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Synthetic method of lithium bis(fluorosulfonyl)imide

A technology of lithium bisfluorosulfonyl imide and bischlorosulfonyl imide, which is applied in the field of synthesis of lithium bisfluorosulfonyl imide, can solve problems such as the difficulty of desolvation and drying, and achieve cheap and easy-to-obtain reagents and rapid reaction And thoroughly, avoid the effect of decomposition

Active Publication Date: 2017-01-04
RONGCHENG QINGMU CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

HFSI reacts with lithium carbonate in a water environment, the reaction is exothermic, and the product is easily decomposed in an aqueous solution, and the introduction of water makes desolvation and drying difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of lithium bisfluorosulfonyl imide, comprising the following steps:

[0027] 1) In a nitrogen atmosphere, take 214g (1mol) of dichlorosulfonimide and 428g of ethyl acetate, mix them thoroughly and put them into a 1000ml four-necked flask filled with nitrogen and equipped with a condenser, stirring, and tail gas absorption. The purity of ethyl acetate is 99.9%, and the water content is 30ppm. Subsequently, 27.3g (1.05mol) lithium fluoride and 24g (1.2mol) liquid hydrogen fluoride were added to the four-necked flask in turn, and the temperature was raised to 40°C for 10 hours. The reaction formula is as follows: HN(SO2Cl)2+LiF+HF→LiN( SO2F)2+2HCl, the purity of the reactant dichlorosulfonimide, lithium fluoride, and hydrogen fluoride used in this embodiment is all greater than 99%.

[0028] 2) Reduce the temperature of the reaction system to 20°C, replace with nitrogen under reduced pressure to completely remove the residual hydrogen fluoride gas, an...

Embodiment 2

[0032] A preparation method of lithium bisfluorosulfonyl imide, comprising the following steps:

[0033] 1) In a nitrogen atmosphere, take 214g (1mol) of dichlorosulfonimide and 428g of acetonitrile, mix them thoroughly and put them into a 1000ml four-necked flask filled with nitrogen and equipped with a condenser, stirring, and tail gas absorption. The purity is 99.9%, and the water content is 40ppm. Then add 27.3g (1.05mol) lithium fluoride and 24g (1.2mol) liquid hydrogen fluoride to the four-necked flask successively, and raise the temperature to 40°C for 10 hours. The reaction formula is as follows: HN(SO2Cl) 2+LiF+HF→LiN(SO2F)2+2HCl, the purity of the reactant bischlorosulfonimide, lithium fluoride, and hydrogen fluoride used in this example is greater than 99%.

[0034] 2) Reduce the temperature of the reaction system to 20°C, replace with nitrogen under reduced pressure to completely remove the residual hydrogen fluoride gas, and filter the reaction liquid remaining in...

Embodiment 3

[0038] A preparation method of lithium bisfluorosulfonyl imide, comprising the following steps:

[0039] 1) In a nitrogen atmosphere, take 214g (1mol) of dichlorosulfonimide and 642g of ethyl acetate, mix them thoroughly and put them into a 1000ml four-necked flask filled with nitrogen and equipped with a condenser, stirring, and tail gas absorption. The purity of ethyl acetate is 99.9%, and the water content is 30ppm. Then, 28.6g (1.1mol) of lithium fluoride and 24g (1.2mol) of liquid hydrogen fluoride are successively added to the four-necked flask, and the temperature is raised to 40°C for 10 hours. The reaction formula is as follows: HN(SO2Cl)2+LiF+HF→LiN(SO2F)2+2HCl, the purity of the reactant bischlorosulfonimide, lithium fluoride and hydrogen fluoride used in this embodiment is greater than 99%.

[0040] 2) Reduce the temperature of the reaction system to 20°C, replace with nitrogen under reduced pressure to completely remove the residual hydrogen fluoride gas, and filt...

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Abstract

The invention provides a method for synthesizing lithium bis(fluorosulfonyl)imide. The synthetic method of the lithium bis(fluorosulfonyl)imide is characterized by comprising the following steps: (1) in a nitrogen atmosphere, sufficiently mixing bis(fluorosulfonyl)imide and an organic solvent, and putting a mixture into a reactor with a condenser; sequentially adding lithium fluoride and liquid-state hydrogen fluoride into the reactor and raising the temperature to react; (2) reducing the temperature of a reaction system, and decompressing and displacing by nitrogen to completely remove residual hydrogen fluoride gas, and filtering a reaction solution under the nitrogen atmosphere to remove insoluble matters, so as to obtain filtrate; (3) concentrating the filtrate by utilizing a high-vacuum decompression and desolvation method; (4) cooling a concentrated solution and adding a low-polarity solvent; recrystallizing at low temperature, and filtering and carrying out decompression and drying treatment at 40 DEG C to obtain the pure lithium bis(fluorosulfonyl)imide. The synthetic method has the advantages that used reagents are cheap and easy to obtain, a preparation process is simple, a reaction is rapid and complete, a few of byproducts are produced and are easy to remove, a post-treatment manner is simple and convenient, a product has high purity and the synthetic method is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a synthesis method of lithium bisfluorosulfonyl imide. Background technique [0002] Lithium bisfluorosulfonyl imide has the advantages of high stability, excellent low temperature performance, good hydrolytic stability and more environmental friendliness. It can be used as an excellent secondary lithium battery electrolyte, and because of its excellent conductivity, it can be used in supercapacitors and Aluminum electrolytic capacitors, etc.; it can also be used as a Lewis acid catalyst and has important industrial production value. [0003] In the prior art, the preparation of bis(fluorosulfonyl)imide lithium mainly has the following reports: [0004] China CN101747242 has reported the preparation method of bis(fluorosulfonyl)imide lithium, under the protection of nitrogen, sulfamic acid, thionyl chloride, chlorosulfonic acid are reacted to generate bis(chlorosulf...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/34C01P2006/80C01P2006/82
Inventor 孙燕超李维平孙朋波
Owner RONGCHENG QINGMU CHEM MATERIALS
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