Purification method of bis(fluorosulfonyl)imide

A technology of bisfluorosulfonimide and purification method, which is applied in the directions of nitrosyl chloride, nitrogen and non-metallic compounds, etc., can solve the problems of loss of bisfluorosulfonimide products, difficult to remove, etc., to solve the problem of sublimation residue, improve quality effect

Pending Publication Date: 2022-01-11
深圳鑫宸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

However, it will inevitably cause the loss of more than 15-30% of the bisfluorosulfonimide product, and some soluble impurities, such as sulfamic acid and fluorine ions, are still entrained in the crystal and are difficult to remove

Method used

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  • Purification method of bis(fluorosulfonyl)imide
  • Purification method of bis(fluorosulfonyl)imide
  • Purification method of bis(fluorosulfonyl)imide

Examples

Experimental program
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Effect test

Embodiment 1

[0030] The purification method of bisfluorosulfonimide, the steps are as follows:

[0031] by SbF 3 The bisfluorosulfonimide crude product prepared by fluorination is 300g, and its chloride content is 1361ppm, and the ion chromatogram is shown in figure 1 ,Depend on figure 1 It can be seen that SbF 3 The HFSI crude product ion chromatogram obtained by fluorination has obvious chloride ion characteristic peak (retention time 4.087), and its chloride ion content is 1361ppm after conversion of the standard curve.

[0032] Under the protection of dry nitrogen, the above crude bisfluorosulfonimide (HFSI) was added into a 1L three-necked flask, and 1.68 g of sulfamic acid was added at the same time. Connect the reflux condenser and the bubbler, heat the device to 60°C with an oil bath, and stir the reaction, during which acid gas will be generated in the bubbler. After 10 hours of reaction, no gas was generated, and the heating was stopped, and the temperature of the contents in...

Embodiment 2

[0034] by SbF 3 The crude product of bisfluorosulfonimide prepared by fluorination was 300g, and its chloride content was 1361ppm. Under the protection of dry nitrogen, the above crude bisfluorosulfonimide (HFSI) was added into a 1L three-necked flask, and 3.45 g of tartaric acid was added at the same time. Connect the reflux condenser and the bubbler, heat the device to 80°C with an oil bath, and stir the reaction, during which acid gas will be generated in the bubbler. After 6 hours of reaction, no gas was generated, and the heating was stopped, and the temperature of the contents in the flask was lowered to below 30°C. Replace the reflux device with a vacuum distillation device, 100Pa, vacuum distillation / rectification at 40-80°C to obtain 281.4g of HFSI with a yield of 93.8%. A light brown solid remained in the flask. The refined HFSI is detected according to HJ / T 343-2007 "Determination of Chloride in Water Quality by Mercury Nitrate Titration (Trial)" method, wherein ...

Embodiment 3

[0036] by BiF 3The crude product of bisfluorosulfonimide prepared by fluorination was 300g, and its chloride content was 738ppm. Under the protection of dry nitrogen, the above crude bisfluorosulfonimide (HFSI) was added into a 1L three-necked flask, and 4.78g of potassium citrate was added at the same time. Connect the reflux condenser and the bubbler, heat the device to 80°C with an oil bath, stir the reaction, no gas generation is observed in the bubbler. After 12 hours of reaction, the heating was stopped, and the temperature of the contents in the flask was lowered to below 30°C. The reflux device was replaced by a vacuum distillation device, 100 Pa, and vacuum distillation / rectification at 40-80 ° C to obtain HFSI291.2g, with a yield of 97.1%. An off-white solid remained in the flask. The refined HFSI is tested according to the method of HJ / T 343-2007 "Determination of Chloride in Water Quality by Mercury Nitrate Titration (Trial)", wherein the chloride content is 4pp...

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Abstract

The invention provides a purification method of bis(fluorosulfonyl)imide. The purification method comprises the following steps: (1) under the protection of inert gas, adding a certain amount of acid or salt into a crude bis(fluorosulfonyl)imide product, and carrying out heating for a react while stirring; and (2) carrying out reduced-pressure distillation / rectification to obtain the bis(fluorosulfonyl)imide with low chloride content. According to the invention, chloride in the bis(fluorosulfonyl)imide can be reduced to 10 ppm or below through one-time distillation or rectification, so the problem of sublimation residues of the chloride in the prior art is solved, and the quality of the bis(fluorosulfonyl)imide is improved.

Description

technical field [0001] The invention belongs to the field of fluorine chemical synthesis, and in particular relates to a method for purifying bisfluorosulfonimide. Background technique [0002] Bisfluorosulfonimide HN(SO 2 f) 2 (referred to as HFSI) due to its large anion size and highly delocalized charge, it is a typical "weakly coordinated" anion and has weak electrostatic interaction with cations. Therefore, its alkali metal salts have many distinctive and excellent properties in the field of electrochemistry. For example, LiFSI has higher ionic conductivity than lithium hexafluorophosphate, excellent thermal stability and hydrolysis resistance in lithium ion battery electrolytes, and can effectively improve the high and low temperature performance and cycle life of lithium ion batteries. It is considered to be the next generation of new lithium salts. [0003] Currently commonly used is the fluorination of bischlorosulfonimide (HCSI) in anhydrous hydrogen fluoride me...

Claims

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Application Information

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IPC IPC(8): C01B21/086
CPCC01B21/086C01P2006/80
Inventor 王驰伟
Owner 深圳鑫宸新能源科技有限公司
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