Method for preparing imidodisulfuryl fluoride lithium with villiaumite as fluorinating agent

A technology of lithium bisfluorosulfonimide and bischlorosulfonimide is applied in the field of preparation of lithium bisfluorosulfonimide, which can solve the problems of high reaction risk, complicated operation, high toxicity and the like, and achieves reaction conditions Mild, simple follow-up treatment, minimal impact on preparation

Inactive Publication Date: 2018-02-02
JIANGSU LEE & MAN CHEM +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the methods for synthesizing LiFSI mainly include: (1) using SOCl 2 , ClSO 3 H and HSO 2 NH 2 Synthesis of HClSI followed by SbF 3 , AsF 3 , RhF 3 Wait for fluorination to obtain HFSI, then synthesize M-FSI with the corresponding metal salt, and finally pass LiBF 4 , LiClO 4 The method is cumbersome to replace with LiFSI, and the purity of the reaction intermediates in each step will have a great impact on the final product.
And As, Sb, Rh, etc. are highly toxic, if they cannot be removed, they will have a great impact on the performance of LiFSI
(2) Huazhong University of Science and Technology doctoral dissertation (20

Method used

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  • Method for preparing imidodisulfuryl fluoride lithium with villiaumite as fluorinating agent
  • Method for preparing imidodisulfuryl fluoride lithium with villiaumite as fluorinating agent
  • Method for preparing imidodisulfuryl fluoride lithium with villiaumite as fluorinating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of Dichlorosulfonimide (ie HClSI)

[0033] Will NH 2 SO 3 H was added to an anhydrous and oxygen-free reaction flask, and SOCl was added under stirring 2 , when the temperature of the reaction system rises to 80°C, the ClSO 3 H was slowly added dropwise into the reaction bottle, and after the drop, the reaction temperature was raised to 130°C, and the reaction continued for 24 hours until no tail gas was generated. During the process, the color of the reaction solution gradually turned brownish red, and the amount of the reaction solution was very Significant reduction of HN(SO 2 Cl) 2 initial product.

[0034] The obtained product is subjected to vacuum distillation at 82-85° C., and the obtained product is a transparent solution. The properties of the product were detected by NMR and LG-MS. The yield of this reaction was integrated to be about 95%.

[0035] 1 H-NMR (CDCl 3 ): δ8.76

[0036] 19 F-NMR (CDCl 3 ): δ58.12

[0037] Reaction formula: ...

Embodiment 2

[0040] Under nitrogen and deoxygenation conditions, add an appropriate amount of LiF (fluorinating agent) and complexing agent 12-crown-4 (1 to 5% of the amount of LiF) into the reaction bottle, and add an appropriate amount of acetonitrile or carbonic acid after water removal treatment. Diethyl ester dissolves LiF and 12-crown-4. Add 20-100 g of HClSI to the reactor under stirring, continue the reaction at a low temperature of -10-0° C. for 10 h, then end the reaction, and collect the filtrate. The solvent was distilled off under reduced pressure to obtain a light yellow viscous concentrated liquid, which was determined by 19 F-NMR, LG-MS and other spectra. The yield of this reaction was integrated to be about 88%.

[0041] 19 F-NMR (CDCl 3 ): δ51.56

[0042] Reaction formula:

[0043]

Embodiment 3

[0045]Under the condition of nitrogen and oxygen removal, add appropriate amount of LiF (fluorinating agent) and complexing agent 14-crown-4 (1 to 5% of the amount of LiF) into the reaction bottle, and add appropriate amount of acetonitrile or carbonic acid after water removal treatment. Diethyl ester dissolves LiF and 14-crown-4. Add 20-100g of HClSI to the reactor under stirring, continue the reaction at a low temperature of -10-0°C for 10 hours, then end the reaction, and collect the filtrate. The solvent was distilled off under reduced pressure to obtain a light yellow viscous concentrated solution, which was determined for 19 F-NMR, LG-MS and other spectra. The yield of this reaction was integrated to be about 80%.

[0046] 19 F-NMR (CDCl 3 ): δ51.53

[0047] Reaction formula:

[0048]

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Abstract

The invention provides a method for preparing imidodisulfuryl fluoride lithium with villiaumite as a fluorinating agent. The method comprises the following specific step: by taking imidodisulfuryl fluoride as a raw material, and a fluorinating agent as a complexing agent, performing a reaction in a polar organic solvent, thereby obtaining the imidodisulfuryl fluoride lithium, wherein the fluorinating agent comprises lithium fluoride or zinc fluoride; the fluorinating agent is 2-4 times of the weight parts of the imidodisulfuryl fluoride; the complexing agent comprises a lithium ion complexingagent or a zinc ion complexing agent; the complexing agent accounts for 0.5-5% of the weight parts of the fluorinating agent; and the polar organic solvent is selected from one or more of saturated carbonic esters, fluoro saturated carbonic esters, acetonitrile or N,N-dimethyl formamide. The imidodisulfuryl fluoride lithium prepared by using the method is low in toxin of reagents used in reactions, gentle in reaction condition, free of extreme condition such as high temperature and high pressure, low in equipment requirement and easy to achieve; in addition, the method provided by the invention is small in middle reaction, simple in later treatment, small in whole product preparation influence and very high in reaction yield, that is, up to 70-88%.

Description

technical field [0001] The invention relates to the technical field of bisfluorosulfonimide lithium electrolyte, in particular to a preparation method of bisfluorosulfonyl imide lithium using fluorine salt as a fluorinating agent. Background technique [0002] The high-nickelization of ternary power high-energy-density lithium-ion secondary batteries plays a decisive role in the rapid development of new energy vehicles and other power battery demand markets. However, the performance requirements of electrolytes are getting higher and higher, and high voltage and high Energy density, safety and other characteristics. [0003] The traditional lithium hexafluorophosphate electrolyte, which is easy to decompose at high temperature, limits its application in the field of high-voltage lithium-ion batteries. Lithium bisfluorosulfonyl imide (LiFSI) is favored by the market because it can improve the cycle and is suitable for both high and low temperatures. However, its synthesis pr...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086
Inventor 陈胜洲蒋家巧谢文健辛伟贤陈新滋
Owner JIANGSU LEE & MAN CHEM
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