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Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude products, and uses of purified products

A kind of technology of fluorosulfonyl and imide, applied in the field of purifying crude HFSI

Pending Publication Date: 2020-09-08
SES HLDG PTE LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the impurities in the basic crude HFSI such as HF, FSO 3 H, HCl and H 2 SO 4 Resulting impurities in LiFSI salt products such as LiF, FSO 3 Li, LiCl, and Li 2 SO 4 can have undesired effects on the operation and life of lithium-ion batteries if their levels do not fall below a certain upper limit

Method used

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  • Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude products, and uses of purified products
  • Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude products, and uses of purified products
  • Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude products, and uses of purified products

Examples

Experimental program
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Effect test

Embodiment 1

[0046] In a 500 mL dry filter funnel, crude HFSI (200 g) with various levels of target impurities, here, FSO 3 H=1000ppm, HCl=200ppm, HF=500ppm, and H 2 SO 4 = 500 ppm, dissolved in 50 g of anhydrous dichloromethane under a dry nitrogen atmosphere, giving a solvent content of 20% by weight for the solution. The filter funnel was closed with a stopper and stored at 0°C for 4 hours. Crystal formation of HFSI product. The HFSI product was filtered under dry nitrogen atmosphere and washed with 25 mL of cold dichloromethane to give colorless crystals in 95% yield. The resulting washed crystallized HFSI product contains the following impurities: FSO 3 H=550ppm; HCl=100ppm; HF=80ppm; and H 2 SO 4 = 500ppm.

Embodiment 2

[0048] In a 500 mL dry filter funnel, crude HFSI (200 g) with various levels of target impurities, here, FSO 3 H=1000ppm, HCl=200ppm, HF=500ppm, and H 2 SO 4 = 500 ppm, dissolved in 75 g of anhydrous dichloromethane under a dry nitrogen atmosphere, giving a solvent content of 27% by weight for the solution. The filter funnel was closed with a stopper and stored at 0°C for 4 hours. Crystal formation of HFSI product. The HFSI product was filtered under dry nitrogen atmosphere and washed with 25 mL of cold dichloromethane to give colorless crystals in 90% yield. The resulting washed crystallized HFSI product contains the following impurities: FSO 3 H=300ppm; HCl=80ppm; HF=60ppm; and H 2 SO 4 = 400ppm.

Embodiment 3

[0050] In a 500 mL dry filter funnel, crude HFSI (200 g) with various levels of target impurities, here, FSO 3 H=1000ppm, HCl=200ppm, HF=500ppm, and H 2 SO 4 = 500 ppm, dissolved in 100 g of anhydrous dichloromethane under a dry nitrogen atmosphere, giving a solvent content of 33% by weight for the solution. The filter funnel was closed with a stopper and stored at 0°C for 4 hours. Crystal formation of HFSI product. The HFSI product was filtered under dry nitrogen atmosphere and washed with 25 mL of cold dichloromethane to give colorless crystals in 85% yield. The resulting washed crystallized HFSI product contains the following impurities: FSO 3 H=215ppm; HCl=50ppm; HF=40ppm; and H 2 SO 4 = 280ppm.

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Abstract

Purified hydrogen bis(fluorosulfonyl)imide (HFSI) products, methods of purifying crude products, and uses of purified products are provided. A method of removing one or more target impurities from crude hydrogen bis(fluorosulfonyl)imide (HFSI) using a crystallization technique is disclosed. In some embodiments, the method includes contacting the crude HFSI with at least one anhydrous solvent to create a solution. The solution is caused to have a temperature sufficient to cause HFSI in the solution to crystallize while the one or more impurities remain dissolved in the mother liquor of the solution. The crystallized HFSI and the mother liquor containing the one or more impurities are separated to obtain a purified HFSI product. Purified HFSI products are also disclosed, as are systems, suchas secondary batteries, incorporating purified HFSI products.

Description

[0001] Related application information [0002] This application claims U.S. Provisional Patent Application No. 62 / 812,371, filed March 1, 2019, entitled "PROCESS FOR PURIFICATION OF HYDROGEN BIS (FLUOROSULFONYL) IMIDE (HFSI)" and filed April 12, 2019, entitled The benefit of priority of US Provisional Patent Application No. 62 / 832,968 for "PROCESS FOR PURIFICATION OF HYDROGEN BIS (FLUOROSULFONYL) IMIDE (HFSI)," each of which is incorporated herein by reference in its entirety. technical field [0003] The present invention relates generally to the field of hydrogen bis(fluorosulfonyl)imides (HFSI). In particular, the invention relates to a purified HFSI product, a method of purifying crude HFSI and the use of the purified HFSI product. Background technique [0004] Hydrogen bis(fluorosulfonyl)imide (HFSI) can be used in the synthesis of any of a variety of compounds, including alkali metal bis(fluorosulfonyl)imide (FSI) salts such as lithium FSI (LiFSI), Sodium FSI (NaFS...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/093H01M10/052H01M10/0525H01M10/0568H01G11/56H01G11/84
CPCC01B21/093H01M10/0568H01M10/052H01M10/0525H01G11/56H01G11/84H01M2300/0025C01B21/088Y02E60/50Y02E60/10H01M10/058H01M8/103C08L2203/20C08L79/08H01M10/0565
Inventor R·P·辛格胡启朝
Owner SES HLDG PTE LTD