IP Library Granted Patent US 12,209,028
Granted Patent B2
US 12,209,028 · App. 18/688,799 · Granted Jan 28, 2025

Method and system for recovering metals from black mass

Inventors: Anne-Marie Suriano (Hamburg, DE); Leslie James Bryson (Hamburg, DE); Marcus Eschen (Senden, DE)
Assignee: AURUBIS AG
C01D15/02C01B25/30C01D15/08C01G45/02C01G53/04C01G53/10C22B3/22C22B3/44C22B7/006C22B23/0461C22B26/12C22B47/00H01M10/54
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Quick Facts
Patent No.
US 12,209,028
App. No.
18/688,799
Granted
Jan 28, 2025
Kind
B2
Abstract

A process recovers metals from a black mass. The process includes the following steps in the following order: step (a) providing the black mass, which comprises Li; step (b) adding water to the black mass and creating a suspension of the black mass in the water; step (c) dosing ozone as an oxidant to the suspension while stirring the suspension; and step (d) filtering and separating a filtrate containing LiOH dissolved in water from a Li depleted residue of the black mass. In step (c), the suspension is stirred with a shear rate greater than 11000 s −1 within the suspension.

Claims (51)

1. A process for recovery of metals from a black mass, the process comprising the following steps in the following order:

step (a) providing the black mass, which comprises Li;

step (b) adding water to the black mass and creating a suspension of the black mass in the water;

step (c) dosing ozone as an oxidant to the suspension while stirring the suspension; and

step (d) filtering and separating a filtrate containing LiOH dissolved in water from a Li depleted residue of the black mass

wherein in step (c), the suspension is stirred with a shear rate greater than 11,000 s-1 within the suspension,

wherein the process further comprises, in a step (e), leaching the Li depleted residue of step (d) in an acidic leach, wherein at least one acid is added and the pH value is dropped below pH 3,

wherein the process further comprises:

adding a calcium source to the leachate or the suspension of step (e); and

in a step (f), filtering the suspension, and

wherein the process further comprises,

in a step (g), dosing ozone as an oxidant to the filtrate of step (f) while stirring, maintaining a pH value in the range of 2 to 4, and filtering the resulting suspension.

2. The process according to claim 1 , wherein:

in step (c), the suspension is stirred with the shear rate greater than 25,000 s-1 within the suspension.

3. The process according to claim 1 , wherein:

step (c) is performed for at least three hours.

4. The process according to claim 1 , wherein:

in step (c), ozone is dosed to the suspension with a rate of at least 0.1 gram (O 3 )/hour/gram (black mass) or with a maximum rate of 2 gram (O 3 )/hour/gram (black mass).

5. The process according to claim 1 , wherein:

in step (c), the temperature of the suspension is in the range from 70° C. to 95° C.

6. The process according to claim 1 , wherein:

in step (c), the suspension of the black mass in the water has a pH value in the range between 6 to 8.

7. The process according to claim 1 , the process further comprising:

adding an acid to the suspension in step (b) or step (c); and

dropping the pH value of the suspension to a pH value in the range between 3.5 and 4.5.

8. The process according to claim 7 , the process further comprising:

after step (c), adding a caustic; and

raising the pH value of the suspension before step (d) or raising the pH value of the filtrate of step (d) to a pH value higher than 6.

9. The process according to claim 1 , the process further comprising:

evaporating at least 20 vol % of the filtrate containing LiOH dissolved in water.

10. The process according to claim 1 , comprising:

precipitating lithium hydroxide (LiOH) from the filtrate containing LiOH dissolved in water by evaporation or crystallization.

11. The process according to claim 1 , the process further comprising:

adding one of the following additives to the filtrate containing LiOH dissolved in water:

a phosphate source and precipitating lithium phosphate (Li 3 PO 4 ); or

a carbonate source and precipitating lithium carbonate (Li 2 CO 3 ).

12. The process according to claim 10 , the process further comprising:

adding a caustic to the filtrate containing LiOH dissolved in water.

13. The process according to claim 10 , the process further comprising:

filtering the precipitated lithium hydroxide (LiOH) out; and

recirculating the filtrate back to the suspension of the black mass and the water in step (b) or (c).

14. The process according to claim 13 , the process further comprising:

bleeding the recirculated filtrate periodically.

15. The process according to claim 1 , the process further comprising:

adding a reductant to the acidic leach step (e).

16. The process according to claim 1 , the process further comprising:

in a step (h), adding sulfuric acid (H 2 SO 4 ) to the filtrate of step (g); and

raising the sulfuric acid (H 2 SO 4 ) concentration to at least 500 g/L to crystallize Ni-sulfate.

17. The process according to claim 11 , the process further comprising:

filtering the precipitated lithium phosphate (Li 3 PO 4 ) or lithium carbonate (Li 2 CO 3 ) out; and

recirculating the filtrate back to the suspension of the black mass and the water in step (b) or (c).

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 26, 2024
From: SURIANO, ANNE-MARIE; BRYSON, LESLIE JAMES; ESCHEN, MARCUS
To: AURUBIS AG
Reel/Frame 068090/0759 →
Priority Claims (1)
DE 10 2021 123 151.5 · Sep 7, 2021 · national
Continuity (1)
Related Publication 20240270590A1 · Aug 15, 2024
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