Fluorine containing sulfonylimine spiro quaternary ammonium salt electrolyte and preparation method and application thereof
A fluorosulfonimide spiro and sulfonimide spiro technology, applied in the field of supercapacitors, can solve the problems of strong corrosiveness of hydrogen fluoride reagent, low product yield and high energy consumption, achieve high electrochemical stability, reduce halogen Content, low corrosive effect
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Embodiment 1
[0037] Example 1: Preparation of bisfluorosulfonimide spiro 1,1'-bispyrrole quaternary ammonium salt (SBP-FSI)
[0038] Under constant temperature stirring at 20°C, 1000 mL of distilled water, 215.91 g (1 mol) of 1,4-dibromobutane, 48 g (1.2 mol) of sodium hydroxide, 263.06 g (1.2 mol) of difluorobutane were sequentially added to a dry three-necked flask Sulfonimide potassium salt was mixed evenly to form a mixed solution, and then slowly added dropwise 71.12g (1mol) of tetrahydropyrrole into the mixed solution for 1 hour, and the dropping temperature was controlled at 20°C, and heated to Stirring was continued at 60°C for 6 h; then the solid was collected by filtration to obtain the crude product of bisfluorosulfonimide spiro 1,1'-bispyrrole quaternary ammonium salt. The obtained difluorosulfonimide spiro 1,1'-bispyrrole quaternary ammonium salt crude product was extracted 3 times with a mixture of dichloromethane (200ml) and water (100ml) at a volume ratio of 2:1, and the or...
Embodiment 2
[0040] Example 2: Preparation of two trifluoromethylsulfonylimide spiro 1,1'-bispyrrole quaternary ammonium salt (SBP-TFSI)
[0041] Under stirring, add 1000mL distilled water, 127.01g (1mol) 1,4-dichlorobutane, 48g (1.2mol) sodium hydroxide, 383.06g (1.2mol) bistrifluoromethylsulfonyl Amine potassium salts were mixed to form a mixed solution, and then 71.12 g (1 mol) tetrahydropyrrole was slowly added dropwise into the mixed solution for 1 hour, and the dropping temperature was controlled at 10°C. After the dropwise addition, the mixture was heated to 60°C and continued to stir for 6 hours, and then the solid was collected by filtration to obtain the crude bistrifluoromethylsulfonimide spiro 1,1'-bispyrrole quaternary ammonium salt. The obtained bistrifluoromethylsulfonylimide spiro 1,1'-bispyrrole quaternary ammonium salt crude product was extracted 3 times with a mixed solution of dichloromethane (200ml) and water (100ml) at a volume ratio of 2:1, Collect the organic phase...
Embodiment 3
[0042] Example 3: Preparation of bisfluorosulfonimide spiropyrrole-1,1'-piperidine quaternary ammonium salt (ASD-FSI)
[0043] Add 1000mL of distilled water, 141.04g (1mol) of 1,5-dichloropentane, 48g (1.2mol) of sodium hydroxide, and 263.06g (1.2mol) of difluorosulfonimide potassium salt into a dry three-necked flask in succession under stirring Mix to form a mixed solution, then slowly dropwise add 71.12g (1mol) tetrahydropyrrole to the mixed solution, dropwise for 1h, dropwise temperature is controlled at 10°C, after the dropwise addition is completed, heat to 60°C and stir for 6h, then The solid was collected by filtration to obtain the crude product of the quaternary ammonium salt of spiropyrrole-1,1'-piperidine of difluorosulfonimide. The obtained bisfluorosulfonimide spiropyrrole-1,1'-piperidine quaternary ammonium salt crude product was extracted 3 times with a mixture of dichloromethane (200ml) and water (100ml) at a volume ratio of 2:1, and collected Organic phase; ...
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