Process for preparing battery grade metal sulphate solutions

Patent metadata

Field	Value
Publication number	US-2023312368-A1
Application number	US-202118044043-A
Country	US
Kind code	A1
Filing date	Sep 7, 2021
Priority date	Sep 9, 2020
Publication date	Oct 5, 2023
Grant date	—

Abstract

Battery grade metal sulfate solutions can be prepared directly from electrolytically produced metal objects, such as cathode plates, when these are subjected to an aqueous leaching solution comprising at least one acid leaching agent and a liquid oxidizing agent in a continuous process at elevated temperature and with vigorous mixing. A leaching arrangement comprising a leaching column or reaction vessel is also disclosed.

First claim

1 . A process for preparing battery grade metal sulfate solutions, characterized in that electrolytically produced metal objects are subjected to an aqueous leaching solution at an elevated temperature and acid pH in a continuous process with mixing, said leaching solution comprising at least one acid leaching agent and an oxidizing agent in liquid form.

2 . The process according to claim 1 , wherein said mixing is achieved by recirculating the aqueous leaching solution through a leaching column operating in counter-current mode.

3 . The process according to claim 1 , wherein the resulting battery grade metal sulfate solution has a residual sulfuric acid concentration in the interval of 0-10 g/l, preferably 0-6 g/l.

4 . The process according to claim 1 , wherein the electrolytically produced metal objects are chosen from nickel cathode plates, squares, rounds, tubes, crowns and chippings and the resulting metal sulfate solution is a battery grade nickel sulfate solution.

5 . The process according to claim 1 , wherein the electrolytically produced metal objects are chosen from cobalt cathode plates, squares, rounds, tubes, crowns and chippings and the resulting metal sulfate solution is a battery grade cobalt sulfate solution.

6 . The process according to claim 1 , wherein the acid leaching agent is selected from the group comprising sulfuric acid, hydrochloric acid, nitric acid, oxalic acid, citric acid, or a combination of at least two of these.

7 . The process according to claim 1 , wherein the liquid oxidizing agent is selected from the group comprising hydrogen peroxide, halogens, and halogen compounds such as chlorates and perchlorates, citric acid or oxalic acid.

8 . The process according to any one of the claims 1 - 7 , wherein the leaching solution comprises a mixture of sulfuric acid and citric acid.

9 . The process according to any one of the claims 1 - 7 , wherein the pH is maintained in an interval of 1-6, preferably pH 1-4.

10 . The process according to any one of the claims 1 - 7 , wherein said oxidizing agent is hydrogen peroxide in liquid form.

11 . The process according to any one of the claims 1 - 7 , wherein the temperature is maintained at a temperature in an interval between 50° C. and up to the boiling point of the leaching solution, preferably between 75° C. and the boiling point of the leaching solution.

12 . The process according to claim 1 , including a step of separation of metal fines from the recirculating leaching solution.

13 . The process according to claim 12 , including a step of removal of copper wherein metallic copper is deposited on the metal fines and said fines are removed from circulation.

14 . An arrangement for performing the process of any one of claims 1 - 13 , characterized in that it comprises at least one reactor vessel with a recirculation loop, a pump, a solid/liquid separator, inlets for the addition of acid, liquid oxidizing agent and electrolytically produced metal objects, and an outlet for removal of metal sulphate solution, wherein metal objects can be added, and battery grade metal sulphate solution removed without interrupting the process.

15 . The arrangement according to claim 14 , wherein the reactor vessel is a substantially vertical column adapted for adding metal objects at one end, and introduction of recirculating leaching solution in a counter-current mode in relation to the direction of addition of the metal objects.

16 . The arrangement according to claim 14 or 15 , wherein the reactor vessel is made from a fiber reinforced polymer material.

Assignees

• Northvolt Ab
• Metal Trade Overseas Ag

Inventors

• Lantto Cornelia
• Niemi Tom
• Alisaari Pekka
• Lindell Esa
• Luoma Rauno
• Laukkanen Tuomo
• Tynjälä Pekka
• Lassi Ulla

Classifications

• C01G53/10 Primary

  Sulfates · CPC title

• C22B23/043

  Sulfurated acids or salts thereof · CPC title

• C01P2006/80

  Compositional purity · CPC title

• C22B23/0415

  with acids or salt solutions except ammonium salts solutions · CPC title

• Y02E60/10

  Energy storage using batteries · CPC title