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A kind of method that utilizes acid anhydride-water system to prepare bis(fluorosulfonyl)imide

A fluorosulfonyl and imide technology, applied in the field of fluorine chemical lithium battery electrolyte, can solve the problems of easy decomposition, difficult to purify, difficult to sublime of HFSI, etc., and achieves the effects of low cost, low cost and simple post-processing

Active Publication Date: 2022-03-22
LEE & MAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, due to the selection of 100% concentrated sulfuric acid, HFSI is difficult to sublimate, and it is easy to decompose during the heating process, and many by-products are obtained, and it is difficult to purify in the later stage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of bis(fluorosulfonyl)imide (HFSI):

[0028] Under nitrogen protection, to a 500mL three-necked flask equipped with a stirrer, first add sodium bis(fluoroacyl)imide (203g, 1mol), then add trifluoroacetic anhydride (105g, 0.5mol) to the reaction flask, stir at room temperature, and then Slowly add one equivalent of water (9g, 0.5mol) dropwise to the reaction system, and the slow dropwise addition can control the slow occurrence of the reaction. After the reaction is complete (ie, the reaction is 2h), directly carry out vacuum distillation at a distillation temperature of 70°C. The distillation pressure is 0.5MPa, and the fraction at about 50°C is collected. After cooling, it becomes a colorless crystal. After melting, it is tested to be bis(fluorosulfonyl)imide HFSI. The yield is 90%, and the content is ≥99.9%.

Embodiment 2

[0030] Preparation of bis(fluorosulfonyl)imide (HFSI):

[0031] Under nitrogen protection, first add bis(fluoroacyl)imide potassium (219g, 1mol) to a 500mL three-necked flask equipped with a stirrer, then add trifluoromethanesulfonic anhydride (141g, 0.5mol) to the reaction flask, stir at room temperature, Slowly add one equivalent of water (9g, 0.5mol) dropwise to the reaction system. Slow dropwise addition can control the slow occurrence of the reaction. After the reaction is complete (ie, react for 2.5h), directly carry out vacuum distillation at a distillation temperature of 60 ℃, the distillation pressure is 0.4MPa, and the distillate at about 50℃ is collected. After cooling, it becomes a colorless crystal. After melting, it is tested as bis(fluorosulfonyl)imide HFSI. The yield is 92%, and the content is ≥99.9%.

Embodiment 3

[0033] Preparation of bis(fluorosulfonyl)imide (HFSI):

[0034]Under nitrogen protection, first add bis(fluoroacyl)imide potassium (219g, 1mol) to a 500mL three-necked flask equipped with a stirrer, then add trifluoroacetic anhydride (105g, 0.5mol) in the reaction flask, stir at room temperature, and then Slowly add one equivalent of water (9g, 0.5mol) dropwise to the reaction system, and the slow dropwise addition can control the slow occurrence of the reaction. After the reaction is complete (ie, the reaction is 2h), directly carry out vacuum distillation at a distillation temperature of 70°C. The distillation pressure is 0.6MPa, and the fraction at about 50°C is collected. After cooling, it becomes a colorless crystal. After melting, it is tested to be bis(fluorosulfonyl)imide HFSI. The yield is 88%, and the content is ≥99.9%.

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Abstract

The invention discloses a method for preparing bis(fluorosulfonyl)imide using an acid anhydride-water system. The method comprises the following steps: The crude product of bis(fluorosulfonyl)imide is prepared by reaction of salt and strong acid anhydride in the presence of water; then high-purity bis(fluorosulfonyl)imide is obtained by vacuum distillation. The preparation method provided by the invention has the advantages of simple method, less side reactions, mild operating conditions, wide application range and the like.

Description

technical field [0001] The invention belongs to the technical field of lithium battery electrolytes in fluorine chemical industry, and in particular relates to a method for preparing bis(fluorosulfonyl)imide using an acid anhydride-water system. Background technique [0002] Bis(fluorosulfonyl)imide (CAS: 14984-73-7), molecular formula HN(SO 2 f) 2 , referred to as HFSI. HFSI is a strong acid, and its salt is widely used in catalysis, electrolyte, fluorinating agent, etc., especially its lithium salt has high thermal stability, does not decompose below 200°C, and has good chemical stability. significantly better than lithium hexafluorophosphate (LiPF 6 ). Therefore, HFSI has become an important product in the study of lithium battery electrolytes. In addition, it is a very good acidic catalyst and has the advantages of being environmentally friendly, so it has important economic and social values. [0003] Bis(fluorosulfonyl)imide is an important raw material for prepar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B21/093H01M10/0567H01M6/16
CPCC01B21/09H01M10/0567H01M6/168H01M2300/0025C01P2006/80Y02E60/10
Inventor 苏秋铭张梦辛伟贤谢文健陈新滋
Owner LEE & MAN CHEM CO LTD
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