IP Library Granted Patent US 11,634,336
Granted Patent B2
US 11,634,336 · App. 17/588,009 · Granted Apr 25, 2023

Processes for preparing lithium carbonate

Inventors: Guy Bourassa (Québec, CA); Gary Pearse (Ottawa, CA); Stephen Charles Mackie (Peterborough, CA); Mykolas Gladkovas (Toronto, CA)
Assignee: NEMASKA LITHIUM INC.
C01D15/08C25B1/16C25B15/08
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Quick Facts
Patent No.
US 11,634,336
App. No.
17/588,009
Granted
Apr 25, 2023
Kind
B2
Abstract

There are provided methods for preparing lithium carbonate. For example, such methods can comprise reacting an aqueous composition comprising lithium hydroxide with CO 2 by sparging the CO 2 the said composition, thereby obtaining a precipitate comprising the lithium carbonate. The methods can also comprise inserting at least a portion of the precipitate into a clarifier and obtaining a supernatant comprising lithium bicarbonate and a solid comprising the lithium carbonate, separating the solid from the supernatant; and heating the supernatant at a desired temperature so as to at least partially convert the lithium bicarbonate into lithium carbonate.

Claims (42)

1. A system for preparing lithium sulphate, the system comprising:

a first reactor,

the first reactor comprising at least one inlet for receiving an acid roasted lithium-containing material, and at least one second inlet for receiving water, wherein the lithium-containing material is a material that has been previously reacted with H 2 SO 4 , and

the first reactor configured to contain a first slurry, the first slurry comprising a solid and an aqueous composition comprising Li + and at least one metal ion;

a second reactor,

the second reactor being in in fluid communication with the first reactor, and configured to receive at least a portion of the first slurry or at least a portion of the aqueous composition comprising Li + and at least one metal ion and to contain a second slurry, the second slurry comprising a first precipitate comprising at least one hydroxide of the at least one metal ion and an aqueous composition comprising Li + and having a reduced amount of the at least one metal ion,

the second reactor comprising at least one inlet for receiving a base, and being fitted with a first pH probe, a first oxidation reduction potential (ORP) probe, and a sparger in fluid communication with the second reactor,

the sparger being configured to sparge a gas into the second reactor,

the first pH probe being configured to at least substantially maintain pH in the second reactor at about 4.5 to about 6.5, and

the first ORP probe being configured to at least substantially maintain ORP at about or above 350 mV;

a first filter,

the first filter being in fluid communication with the second reactor to receive at least a portion of the second slurry and being configured to separate the first precipitate from the aqueous composition comprising Li + and having a reduced amount of the at least one metal ion;

a third reactor,

the third reactor being in fluid communication with the first filter to receive at least a portion of the aqueous composition comprising Li + and having a reduced amount of the at least one metal ion;

the third reactor comprising at least one inlet for receiving a second base and being fitted with a second pH probe;

the second pH probe being configured to at least substantially maintain pH in the third reactor at about 9.5 to about 11.5,

the third reactor further comprising at least one inlet for receiving at least one metal carbonate, and

the third reactor being configured to contain a third slurry, the third slurry comprising a second precipitate comprising at least one carbonate of the at least one metal ion and an aqueous composition comprising Li + and having a further reduced amount of the at least one metal ion;

a second filter,

the second filter being in fluid communication with the third reactor to receive at least a portion of the third slurry and being configured to separate the second precipitate from the aqueous composition comprising Li + and having a further reduced amount of the at least one metal ion; and

a fourth reactor,

the fourth reactor in fluid communication with the second filter to receive at least a portion of the aqueous composition comprising Li + and having a further reduced amount of the at least one metal ion, and

the fourth reactor comprising an ion exchange resin, the ion exchange resin being configured to contact the aqueous composition comprising Li + and having a further reduced amount of the at least one metal ion and thereby to remove the at least one metal ion and to obtain an aqueous composition comprising lithium sulphate.

