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Method for synthesizing perfluoroalkyl sulfimide alkali metal salt and ionic liquid synthesized by same

A technology of perfluoroalkyl sulfonimide and alkali metal salt, applied in the field of organic fluorine chemical synthesis, can solve the problem of rare ionic liquid, meet the requirements of high current charge and discharge, speed up the reaction and improve the yield Effect

Active Publication Date: 2010-06-23
武汉市瑞华新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the application of M[PFSI] ionic liquids in electrolyte materials and organic chemical reactions, although there have been a large number of literature reports, the cations in the current ionic liquids are mainly common imidazoles or quaternary ammonium salts. Cations (see recent representative literature: S.Maehama, H.Yoshimura, JP 2005200359, 2005; M.Kikuta, H.Uchimura, A. Hatakeyama, JP2007182410, 2007; A.Kawada, A.Tashiro, T.Kumagai, WO 2008108221, 2008; J. Rymarczyk, M. Carewska, G.B. Appetecchi, F. Alessandrini, S. Passerini, Eur. Polymer J., 2008, 44, 2153-2161; S. Seki, Y. Ohno, H. Miyashiro, Y.Kobayashi, A.Usami, Y.Mita, N.Terada, K.Hayamizu, S.Tsuzuki, M.Watanabe, J.Electrochem.Soc., 2008, 155, A421-A427.), and multifunctional Ionic liquids with branched cations are rare

Method used

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  • Method for synthesizing perfluoroalkyl sulfimide alkali metal salt and ionic liquid synthesized by same
  • Method for synthesizing perfluoroalkyl sulfimide alkali metal salt and ionic liquid synthesized by same
  • Method for synthesizing perfluoroalkyl sulfimide alkali metal salt and ionic liquid synthesized by same

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Experimental program
Comparison scheme
Effect test

Embodiment 1-12

[0058] Embodiment 1-12 relates to the preparation of M[PFSI]

Embodiment 1

[0059] Example 1: Preparation of potassium bis(trifluoromethylsulfonyl)imide (K[TFSI]).

[0060] The synthesis reaction scheme is as follows:

[0061]

[0062] 26.4 grams (0.14mol) trifluoromethanesulfonamide potassium salt, 13.4 grams (0.097mol) anhydrous potassium carbonate are placed in the three-necked flask of 250 milliliters, add 150 milliliters of acetonitriles as solvent, then add 24.0 grams (0.14mol) trifluoromethanesulfonyl chloride, stirred at room temperature for 8 hours.

[0063] The solvent was distilled off under reduced pressure to obtain a white solid, which was added with 150 ml of tetrahydrofuran, stirred at room temperature for 0.5 hour, and the insoluble matter was removed by filtration. The filtrate was distilled under reduced pressure, and the remaining solid was recrystallized with n-butanol. After filtration and drying, 39.2 g (0.12 mol) of K[TFSI] solid was obtained, with a yield of 88%. 19 F NMR (acetonitrile-d 3 , CCl 3 F, 376.5MHz): δ=-78.6p...

Embodiment 2

[0064] Example 2: Preparation of lithium bis(trifluoromethylsulfonyl)imide (Li[TFSI]).

[0065] The synthesis reaction scheme is as follows:

[0066] K[N(SO 2 CF 3 ) 2 ]+LiClO 4 →Li[N(SO 2 CF 3 ) 2 ]+KClO 4

[0067]In a vacuum glove box, 31.9 g (0.1 mol) of K[TSFI] was dissolved in 50 ml of acetonitrile solvent, and then equimolar lithium perchlorate was added in portions. After stirring the reaction at room temperature for 20 hours, insoluble potassium perchlorate was removed by filtration. Concentrate the filtrate to about 20 mL, add an equal volume of CH 2 Cl 2 Perform recrystallization. Filtration, CH 2 Cl 2 After washing and vacuum drying, 27.3 g (0.095 mol) of white solid powder Li[TFSI] was obtained. 19 F NMR (acetonitrile-d 3 , CCl 3 F, 376.5MHz): δ=-78.8ppm(s).

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Abstract

The invention discloses a method for synthesizing perfluoroalkyl sulfimide alkali metal salt (M[Rf1SO2NSO2Rf2]) which is abbreviated to M[PFSI], wherein Rf1 and Rf2=CmF2m+1, m=1-8, M=Li, Na, K, Rb, and Cs. The method utilizes potassium (rubidium and cesium) salt of perfluoroalkyl sulfamide and perfluoroalkyl sulfonyl fluoride for reaction in the existence of potassium carbonate (rubidium and cesium), so that the potassium (rubidium and cesium) salt of the perfluoroalkyl sulfimide can be conveniently prepared with high yield which is 70-90%; the high-purity corresponding lithium (or sodium) salt (M[PFSI], M=Li and Na) can be obtained through double decomposition exchange reaction of the potassium (rubidium and cesium) salt and lithium perchlorate (or sodium) in aprotic polar solvent (such as acetonitrile, dimethyl carbonate, nitromethane and the like); and the hydrophobic functionalized ionic liquid composed of cations of sulfonium, ammonium or phosphorus with the [PFSI] through reaction of the prepared alkali metal salt and the sulfonium salt, ammonium salt or phosphorus salt of which the side chain contains functionalized functional groups.

Description

technical field [0001] The invention belongs to organic fluorine chemical synthesis technology, in particular to a perfluoroalkylsulfonimide (H[R f 1 SO 2 NSO 2 R f 2 ],R f 1 , R f 2 =C m f 2m+1 , m=1-8) alkali metal salt (M[R f 1 SO 2 NSO 2 R f 2 ], M=Li, Na, K, Rb, the preparation method of Cs), and the ionic liquid synthesized by this type of salt. Background technique [0002] Perfluoroalkylsulfonylimide (H[R f 1 SO 2 NSO 2 R f 2 ], hereinafter referred to as H[PFSI]; R f 1 , R f 2 =C m f 2m +1, m=1-8) alkali metal salt (M[R f 1 SO 2 NSO 2 R f 2 ], M=Li, Na, K, Rb, Cs; hereinafter referred to as M[PFSI]) is an important class of fluorine-containing organic compounds, which have important application value in the development of high-performance electrolyte materials and new catalysts. [0003] The general structural formula of perfluoroalkylsulfonylimide alkali metal salt is as shown in formula (I): [0004] [0005] Wherein: M+=Li, ...

Claims

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Application Information

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IPC IPC(8): C07C311/02C07C303/36
Inventor 聂进周志彬周宜轩徐冰刘凯郭鹏
Owner 武汉市瑞华新能源科技有限公司
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