Preparation method for lithium bis(fluorosulfonyl)imide
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A technology of lithium bisfluorosulfonyl imide and bisfluorosulfonimide, which is applied in the field of compound preparation, can solve the problems of high content of ionic impurities and low yield, and achieve simple preparation process, high yield and short reaction time Effect
Active Publication Date: 2017-09-22
常德市大度新材料有限公司
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Problems solved by technology
However, the existing methods have defects such as low yield and high content of ionic impurities.
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Embodiment 1
[0022] FSO 2 NH 2 +Li 2 CO 3 →FSO 2 NHL
[0023] SO 2 Cl 2 +KF→SO 2 f 2
[0024] FSO 2 NHLi+SO 2 f 2 +Py→FSO 2 NHSO 2 F·Py
[0025]
[0026] FSO 2 NHSO 2 F+Li 2 CO 3 →FSO 2 NNSO 2 f
[0027] Add 49.5g (0.5mol) fluorosulfonamide in the reaction bottle of 500mL, add acetonitrile under ice-water bath as solvent, add 20.4g (0.275mol) lithium carbonate anhydrous, stir to neutrality, filter under reduced pressure, reduce after obtaining clear filtrate Dry under pressure to obtain the crude product of lithium fluorosulfonamide.
[0028] To a 500mL reaction flask, add the lithium fluorosulfonamide prepared in the previous step, add 200mL dry acetonitrile and 39.5g (0.5mol) pyridine, take an ice-water bath, take another 500mL reaction flask, add 135g (1mol) sulfuryl chloride, 200mL dicarbonate Ethyl ester, 69.6g (1.2mol) anhydrous potassium fluoride, magnetic stirring, temperature control 80 degrees, reaction flask connected to -20 degrees reflux condenser, th...
Embodiment 2
[0031] FSO 2 NH 2 +LiOH→FSO 2 NHL
[0032] SO 2 Cl 2 +NaF→SO 2 f 2
[0033] FSO 2 NHLi+SO 2 f 2 +(C 2 h 5 ) 3 N→FSO 2 NHSO 2 F·Py
[0034]
[0035] FSO 2 NHSO 2 F+LiOH→FSO 2 NNSO 2 f
[0036] Add 49.5g (0.5mol) fluorosulfonamide to a 500mL reaction flask, add acetonitrile as a solvent in an ice-water bath, add 6.6g (0.275mol) lithium hydroxide, stir until neutral, filter under reduced pressure, and depressurize after obtaining a clear filtrate After drying, the crude product of lithium fluorosulfonamide was obtained.
[0037] To a 500mL reaction flask, add the lithium fluorosulfonamide prepared in the previous step, add 200mL dry acetonitrile and 50.5g (0.5mol) triethylamine, take an ice-water bath, take another 500mL reaction flask, add 135g (1mol) sulfuryl chloride, 200mL Diethyl carbonate, 50.4g (1.2mol) anhydrous sodium fluoride, magnetic stirring, temperature control 80 degrees, the reaction bottle is connected to a reflux condenser at -20 degrees...
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Abstract
The invention discloses a preparation method for lithium bis(fluorosulfonyl)imide. The preparation method comprises the following steps: 1) preparing fluorine sulfamide lithium; 2) preparing sulfuryl fluoride, and pumping the sulfuryl fluoride into the fluorine sulfamide lithium solution, and adding an acid-binding agent to prepare bifluorine sulfimide ammonium salt; 3) dissolving the bifluorine sulfimide ammonium salt in water solution, to obtain bifluorine sulfimide water solution through the acid resin exchange; 4) adding lithium carbonate, regulating the PH value to be neutral, filtering and removing undissolved substances, depressurizing and removing the most of the water, and adding a weak-polarity organic solvent to separate out a coarse product of the lithium bis(fluorosulfonyl)imide, further depressurizing and drying; and 5) adding a polarity solvent to the coarse product of the lithium bis(fluorosulfonyl)imide, stirring and dissolving, filtering and removing the undissolved substances, depressurizing and removing a strong-polarity solvent, and adding the weak-polarity organic solvent to perform the recrystallization, and depressurizing and drying to obtain a product after filtering. The preparation method is simple, the reaction time is short, the yield is high, and metal ion and negative ion impurities can be effectively controlled, so that the product with the high purity can be obtained.
Description
technical field [0001] The invention relates to the technical field of compound preparation, in particular to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Fluorosulfonyl imide and related compounds play an extremely important role in the field of material chemistry and electrochemical energy storage, especially lithium trifluoromethanesulfonyl imide and lithium bisfluorosulfonyl imide have Important industrial application value. Bisfluorosulfonimide is an important raw material for the preparation of lithium salts and other alkali metal salts and derivatives. Bisfluorosulfonimide is generally prepared by fluorination of bischlorosulfonimide. The preparation process of bischlorosulfonimide is mainly Including: 1) Preparation by reaction of phosphorus pentachloride, sulfamic acid and chlorosulfonic acid (K.Ruff et al, Inorg.Synth.1968, 11, 138); 2) Preparation by reaction of sulfamic acid, thionyl chloride and chlorosulfonic acid (M....
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