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

An alkali metal salt and sulfonamide technology, applied in the field of fluorine chemical synthesis, can solve the problems of difficult product purification, cumbersome operation, and environmental pollution, and achieve the effects of avoiding product agglomeration, easy operation, high yield and purity

Active Publication Date: 2012-11-21
武汉市瑞华新能源科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 separ

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Preparation of potassium bis(fluorosulfonyl)imide (K[FSI])

[0045] The synthesis reaction scheme is as follows:

[0046] HOSO 2 NH 2 +SOCl 2 +HOSO 2 Cl→H[N(SO 2 Cl) 2 ]+SO 2 ↑+HCl↑

[0047]

[0048] Under the protection of nitrogen, add 480 grams (5mol) of sulfamic acid, 1780 grams (15mol) of thionyl chloride, and 580 grams (0.5mol) of chlorosulfonic acid into a 5000mL reaction flask in sequence, and stir and react at 130°C for 24 hours , Atmospheric pressure distillation removes excessive low-boiling point reactant, then carries out vacuum distillation, collects the cut of 112-114 ℃ / 2mmHg, obtains two (chlorosulfonyl)imides (HN(SO 2 Cl) 2 ) 880 g (4.1 mol) of colorless crystals, yield 82%.

[0049] Under magnetic stirring and nitrogen protection, 96 grams (0.45mol) of bis(chlorosulfonyl)imide and 54 grams (0.3mol) of anhydrous antimony trifluoride were placed in a 500mL three-necked flask, and stirred at room temperature After reacting for 12 ...

Embodiment 2

[0051] Embodiment 2: Preparation of bis(fluorosulfonyl)imide cesium (Cs[FSI])

[0052] The synthesis reaction scheme is as follows:

[0053]

[0054] Under magnetic stirring and nitrogen protection, 9.6 grams (0.045mol) of bis(chlorosulfonyl)imide (prepared according to the operation of Example 1) and 5.4 grams (0.03mol) of anhydrous antimony trifluoride were placed in 100mL In a three-necked flask, after stirring for 12 hours at room temperature, 40 mL of acetonitrile was added to the reaction flask. After most of the solids were dissolved, 8.9 g (0.03 mol) of anhydrous cesium carbonate was added in portions under stirring, and the reaction was continued for 12 hours after the addition was complete. Then, the pH value of the system was adjusted to neutral with 2M HCl. Filter under reduced pressure to remove solid insoluble matter, concentrate the filtrate to about 10 mL, add an equal volume of CH 2 Cl 2 Perform recrystallization. After filtration, washing and drying, ...

Embodiment 3

[0055] Embodiment 3: Preparation of bis(fluorosulfonyl)imide lithium (Li[FSI])

[0056] The synthesis reaction scheme is as follows:

[0057]

[0058] In a vacuum glove box, add 91.5 g (0.34 mol) of potassium bis(fluorosulfonyl)imide (K[FSI]) and 250 mL of anhydrous acetonitrile into a 500 mL three-necked flask in sequence, stir to dissolve, and slowly Lithium perchlorate (LiClO 4 ) of acetonitrile solution 150mL (containing 36.2 grams of LiClO 4 ), stirred and reacted at room temperature for 24 hours, stood still overnight, and filtered under reduced pressure to remove insoluble potassium perchlorate (KClO 4 ), the filtrate was concentrated to about 60mL, and an equal volume of CH was added 2 Cl 2 Perform recrystallization. Filtration, CH 2 Cl 2 After washing and vacuum drying, 62 g (0.33 mol) of white solid powder Li[FSI] was obtained. 19 F NMR (acetone-d 6 , CCl 3 F, 376.5MHz): δ=51.8ppm(s).

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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...

Claims

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Application Information

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IPC IPC(8): C07C311/48C07C303/36
Inventor 周志彬韩洪波聂进刘凯郭鹏周宜轩
Owner 武汉市瑞华新能源科技有限公司
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