Imine alkali metal salt and ion liquid and application of same as non water electrolyte
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A technology of alkali metal salts and imine bases, applied in circuits, electrical components, secondary batteries, etc., can solve the problems of long synthesis route, high price, and unsuitable for large-scale preparation.
Inactive Publication Date: 2012-12-12
HUAZHONG UNIV OF SCI & TECH +1
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But the shortcoming of this preparation method is: (1) with trifluoromethanesulfonyl isothiocyanate (CF 3 SO 2 N=S=O) is a raw material, and the yield of synthesizing this raw material is lower; (2) use Ruppert reagent (trimethyltrifluoromethylsilane, CF 3 SiMe 3 ), the price is more expensive, not suitable for large-scale preparation; (3) from the raw material trifluoromethylsulfonyl isothiocyanate (CF 3 SO 2 N=S=O) to the final product, the synthetic route is longer, and the overall yield is low
[0010] 2) Trifluoromethyl (S-trifluoromethylsulfonylimide) sulfonyl chloride (CF 3 (CF 3 SO 2 N) SOCl, formula (II)) through fluorination reaction to obtain trifluoromethyl (S-trifluoromethylsulfonylimide) sulfonyl fluoride (CF 3 (CF 3 SO 2 N)SOF), further and lithium nitride (Li 3 N) reaction to synthesize bis(trifluoromethyl (S-trifluoromethylsulfonimide) sulfonyl)imide lithium ([(
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Embodiment 1-9
[0115] Embodiment 1-9 relates to the preparation of imide alkali metal salt containing "S-fluoroalkylsulfonylimide group"
Embodiment 1
[0116] Embodiment 1: (trifluoromethylsulfonyl) (trifluoromethylsulfinyl) potassium imide ([(CF 3 SO 2 )(SOCF 3 )N] K) The preparation synthesis reaction scheme is as follows:
[0117] CF 3 SO 2 Na+SOCl 2 → CF 3 SOCl+NaCl+SO 2
[0118]
[0119] Add sodium trifluoromethanesulfinate (CF 3 SO 2 Na) (65.5 g, 0.42 mol), 100 mL of chlorobenzene. Stir mechanically, heat to 30°C, slowly add SOCl dropwise 2 (59.5 g, 0.5 mol), stirring was continued for 2 hours after the dropwise addition was completed. Atmospheric distillation, collecting fractions at 30°C. 55 g of trifluoromethanesulfonyl chloride (pale brown liquid) are obtained, yield 87%.
[0120] Add trifluoromethanesulfonamide (CF 3 SO 2 NH 2 ) (29.8g, 0.2mol), acetonitrile (80mL), and pyridine (31.6g, 0.4mol) were used as acid-binding agents, stirred and dissolved, and trifluoromethylsulfinyl chloride (CF 3 SOCl) (35g, 0.23mol), the ice bath was removed after the dropwise addition, and after stirring at room t...
Embodiment 2
[0121] Example 2: Trifluoromethyl (S-trifluoromethylsulfonimide) sulfonamide (CF 3 (CF 3 SO 2 N)SONH 2 ) preparation
[0122]
[0123] Potassium (trifluoromethylsulfonyl) (trifluoromethylsulfinyl)imide ([(CF 3 SO 2 )(SOCF 3 )N]K) (66.7g, 0.22mol) was dissolved in 200mL distilled water, and was added successively under mechanical stirring 2 OSO 3 H) (38.2g, 0.34mol) and sodium acetate (CH 3 CO 2 Na) (27.9g, 0.34mol), after stirring for 8 hours, extracted with ether (50mLx3), and combined the organic phases. After adding anhydrous magnesium sulfate to dry, filter, collect the filtrate, and remove ether by rotary evaporation to obtain a white flaky solid. Yield 34.8g, 60% yield.
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Abstract
The invention provides ion liquid composed of fluoroalkyl sulfimide salt alkali metal salt containing 'S-fluoroalkyl sulfimide group', fluoroalkyl sulfimide negative ions containing 'S-fluoroalkyl sulfimide group' and positive ions of sulfonium salt, ammonium salt and microcosmic salt. The ion liquid utilizes (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine with sulfur valence state as +4 and hydroxylamine oxygen sulfonic acid to react to prepare intermediate fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide, effectively shortens the line that the (fluoroalkyl sulfonyl) (fluoroalkyl sulfinyl) imine is utilized to prepare fluoro alkyl (S- fluoroalkyl sulfimide group) sulfamide of fluoroalkyl sulfimide through the three steps of chlorination, fluorination and amination, and is convenient to operate and high in yield and purity. The alkali metal salt has good heat stability and hydrolysis resistance, has high conductivity and oxidation potential in traditional carbonic ester solution, and is good in compatibility with electrode materials widely used. The ion liquid can be applied to lithium ion batteries and carbon-based super capacitors.
Description
technical field [0001] The invention belongs to the field of organic fluorine chemistry, new materials and advanced power supply technology, and specifically relates to an alkali metal salt of a fluoroalkylsulfonimide containing an "S-fluoroalkylsulfonimide group", an ionic liquid and its preparation Method, and the application of the alkali metal salt and ionic liquid as electrolyte materials in secondary lithium (ion) batteries and carbon-based supercapacitors. Background technique [0002] Fluorine-containing sulfonyl imides and their alkali metal salts, especially lithium salts, are important fluorine-containing ion compounds. They are used in high-performance nonaqueous Electrolyte materials, new high-efficiency catalysts and other fields have important industrial application value. [0003] At present, most of the researches on fluorine-containing sulfonimides focus on monobasic fluorine-containing sulfonimides (Coord.Chem.Revs., 1997, 158, 413.), that is, the anion s...
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