IP Library Granted Patent US 11,084,723
Granted Patent B2
US 11,084,723 · App. 16/331,242 · Granted Aug 10, 2021

Method for drying and purifying LiFSI

Inventors: Grégory Schmidt (Saint Andeol le Chateau, FR); Rémy Teissier (Francheville, FR)
Assignee: ARKEMA FRANCE
C01B21/086B01D1/22C01B21/0935H01M10/0525H01M10/0568C01P2006/40H01M2300/0025Y02P20/133
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Quick Facts
Patent No.
US 11,084,723
App. No.
16/331,242
Granted
Aug 10, 2021
Kind
B2
Abstract

The present invention relates to a method for drying and purifying a lithium bis(fluorosulfonyl)imide salt in solution in an organic solvent S1, said method comprising the following steps: a) adding deionised water to dissolve and extract the lithium bis(fluorosulfonyl)imide salt, forming an aqueous solution of said salt; b) extracting the lithium bis(fluorosulfonyl)imide salt from said aqueous solution, using an organic solvent S2, said step being repeated at least once; c) concentrating the lithium bis(fluorosulfonyl)imide salt by evaporating said organic solvent S2 and the water, in a short-path thin-film evaporator, under the following conditions: temperature of 30° C. to 95° C., pressure of 10 −3 mbar abs to 5 mbar abs, residence time no longer than 15 min; and d) optionally crystallising the lithium bis(fluorosulfonyl)imide salt. The present invention likewise relates to a composition made of lithium bis(fluorosulfonyl)imide salt, and the uses thereof in Li-ion batteries.

Claims (34)

1. A composition C comprising:

at least 99.80% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C;

between 5 ppm and 45 ppm by mass of water relative to the total mass of composition C; and

a mass content of sulfate ions of less than or equal to 100 ppm by mass relative to the total mass of composition C.

2. The composition C as claimed in claim 1 , comprising a mass content of sulfate ions of between 2 and 100 ppm by mass relative to the total mass of said composition C.

3. The composition C as claimed in claim 1 , comprising:

a mass content of water of between 5 and 45 ppm by mass relative to the total mass of said composition C;

a mass content of sulfate ions of less than or equal to 100 ppm relative to the total mass of said composition C;

a mass content of Cl − of less than or equal to 50 ppm by mass relative to the total mass of said composition C.

4. The composition C as claimed in claim 1 , wherein the sum of the water content and of the sulfate content is less than or equal to 100 ppm.

5. A Li-ion battery comprising a composition C as claimed in claim 1 .

6. The Li-ion battery as claimed in claim 5 , wherein the Li-ion battery is in a mobile device, an electric vehicle, or a renewable energy generation system.

7. The composition C as claimed in claim 1 , comprising at least 99.85% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C.

8. The composition C as claimed in claim 1 , comprising at least 99.90% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C.

9. The composition C as claimed in claim 1 , comprising at least 99.95% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C.

10. The composition C as claimed in claim 1 , comprising between 5 and 40 ppm by mass of water relative to the total mass of composition C.

11. The composition C as claimed in claim 1 , comprising a mass content of sulfate ions of less than or equal to 90 ppm by mass relative to the total mass of composition C.

12. The composition C as claimed in claim 1 , comprising a mass content of sulfate ions of less than or equal to 50 ppm by mass relative to the total mass of composition C.

13. The composition C as claimed in claim 1 , comprising a mass content of sulfate ions of less than or equal to 10 ppm by mass relative to the total mass of composition C.

14. The composition C as claimed in claim 1 , comprising a mass content of Cl − of less than or equal to 40 ppm by mass relative to the total mass of said composition C.

15. The composition C as claimed in claim 1 , comprising a mass content of Cl − of less than or equal to 25 ppm by mass relative to the total mass of said composition C.

16. The composition C as claimed in claim 1 , wherein the sum of the water content and of the sulfate content is between 5 and 90 ppm.

17. The composition C as claimed in claim 1 , wherein the sum of the water content and of the sulfate content is between 10 and 60 ppm.

18. The composition C as claimed in claim 1 , comprising:

at least 99.90% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C;

between 5 and 40 ppm by mass of water relative to the total mass of composition C;

a mass content of sulfate ions of less than or equal to 50 ppm by mass relative to the total mass of composition C; and

a mass content of Cl − of less than or equal to 45 ppm by mass relative to the total mass of said composition C.

19. The composition C as claimed in claim 18 , wherein the sum of the water content and of the sulfate content is between 10 and 60 ppm.

20. The composition C as claimed in claim 1 , comprising:

at least 99.95% by weight of lithium bis(fluorosulfonyl)imide salt relative to the total weight of said composition C;

between 5 and 40 ppm by mass of water relative to the total mass of composition C;

a mass content of sulfate ions of less than or equal to 10 ppm by mass relative to the total mass of composition C; and

a mass content of Cl − of less than or equal to 25 ppm by mass relative to the total mass of said composition C.

Assignments (2)
CHANGE OF ADDRESS Recorded Jul 4, 2025
From: ARKEMA FRANCE
To: ARKEMA FRANCE
Reel/Frame 071814/0739 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 12, 2019
From: SCHMIDT, GRÉGORY; TEISSIER, RÉMY
To: ARKEMA FRANCE
Reel/Frame 048571/0576 →