IP Library Granted Patent US 11,486,045
Granted Patent B1
US 11,486,045 · App. 16/929,281 · Granted Nov 1, 2022

Low temperature lithium production

Inventor: John W. Freiderich (Oak Ridge, TN)
Assignee: CONSOLIDATED NUCLEAR SECURITY, LLC
C25C1/02C25C7/00
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Quick Facts
Patent No.
US 11,486,045
App. No.
16/929,281
Granted
Nov 1, 2022
Kind
B1
Abstract

A method and electrolysis cell for producing lithium metal at a low temperature. The method includes combining (i) acetonitrile and (ii) a cation bis(trihaloalkylsulfonyl)imide, cation bis(trihalosulfonyl)imidic acid, a cation bis(trihaloalkylsulfonyl)amide, or cation bis(trihaloalkylsulfonyl)amidic acid in a weight ratio of (i) to (ii) about 100:1 to about 5:1 to provide a non-aqueous electrolyte composition. A lithium compound selected from the group consisting of LiOH, Li 2 O and Li 2 CO 3 is dissolved in the electrolyte composition to provide a lithium doped electrolyte composition. Power is applied to the electrolyte composition to form lithium metal on a cathode of an electrolysis cell. The lithium metal separated from the cathode has a purity of at least about 95 wt. %.

Claims (35)

1. A method of producing lithium metal in an electrolysis cell, the method comprising the steps of:

combining (i) acetonitrile and (ii) a cation bis(trihaloalkylsulfonyl)imide, a cation bis(trihalo-sulfonyl)imidic acid, a cation bis(trihaloalkylsulfonyl)amide, or a cation bis(trihaloalkylsulfonyl)amidic acid to provide a non-aqueous electrolyte composition,

dissolving a lithium compound selected from the group consisting of LiOH, Li 2 and Li 2 CO 3 in the non-aqueous electrolyte composition to provide a doped lithium electrolyte composition,

applying power to the electrolysis cell to form lithium metal on a cathode of an electrolysis cell, and

separating lithium metal from the cathode.

2. The method of claim 1 , wherein the doped lithium electrolyte composition further comprises a zwitterion or internal salt compound.

3. The method of claim 2 , wherein the zwitterion comprises a (carboxyalkyl)trialkyl ammonium compound.

4. The method of claim 1 , wherein the weight ratio of (i) to (ii) of the non-aqueous electrolyte composition is about 60:1 to 5:1.

5. The method of claim 4 , wherein a weight ratio of non-aqueous electrolyte composition to lithium compound ranges from about 5:1 to about 2:3.

6. The method of claim 5 , wherein a weight ratio of non-aqueous electrolyte composition to lithium compound ranges from about 3:1 to about 3:4.

7. The method of claim 1 , wherein the doped lithium electrolyte composition is at a temperature ranging from about 0° to less than about 180° C.

8. The method of claim 1 , wherein the doped lithium electrolyte composition is at a temperature ranging from about 0° to less than about 100° C.

9. The method of claim 1 , wherein the doped lithium electrolyte composition is at a temperature ranging from about 15° to less than about 81° C.

10. The method of claim 1 , wherein the electrolysis cell contains a cover gas above the doped lithium electrolyte composition.

11. The method of claim 1 , wherein the electrolysis cell comprises an anode compartment, a cathode compartment and a separator between the anode compartment and the cathode compartment.

12. The method of claim 11 , wherein the separator is selected from the group consisting of a fritted glass separator, a microporous membrane, and a salt bridge.

13. The method of claim 1 , wherein the cation is selected from the group consisting of a phosphonium ion, a sulfonium ion, an ammonium ion, an imidazolium ion, a piperidinium ion, a pyridinium ion and a pyrrolidinium ion.

14. The method of claim 1 , wherein the cation is selected from the group consisting of an alkali metal, an alkaline earth metal, a metalloid, a transition metal, and a lanthanide.

15. The method of claim 1 , wherein the halo ion is a fluoride ion.

16. The method of claim 1 , wherein the alkyl group is a methyl group.

17. The method of claim 1 , wherein power is applied to the anode and cathode at a current density ranging from about 0.1 mA/cm 2 to about 2.5 mA/cm 2 .

18. An electrolysis cell for producing lithium metal at a temperature comprising:

a cathode compartment comprising a cathode,

an anode compartment comprising an anode,

a separator between the anode compartment and the cathode compartment,

a non-aqueous electrolyte composition in the anode and cathode compartments comprising (i) acetonitrile and (ii) a cation bis(trihaloalkylsulfonyl)imide, a cation bis(trihalosulfonyl)imidic acid, a cation bis(trihaloalkylsulfonyl)amide, or a cation bis(trihaloalkylsulfonyl)amidic acid, wherein the electrolyte composition further comprises a lithium compound selected from the group consisting of LiOH, Li 2 O and Li 2 CO 3 dissolved in the electrolyte composition, and wherein the separator is selected from the group consisting of a fritted glass separator, a microporous membrane, and a salt bridge,

whereby power applied to the anode and cathode forms lithium metal on the cathode of the electrolysis cell with a lithium metal purity of greater than 95 wt. %.

19. The electrolysis cell of claim 18 , wherein a weight ratio of non-aqueous electrolyte composition to lithium compound ranges from about 5:1 to about 2:3.

20. The electrolysis cell of claim 18 , wherein the electrolyte composition further comprises a (carboxyalkyl)trialkyl ammonium compound.

21. The electrolysis cell of claim 18 , wherein the cation is selected from the group consisting of a phosphonium ion, a sulfonium ion, an ammonium ion, an imidazolium ion, a piperidinium ion, a pyridinium ion, and a pyrrolidinium ion.

22. The electrolysis cell of claim 18 , wherein the cation is selected from the group consisting of an alkali metal, an alkaline earth metal, a metalloid, a transition metal, and a lanthanide.

23. The electrolysis cell of claim 18 , wherein the halo ion is a fluoride ion.

24. The electrolysis cell of claim 18 , wherein the alkyl group is a methyl group.

25. The electrolysis cell of claim 18 , wherein the electrolysis cell temperature is below about 180° C.

26. The method of claim 1 , wherein the lithium metal on the cathode has a purity of at least about 97 wt. %.

Assignments (2)
CONFIRMATORY LICENSE Recorded Aug 10, 2020
From: CONSOLIDATED NUCELAR SECURITY, LLC
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 053442/0979 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 15, 2020
From: FREIDERICH, JOHN W
To: CONSOLIDATED NUCLEAR SECURITY, LLC
Reel/Frame 053213/0239 →