Granted Patent B2

US 12,187,609 · App. 17/585,990 · Granted Jan 7, 2025

Inventors: Matthew H. Luly (Hamburg, NY); Bernard E. Pointner (Buffalo, NY)

Assignee: Honeywell International Inc.

C01B21/093

Abstract

Claims (26)

1. A method of producing purified bis(fluorosulfonyl) imide, the method comprising:

reacting urea with fluorosulfonic acid to form a first liquid mixture comprising bis(fluorosulfonyl) imide and unreacted fluorosulfonic acid;

contacting the first liquid mixture with gaseous ammonia, wherein the gaseous ammonia reacts with the fluorosulfonic acid to produce a second liquid mixture comprising ammonium fluorosulfate; and

separating the ammonium fluorosulfate from the second liquid mixture.

2. The method of claim 1 , wherein after the reacting step, a concentration of the fluorosulfonic acid in the first liquid mixture is from about 0.001 mol % to about 70 mol %.

3. The method of claim 1 , wherein contacting the first liquid mixture with gaseous ammonia includes introducing the gaseous ammonia into a headspace of a vessel containing the first liquid mixture.

4. The method of claim 3 , wherein the gaseous ammonia is supplied at a pressure between about 100 kPa and about 200 kPa.

5. The method of claim 1 , wherein contacting the first liquid mixture with gaseous ammonia includes bubbling the gaseous ammonia into the first liquid mixture.

6. The method of claim 1 , wherein contacting the first liquid mixture with gaseous ammonia includes flowing the gaseous ammonia and the first liquid mixture in a counterflow column.

7. The method of claim 1 , wherein separating the the ammonium fluorosulfate from the second liquid mixture includes filtering the ammonium fluorosulfate from the second liquid mixture.

8. The method of claim 1 , wherein separating the ammonium fluorosulfate from the second liquid mixture includes flash distilling the bis(fluorosulfonyl) imide from the ammonium fluorosulfate.

9. The method of claim 1 , wherein a concentration of the bis(fluorosulfonyl) imide in a remaining second liquid mixture obtained after separating the ammonium fluorosulfate from the second liquid mixture is from about 90 mol % to about 99.95 mol %.

10. The method of claim 1 , further comprising:

providing a remaining second liquid mixture obtained after separating the ammonium fluorosulfate from the second liquid mixture, the remaining second liquid mixture including the bis(fluorosulfonyl) imide and residual fluorosulfonic acid;

contacting the remaining second liquid mixture with gaseous ammonia, wherein the gaseous ammonia reacts with the residual fluorosulfonic acid in the remaining second liquid mixture to produce a third liquid mixture comprising additional ammonium fluorosulfate; and

separating the additional ammonium fluorosulfate from the third liquid mixture.

11. The method of claim 10 , wherein in the providing step, the concentration of the residual fluorosulfonic acid in the remaining second liquid mixture is from about 0.1 mol % to about 20 mol %.

12. The method of claim 10 , wherein contacting the remaining second liquid mixture with gaseous ammonia includes introducing the gaseous ammonia into a headspace of a vessel containing the remaining second liquid mixture.

13. The method of claim 12 , wherein the gaseous ammonia is supplied at a pressure between about 100 kPa and about 200 kPa.

14. The method of claim 10 , wherein contacting the remaining second liquid mixture with gaseous ammonia includes bubbling the gaseous ammonia into the remaining second liquid mixture.

15. The method of claim 10 , wherein contacting the remaining second liquid mixture with gaseous ammonia includes flowing the gaseous ammonia and the remaining second liquid mixture in a counterflow column.

16. The method of claim 10 , wherein separating the additional ammonium fluorosulfate from the third liquid mixture includes filtering the ammonium fluorosulfate from the third liquid mixture.

17. The method of claim 10 , wherein separating the additional ammonium fluorosulfate from the third liquid mixture includes flash distilling the bis(fluorosulfonyl) imide from the ammonium fluorosulfate.

18. The method of claim 10 , wherein the bis(fluorosulfonyl) imide concentration in a remaining third liquid mixture obtained after separating the additional ammonium fluorosulfate from the third liquid mixture is from about 98 mol % to about 99.95 mol %.

19. The method of claim 1 , further including distilling the remaining second liquid mixture including the bis(fluorosulfonyl) imide and the residual fluorosulfonic acid before the providing step.

20. The method of claim 19 , wherein in the providing step, a concentration of the fluorosulfonic acid in the remaining second liquid mixture is from about 1 mol % to about 20 mol %.

Assignments (2)

Continuity (3)

References Cited (202)