Preparation method of bis(sulfonyl fluoride) imine and (perfluoroalkyl sulfonyl fluorine sulfonyl) imine alkali metal salt

Abstract

The invention discloses a method for preparing bis(sulfonyl fluoride) imine and (perfluoroalkyl sulfonyl fluorine sulfonyl) imine alkali metal salt. According to the method, sulfamide is utilized to take reaction with thionyl chloride and chlorosulfonic acid for preparing bis(sulfonyl fluoride) imine or (perfluoroalkyl sulfonyl fluorine sulfonyl) imine, then, the bis(sulfonyl fluoride) imine or (perfluoroalkyl sulfonyl fluorine sulfonyl) imine takes reaction with antimony trifluoride and potassium (rubidium or caesium and the like) carbonate, and corresponding high-purity bis(sulfonyl fluoride) imine potassium (rubidium or caesium) salt or (perfluoroalkyl sulfonyl fluorine sulfonyl) imine potassium (rubidium or caesium) salt can be obtained; and the double decomposition exchange reaction of the potassium (rubidium or caesium) salt and lithium (or sodium) perchlorate or lithium (or sodium) tetrafluoroborate and the like in aprotic polar solvents is utilized to obtain corresponding high-purity lithium (or sodium) salt. The method provided by the invention has the characteristics that the operation step is simple, the products can be easily separated and purified, the purity and the yield are high, the environment pollution is avoided, the method is suitable for industrial mass production, and the like.

Description

technical field [0001] The invention belongs to the chemical synthesis of fluorine, and relates to a preparation method of an alkali metal salt of a fluorine-containing imine, in particular to a bis(fluorosulfonyl)imide (H[N(SO 2 F) 2 ]) and (perfluoroalkylsulfonylfluorosulfonyl)imine (H[R f SO 2 NSO 2 F], R f =C m f 2m+1 , m=1-8) alkali metal salt (M[N(SO 2 F) 2 ], M[R f SO 2 NSO 2 F)]; Preparation of M = Li, Na, K, Rb, Cs). Background technique [0002] Bis(fluorosulfonyl)imide (H[N(SO 2 F) 2 ], hereinafter referred to as H[FSI]) and (perfluoroalkylsulfonylfluorosulfonyl)imine (H[R f SO 2 NSO 2 F)], R f =C m f 2m+1 , m=1-8; hereinafter referred to as H[R f FSI]) alkali metal salts, especially lithium salts, are important fluorine-containing organic ion compounds, which are used in high-performance non-aqueous electrolyte materials for clean energy devices such as secondary lithium batteries, supercapacitors, and aluminum electrolytic capacitors, as well...

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Problems solved by technology

[0013] The object of the present invention is to provide a kind of bis (fluorosulfonyl) imide (H [N (SO 2 f) 2 ], referred to as H[FSI]) and (perfluoroalkylsulfonylfluorosulfonyl)imine (H[R f SO 2 NSO 2 F]), referred to as H[R f FSI];R f =C m f 2m+1 , m=1-8) alkali metal salt (M[FSI], M[R f FSI]; the preparation method of M=Li, Na, K, Rb, Cs) makes it have characteristics such as simple operation steps, easy separation and purification of products, high purity and yield, no environmental pollution, and being suitable for industrialized mass production. Overcome the shortcomings of existing methods such as cumbersome operation, low yield, pollution of the environment by using toxic reagents, use of difficult-to-operate fluorine-containing gas reagents, cumbersome product separation operations, and difficult purification of products.

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