Method for preparing bi-(sulfonyl fluoride) imine and (fluorinated alkyl sulfonyl fluorine sulfonyl) imine alkali metal salt

A technology of alkali metal salt and sulfonamide, applied in the field of fluorine chemical synthesis, can solve the problems of difficult purification of the product, pollute the environment, complicated operation, etc., and achieve the effects of avoiding product agglomeration, high yield and purity, and easy operation.

A technology of alkali metal salt and sulfonamide, applied in the field of fluorine chemical synthesis, can solve the problems of difficult purification of the product, pollute the environment, complicated operation, etc., and achieve the effects of avoiding product agglomeration, high yield and purity, and easy operation.

CN101747242BActive Publication Date: 2013-06-19武汉市瑞华新能源科技有限公司
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  • Method for preparing bi-(sulfonyl fluoride) imine and (fluorinated alkyl sulfonyl fluorine sulfonyl) imine alkali metal salt
  • Method for preparing bi-(sulfonyl fluoride) imine and (fluorinated alkyl sulfonyl fluorine sulfonyl) imine alkali metal salt
  • Method for preparing bi-(sulfonyl fluoride) imine and (fluorinated alkyl 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]

[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 to remove excess low-boiling reactants, then carry out vacuum distillation, collect 112-114 ° C / 2mmHg fraction, at room temperature to obtain bis (chlorosulfonyl) imide (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 hours, 350 mL of acetonitrile was added to the re...

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 bi-(sulfonyl fluoride) imine and (fluorinated alkyl sulfonyl fluorine sulfonyl) imine alkali metal salt. The method comprises the following steps of: reacting sulfamide and thionyl chloride and chlorosulfonic acid to prepare bi-(sulfonyl chlorine) imine and (fluorinated alkyl sulfonyl chlorine sulfonyl) imine, reacting with antimony trifluoride and potassium carbonate (rubidium or caesium) to obtain corresponding high-purity bi-(sulfonyl fluoride) imine potassium (rubidium or caesium) salt or (fluorinated alkyl sulfonyl fluorine sulfonyl) imine potassium (rubidium or caesium) salt, performing double decomposition exchange reaction using the potassium (rubidium or caesium) salt with the lithium perchlorate (or sodium) or lithium tetrafluoroborate (or sodium) in the aprotic polar solvent to obtain corresponding lithium (or sodium) salt with high purity. The method in the invention has the characteristics of simple operating steps, easy separation and extraction of output, high purity and yield, no environmental pollution, and the like, and is suitable for mass industrial production.

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

Patent Timeline
19 Jun 2013
Publication
CN101747242B
IPC
C07C311/01; C07C303/36
Inventors
周志彬; 韩洪波