2. The system of claim 1 , wherein the first pH probe is configured to at least substantially maintain pH in the second reactor at about 5.0 to about 6.2.

3. The system of claim 1 , wherein the first pH probe is configured to at least substantially maintain pH in the second reactor at about 5.4 to about 5.8.

4. The system of claim 1 , wherein the first base is lime.

5. The system of claim 1 , wherein the at least one metal ion of the aqueous composition comprising Li ± and at least one metal ion comprises Fe 3+ .

6. The system of claim 1 , wherein the at least one metal ion of the aqueous composition comprising Li ± and at least one metal ion comprises Al 3+ .

7. The system of claim 1 , wherein the first precipitate comprises Al(OH) 3 , Fe(OH) 3 , or mixtures thereof.

8. The system of claim 1 , wherein the second pH probe is configured to at least substantially maintain pH in the third reactor at about 10 to about 11.

9. The system of claim 1 , wherein the second pH probe is configured to at least substantially maintain pH in the third reactor at about 9.8 to about 10.2.

10. The system of claim 1 , wherein the ion exchange resin is cationic resin.

11. The system of claim 10 , wherein the cationic resin is substantially selective for divalent and/or trivalent metal ions.

12. The system of claim 1 , wherein the at least metal ion of the aqueous composition comprising Li ± and at least one metal ion comprises iron, aluminum, manganese, magnesium, or mixtures thereof.

13. The system of claim 1 , wherein the at least metal ion of the aqueous composition comprising Li ± and at least one metal ion comprises Al 3+ , Fe 3+ , Fe 2+ , Mg 2+ , Ca 2+ , Cr 2+ , Cr 3+ , Cr 6+ , Zn 2+ , M 2+ , or mixtures thereof.

14. The system of claim 1 , wherein the acid roasted lithium-containing material is β-spodumene that has been previously reacted with H 2 SO 4 .

15. The system of claim 1 , wherein the acid roasted lithium-containing material is α-spodumene, β-spodumene, epidolite, pegmatite, petalite, amblygonite, hectorite, smectite, clays, or mixtures thereof, that has been previously reacted with H 2 SO 4 .

16. The system of claim 1 , wherein the gas comprises oxygen.

17. The system of claim 1 , wherein the first reactor, the second reactor, the third reactor and the fourth reactor are each independently glass reactor, plastic reactor, or polytetrafluoroethylene reactor.

18. The system of claim 1 , wherein the first reactor, the second reactor, the third reactor and the fourth reactor each independently further comprises an impeller.

19. The system of claim 18 , wherein the first reactor comprises the impeller and wherein the sparger is below the impeller.

20. The system of claim 1 , wherein the first reactor is in fluid communication with the second reactor through a second filter or a clarifier, the second filter or the clarifier being configured to separate the solid from the aqueous composition comprising Li ± and at least one metal ion, and at least a portion of the aqueous composition comprising Li ± and at least one metal ion is received by the second reactor.

Assignments (4)
CHANGE OF ADDRESS FOR ASSIGNEE Recorded May 18, 2023
From: NEMASKA LITHIUM INC.
To: NEMASKA LITHIUM INC.
Reel/Frame 063903/0303 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 17, 2022
From: BOURASSA, GUY; PEARSE, GARY
To: NEMASKA LITHIUM INC.
Reel/Frame 059935/0329 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 17, 2022
From: MACKIE, STEPHEN CHARLES; GLADKOVAS, MYKOLAS
To: SGS CANADA INC.
Reel/Frame 059935/0575 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 17, 2022
From: SGS CANADA INC.
To: NEMASKA LITHIUM INC.
Reel/Frame 059935/0851 →
Continuity (7)
Continuation 16989877 · Aug 10, 2020
Continuation 15861587 · Jan 3, 2018
Continuation 15190296 · Jun 23, 2016
Continuation 14404466
Provisional Application 61767328 · Feb 21, 2013
Provisional Application 61653035 · May 30, 2012
Related Publication 20220259060A1 · Aug 18, 2022