90076-65-6Relevant articles and documents
7Li NMR studies on complexation reactions of lithium ion with cryptand C211 in ionic liquids: Comparison with corresponding reactions in nonaqueous solvents
Shirai, Atsushi,Ikeda, Yasuhisa
, p. 1619 - 1627 (2011)
7Li NMR spectra of DEME-TFSA [DEME = N,N-diethyl-N-methyl-N-(2- methoxyethyl)ammonium; TFSA = bis(trifluoromethanesulfonyl)amide], EMI-TFSA (EMI = 1-ethyl-3-methylimidazolium), MPP-TFSA (MPP = N-methyl-N-propylpyridinium), DEME-PFSA [PFSA = bis(pentafluoroethanesulfonyl)amide], and DEME-HFSA [HFSA = bis(heptafluoropropanesulfonyl)amide] ionic liquid (IL) solutions containing LiX (X = TFSA, PFSA, or HFSA) and C211 (4,7,13,18-tetraoxa-1,10-diazabicyclo[8.5.5] eicosane) were measured at various temperatures. As a result, it was found that the uncomplexed Li(I) species existing as [Li(X)2]- in the present ILs exchange with the complexed Li(I) ([Li?C211]+) and that the exchange reactions proceed through the bimolecular mechanism, [Li?C211]+ + [*Li(X)2]- = [*Li?C211]+ + [Li(X)2]-. Kinetic parameters [ks/(kg m-1 s-1) at 25 °C, ΔH?/(kJ mol-1), ΔS?/ (J K-1 mol-1)] are as follows: 5.57 × 10 -2, 69.8 ± 0.4, and -34.9 ± 1.0 for the DEME-TFSA system; 5.77 × 10-2, 70.6 ± 0.2, and -31.9 ± 0.6 for the EMI-TFSA system, 6.13 × 10-2, 69.0 ± 0.3, and -36.7 ± 0.7 for the MPP-TFSA system; 1.35 × 10-1, 65.2 ± 0.5, and -43.1 ± 1.4 for the DEME-PFSA system; 1.14 × 10-1, 64.4 ± 0.3, and -47.1 ± 0.6 for the DEME-HFSA system. To compare these kinetic data with those in conventional nonaqueous solvents, the exchange reactions of Li(I) between [Li?C211]+ and solvated Li(I) in N,N-dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) were also examined. These Li(I) exchange reactions were found to be independent of the concentrations of the solvated Li(I) and hence proposed to proceed through the dissociative mechanism. Kinetic parameters [ks/s -1 at 25 °C, ΔH?/(kJ mol-1), ΔS?/(J K-1 mol-1)] are as follows: 1.10 × 10-2, 68.9 ± 0.2, and -51.3 ± 0.4 for the DMF system; 1.13 × 10-2, 76.3 ± 0.3, and -26.3 ± 0.8 for the DMSO system. The differences in reactivities between ILs and nonaqueous solvents were proposed to be attributed to those in the chemical forms of the uncomplexed Li(I) species, i.e., the negatively charged species ([Li(X)2]-) in ILs, and the positively charged ones ([Li(solvent)n]+) in nonaqueous solvents.
Preparation method of lithium bis (trifluoromethanesulfonyl) imide
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Paragraph 0038-0046, (2021/01/11)
The invention provides a preparation method of lithium bis (trifluoromethanesulfonyl) imide. The method mainly comprises the following steps: neutralizing trifluoromethanesulfonamide with an alkali metal lithium salt to obtain a lithium trifluoromethanesulfonamide salt, the reaction yield is up to 99%, and reaction can be completed after 20 minutes of quick reaction; reacting the obtained lithiumtrifluoromethanesulfonamide with trifluoromethanesulfonyl chloride under the catalytic action of lithium carbonate, saccharin lithium, lithium oxalate and other lithium salts to obtain lithium bis (trifluoromethanesulfonyl) imide with the purity of 99.9% and the yield of higher than 95%. The preparation method of the lithium bis (trifluoromethanesulfonyl) imide is more convenient, safer, low in cost and free of metal impurities.
Preparation method of lithium bis(trifluoromethanesulphonyl)imide salt
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Paragraph 0033; 0034, (2019/03/08)
The invention provides a preparation method of lithium bis(trifluoromethanesulphonyl)imide salt. The preparation method is characterized by comprising steps as follows: trifluoromethane gas is introduced into a non-polar solvent solution of lithium alkylide at low temperature under anhydrous and nitrogen protective conditions and subjected to a reaction, trifluoromethyl lithium is prepared, afterthe reaction, a lithium bis(fluorosulfonyl)imide solution is slowly dropwise added to the trifluoromethyl lithium solution at the low temperature, white solids can be separated out in a dropwise adding process, a reaction solution is filtered after dropwise addition is finished, a filtrate is evaporated under reduced pressure to be dry, white solid wet salt is obtained and subjected to vacuum drying, and lithium bis(trifluoromethanesulphonyl)imide salt is obtained. The preparation method has the advantages as follows: bis(trifluoromethanesulphonyl)imide is synthesized with a one-pot method, compared with a traditional method, a process route is greatly simplified, separating difficulty of a product and a byproduct in a reaction process is reduced, product purity is improved, so that production cost is further reduced, product performance and cost competitiveness are improved, and feasible technical support is provided for large-scale industrial production.
A method of preparing lithium imide fluorine sulfuryl
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Paragraph 0048-0049; 0053-0054, (2017/01/19)
The invention relates to a method for preparing fluorine sulfimide lithium and belongs to the field of fine chemical industries. The method comprises the steps as follows: lithium salt and deionized water are prepared into a turbid liquid with the mass concentration of the lithium salt in a range of 20-50% in a reaction still, a refined fluorine sulfimide acid solution is added dropwise to obtain a reaction solution under the condition of stirring, the mass content of the deionized water in the fluorine sulfimide acid solution is in a range of 5-20%, the reaction temperature is in a range of 50-150 DEG C, and the reaction is stopped when the pH value of the reaction solution is in a range of 6-8. Non-vacuum drying is performed on the reaction solution firstly, and when the mass content of the deionized water is lower than or equal to 0.5%, vacuum drying is performed. The method is easy to operate, higher in process safety and capable of effectively improving the purity of products and satisfying requirements of lithium battery industries for the high purity.
