Preparation method of lithium bis(fluorosulfonyl)imide

A technology of bisfluorosulfonimide lithium salt and bisfluorosulfonimide, which is applied in the field of preparation of bisfluorosulfonimide lithium salt, can solve the problems of low product purity and yield, complex industrial operations, raw material consumption and Waste generation and other issues, to achieve the effect of reasonable production cost, simple operation steps and stable product quality

Active Publication Date: 2016-12-21
SHANGHAI CHEMSPEC CORP
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Problems solved by technology

The problem that the method that this patent reports exists is that product purity and yield are too low, raw material consumption and waste generation are too much, and manufacturing cost is too high
The problems in the method reported by this patent are also that the product purity and yield are too low, the raw material consumption and waste generation are too much, and the manufacturing cost is too high
[0008] The above production process of LiFSI has higher requirements on reaction equipment, more raw material consumption and waste, complicated industrial operation, and some safety problems; and the product yield is low, and the water, potassium ion, sodium ion, calcium ion, chlorine Impurities such as ions and sulfate ions cannot be effectively controlled, resulting in poor product quality, which makes LiFSI difficult to meet the quality requirements and is not suitable for industrial applications

Method used

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  • Preparation method of lithium bis(fluorosulfonyl)imide

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[0036] One aspect of the present invention provides a method for preparing lithium salt of bisfluorosulfonimide. The method for preparing lithium salt of bisfluorosulfonimide may include: performing a displacement reaction between bisfluorosulfonimide and LiX, wherein, X is selected from Cl, Br or I.

[0037] In the above reaction process, the amount of bisfluorosulfonimide used can be excessive relative to LiX, for example, the molar ratio of LiX to bisfluorosulfonimide can be 0.9-1:1, and can also be 0.95-1:1.

[0038]During the above reaction process, the reaction temperature can be normal temperature, for example, the reaction temperature can be 0-50°C, 10-40°C, or 25-40°C. The method for changing the temperature of the reaction system is not particularly limited, as long as it does not limit the purpose of the present invention, for example, the temperature of the reaction system can be controlled by using a water bath or the like. Those skilled in the art can adjust the...

Embodiment 1

[0060] Into a 1000mL reaction flask, add 300g of dimethyl carbonate and 20.8g of lithium chloride, cool down to 15-25°C, and add 90g of HFSI dropwise under stirring. After stirring for 18 hours, a dimethyl carbonate solution containing 0.1 g of hydrogen fluoride was added dropwise. After stirring and reacting, the mixture was filtered, and the filtrate was precipitated under reduced pressure to obtain a viscous concentrate. 400 g of dichloromethane was added to the concentrate, and the product was precipitated. After filtering and drying, 90.6 g of the product was obtained, with a yield of 98%. Test result: AAS: Na + (7ppm), K + (5ppm), Fe + + - (5ppm), SO4 2- (21ppm). The product is a white powdery solid with a melting point of 124-128°C.

Embodiment 2

[0062]Into a 500mL reaction flask, add 150g of propyl ether and 20.1g of LiCl, control the temperature to 25-30°C, and add 90g of HFSI dropwise under stirring. After stirring for 20 hours, a propyl ether solution containing 0.15 g of hydrogen fluoride was added dropwise, stirred for reaction, filtered, and the filtrate was precipitated under reduced pressure to obtain a viscous concentrate. 200g of dichloroethane was added to the concentrate, the product was precipitated, and 87g of the product was obtained after filtration and drying. (Test result: AAS (ppm): Na + (4ppm), K + (4ppm), Fe + + - (7ppm), SO4 2- (23ppm)).

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Abstract

The invention relates to the field of chemical synthesis, and concretely relates to a preparation method of lithium bis(fluorosulfonyl)imide. The preparation method of lithium bis(fluorosulfonyl)imide comprises the following steps: 1, carrying out a displacement reaction on bis(fluorosulfonyl)imide and LiX, wherein X is selected from Cl, Br and I; 2, mixing a proper amount of hydrogen chloride with a reaction solution obtained through the displacement reaction; and 3, carrying out solid-liquid separation on a reaction solution obtained in step 2, concentrating the obtained liquid phase, adding a poor solvent to crystallize, and carrying out solid-liquid separation to obtain the bis(fluorosulfonyl)imide. The preparation method of bis(fluorosulfonyl)imide allows highly pure LiFSI to be obtained, and has the advantages of realization of stable quality and high yield of the above product, effective reduction of the content of potassium ions, sodium ions, chloride ions, sulfate radicals, water and other impurities, simple operating steps, reasonable production cost, high safety, and suitableness for industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonyl imide, referred to as LiFSI, is a key high-performance electrolyte material in new energy devices such as lithium-ion batteries and supercapacitors, and has high industrial application value. However, the product is easy to absorb water and decompose by heat, and moisture and impurities have adverse effects on its performance. In order to meet the requirements for the use of electrolytes, LiFSI has strict restrictions on indicators such as moisture and various impurity ions. However, there is currently no effective product purification method. Once impurities are introduced, it is difficult to meet the indicator requirements through purification. [0003] Patents US2013331609, US2012041233, etc. have reported the synthesis method of LiFSI, all of which are to prepare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 何立袁云龙杨东杨建华赵姗姗
Owner SHANGHAI CHEMSPEC CORP
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