salt, 56g potassium hydroxide, 500g aqueous solution, stirred and mixed at room temperature (25℃), reacted for 2 hours, after the reaction was completed, the resulting solution was distilled at 80℃ / 50Pa The water and the generated pyridine are removed, the solution is evapo...

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PUM

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Abstract

The invention discloses a method for preparing bis(trifluoromethylsulfonyl)imide metallic salt. The method comprises the following steps: trifluoromethane halogenated sulfonyl, liquid ammonia and organic amine alkali as raw materials are used to generate a mixture solvent containing bis(trifluoromethylsulfonyl)imide quaternary ammonium salt by a nonpolar inert solvent; the mixture containing the bis(trifluoromethylsulfonyl)imide quaternary ammonium salt is distilled to reclaim the solvent so as to obtain a bis(trifluoromethylsulfonyl)imide quaternary ammonium salt solid; the bis(trifluoromethylsulfonyl)imide quaternary ammonium salt solid reacts with alkali metal oxide in an aqueous solution to generate a mixture of the bis(trifluoromethylsulfonyl)imide metallic salt; and finally, the target product is prepared by the obtained mixture of the bis(trifluoromethylsulfonyl)imide metallic salt through decompressed dehydrating, decompressed drying and other steps. The process has a simple route, and does not pollute the environment. The purity of the bis(trifluoromethylsulfonyl)imide metallic salt prepared by the method is more than 99 percent, and the yield is over 90 percent.

Description

Technical field [0001] The invention relates to a method for preparing bistrifluoromethanesulfonimide metal salt. Background technique [0002] Bistrifluoromethanesulfonimide metal salt as a high-voltage and high-temperature resistant electrolyte lithium salt is mainly used in the field of lithium battery electrolyte additives. At present, the preparation of the lithium salt is still under research at home and abroad, and there is basically no literature report on its synthesis process. Based on the potential demand of the lithium battery market, the preparation of bistrifluoromethanesulfonimide metal salt has been one of the hot spots of research. . It has been reported in foreign countries that the trifluorosulfonyl halide reacts with liquid ammonia to generate trifluorosulfonamide ammonium salt. After acidification with hydrochloric acid, trifluorosulfonamide is obtained by reacting with sodium methoxide under the protection of hexamethyldisilazane. The preparation method of b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/03C07C303/38H01M10/40
CPCY02E60/10
Inventor 张先林刘东杨志勇林刚李伟峰
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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