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Preparation method of difluoro-sulfonyl imide lithium

A technology of lithium bisfluorosulfonyl imide and bischlorosulfonimide, which is applied in the field of preparation of lithium bisfluorosulfonyl imide, can solve the problem of low purity of lithium bisfluorosulfonyl imide, various types of raw materials and reagents, There are many types and contents of impurities, etc., to achieve good fluorination effect, good economic and environmental benefits, and easy control

Active Publication Date: 2016-07-06
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the above preparation method has produced lithium bisfluorosulfonyl imide, it uses a solvent to dissolve lithium bischlorosulfonyl imide in the fluorination stage, and adds solid fluorinating agent (zinc fluoride) and triethylamine to carry out reflux reaction, There are many types of raw materials and reagents used, the operation is complicated, and the types and contents of impurities produced are many, which are difficult to remove in the follow-up; the solid fluorination itself has many side reactions, and the fluorination effect is poor. Low purity, low yield, can not meet the requirements of use

Method used

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  • Preparation method of difluoro-sulfonyl imide lithium
  • Preparation method of difluoro-sulfonyl imide lithium

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Embodiment 1

[0058] The preparation method of the bisfluorosulfonyl imide lithium of the present embodiment, such as figure 1 shown, including the following steps:

[0059] 1) Preparation of bischlorosulfonimide:

[0060] a) Under nitrogen protection, according to the ratio of 2.0:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) of thionyl chloride and 102g (100%, 100% sulfamic acid was added to the reactor, and after stirring at room temperature, 123g (100%, 100%) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 5h;

[0061] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 1 hour, then open the outlet valve of the reactor, discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed solution A;

[0062] b) After the pressure in the reactor is stable, the liquid in...

Embodiment 2

[0071] The preparation method of the lithium bisfluorosulfonyl imide of the present embodiment (the process flow diagram is the same as that of Example 1), comprises the following steps:

[0072] 1) Preparation of bischlorosulfonimide:

[0073] a) Under nitrogen protection, according to the ratio of 2.5:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) thionyl chloride and 81.5g (100% , 100 percent) sulfamic acid was added to the reactor, and after stirring at room temperature, 98 g (100 percent, 100 percent) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 5 hours;

[0074] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 0.5h, then open the outlet valve of the reactor to discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed liquid A ;

[0075] b)...

Embodiment 6

[0088] The preparation method of the bisfluorosulfonyl imide lithium of the present embodiment, such as figure 2 shown, including the following steps:

[0089] 1) Preparation of bischlorosulfonimide:

[0090] a) Under nitrogen protection, according to the ratio of 2.1:1.0:1.0 in the molar ratio of thionyl chloride, sulfamic acid and chlorosulfonic acid, 250g (100%, folded) thionyl chloride and 97.8g (100% , 100% sulfamic acid was added to the reaction kettle, and after stirring at room temperature, 117.6g (100%, 100% percent) chlorosulfonic acid was added at a constant speed, and the addition time was controlled to be 4h;

[0091] After the addition of chlorosulfonic acid, continue to stir and react at room temperature for 0.5h, then open the outlet valve of the reactor to discharge and recover the unreacted thionyl chloride and protective atmosphere in the reactor; the remaining liquid in the reactor is mixed liquid A ;

[0092] b) After the pressure in the reaction kettl...

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Abstract

The invention discloses a preparation method of difluoro-sulfonyl imide lithium. The preparation method comprises the following steps: 1) under a protective atmosphere, adding a fluorizating agent into difluoro-sulfonyl imide to perform a fluorination reaction so as to obtain a mixture, wherein the fluorizating agent is one of or a combination of fluorine, a fluorine-containing mixed gas, anhydrous hydrogen fluoride, potassium fluoride, antimonic fluoride and rubidium fluoride; 2) performing reduced pressure distillation on the obtained mixture to obtain a di(fluoro-sulfonyl) imide intermediate; and 3) under a protective atmosphere, performing synthetic reaction on the obtained di(fluoro-sulfonyl) imide intermediate and a lithium source, and performing solid-liquid separation to obtain difluoro-sulfonyl imide lithium. According to the preparation method disclosed by the invention, the fluorination reaction does not need a solvent or other auxiliary agent, is less in types of adopted reagents, does not introduce a new impurity, is simple in operation, and is easy to control; the method is less in side reaction, good in fluorination effect and low in fluorination cost; and the purity and the yield of the product namely difluoro-sulfonyl imide lithium obtained by a subsequent synthetic reaction are improved on the whole, and the method has good economic and environmental benefits.

Description

technical field [0001] The invention belongs to the technical field of electrolyte lithium salts for lithium ion batteries, and in particular relates to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] The electrolyte solution is an important part of the lithium-ion battery, which plays the role of transporting ions and conducting current between the positive and negative electrodes, and is an indispensable part to complete the electrochemical reaction. Selecting a suitable electrolyte is also the key to obtaining a lithium-ion battery with high energy density and power density, long cycle life and good safety performance. The performance of the electrolyte directly affects the optimization and improvement of the performance of the lithium-ion battery. At present, the electrolyte of commercial lithium-ion batteries is mainly lithium hexafluorophosphate (LiBF 6 ). Lithium hexafluorophosphate can form a stable SEI film on the carbon nega...

Claims

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Application Information

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IPC IPC(8): C01B21/086H01M10/0568
CPCC01B21/086C01P2006/80H01M10/0568Y02E60/10
Inventor 侯红军薛旭金杨华春薛峰峰刘海霞李云峰王鹏杰司腾飞
Owner DO FLUORIDE CHEM CO LTD
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