Battery recycling by reduction and carbonylation

Patent metadata

Field	Value
Publication number	US-12412942-B2
Application number	US-202117906750-A
Country	US
Kind code	B2
Filing date	Mar 23, 2021
Priority date	Mar 23, 2020
Publication date	Sep 9, 2025
Grant date	Sep 9, 2025

Abstract

The present invention relates to a process for the recovery of transition metals from battery materials comprising (0.1) providing a battery material which comprises oxidic nickel and/or cobalt compounds, (1.1) heating the battery material above 350° C. to yield a reduced material which contains nickel and/or cobalt in elemental form, (2.1) carbonylating the reduced material with carbon monoxide optionally in the presence of a reactive gas to yield a solid carbonylation residue and a volatile carbonyl which comprises nickel and/or cobalt carbonyl containing compounds, and (3.1) separating the volatile carbonyl from the solid carbonylation residue by evaporation.

First claim

The invention claimed is:

1. A process for recovering transition metals from a battery material comprising:
(0.1) providing the battery material, wherein the battery material comprises oxidic nickel compounds, oxidic cobalt compounds, or combinations thereof,
(1.1) heating the battery material above 350° C. to yield a reduced material comprising nickel in elemental form, cobalt in elemental form, or combinations thereof,
(2.1) carbonylating the reduced material with carbon monoxide, optionally in the presence of a reactive gas, to yield a solid carbonylation residue and a volatile carbonyl, wherein the volatile carbonyl comprises nickel carbonyl containing compounds, cobalt carbonyl containing compounds, or combinations thereof, and
(3.1) separating the volatile carbonyl from the solid carbonylation residue by evaporation.

2. The process according to claim 1 , wherein the battery material is lithium ion battery materials.

3. The process according to claim 1 , wherein the battery material comprises complete batteries, mechanically treated waste batteries or battery scraps, or scrap from the production of batteries or battery components.

4. The process according to claim 1 , wherein the battery material comprises from 1 wt % to 30 wt %, oxidic nickel compounds.

5. The process according to claim 1 , wherein the battery material comprises from 1 wt % to 30 wt %, oxidic cobalt compounds.

6. The process according to claim 1 , wherein step (1.1) comprises heating the battery material in an inert, hydrogen, or oxygen atmosphere.

7. The process according to claim 1 , wherein the carbonylating is achieved at a temperature ranging from 30° C. to 300° C. and a partial pressure ranging from 1 bar to 300 bar.

8. The process according to claim 1 , wherein the volatile carbonyl comprises Ni(CO) 4 , HCo(CO) 4 , (NO)Co(CO) 3 , or combinations thereof.

9. The process according to claim 1 , wherein the carbonylating step further comprises carbonylating with a gas comprising an inert gas, a reactive gas, or a combination thereof.

10. The process according to claim 9 , wherein the carbonylating step comprises carbonylating with the inert gas, and the inert gas is selected from the group consisting of nitrogen, argon, carbon dioxide, and combinations thereof.

11. The process according to claim 9 , wherein the carbonylating step comprises carbonylating with the reactive gas, and the reactive gas is selected from the group consisting of hydrogen, nitric oxide, and combinations thereof.

12. The process according to claim 1 , wherein during the carbonylating step, a carbonylation catalyst is present and the carbonylation catalyst is selected from ammonia, sulfur, and sulfur compounds.

13. The process according to claim 1 , wherein nickel and cobalt are present in the reduced material and the reduced material is first carbonlyated in the absence of a reactive gas to yield a volatile nickel carbonyl, and next in the presence of reactive gas to yield a volatile cobalt carbonyl or vice versa.

14. The process according to claim 1 , further comprising:
(4.1) decomposing the volatile carbonyl to yield nickel in elemental form or as salts, cobalt in elemental form or as salts, or combinations thereof.

15. The process according to claim 1 , wherein step (0.1) comprises at least one of the following steps:
(0.2) optionally washing the battery material with an organic solvent to remove organic electrolyte and polymeric binder,
(0.3) optionally washing the battery material with an aqueous medium,
(0.4) optionally subjecting the battery material to a solid-solid separation to remove solids,
(0.5) optionally heating the battery material up to 350° C. to evaporate organic components of the electrolyte;
wherein step (1.1) comprises at least one of the following steps:
(1.2) optionally subjecting the reduced material to a dry solid-solid separation to remove solids,
(1.3) optionally treating the reduced material with an aqueous medium, which is optionally acidic, to yield a slurry comprising a dissolved lithium salt and an undissolved material, optionally further subjecting the slurry to a solid-liquid separation to separate the dissolved lithium salt from the undissolved material, and optionally further subjecting the undissolved material to a solid-solid separation to remove solids;
wherein step (3.1) comprises at least one of the following steps:
(3.2) optionally purifying the separated volatile carbonyl by adsorption, condensation, distillation, or vaporization,
(3.3) optionally decomposing a non-volatile metal carbonyl in the solid carbonylation residue,
(3.4) optionally subjecting the solid carbonylation residue to a dry solid-solid separation to remove solids,
(3.5) optionally treating the solid carbonylation residue with an aqueous medium, which is optionally acidic, to yield a slurry comprising a dissolved lithium salt and an undissolved material, optionally further subjecting the slurry to a solid-liquid separation to separate the dissolved lithium salt from the undissolved material, and optionally further subjecting the undissolved material to a solid-solid separation to remove solids; and
further comprising at least one of the following:
(4.1) optionally decomposing the volatile carbonyl to yield nickel in elemental form or as salts, cobalt in elemental form or as salts, or combinations thereof,
(4.2) optionally further purifying the nickel, cobalt, or combinations thereof.

Assignees

• Basf Se

Inventors

• Rohde Wolfgang
• Adermann Torben
• Schierle-Arndt Kerstin
• Huguet Subiela Nuria
• Kempter Andreas
• Gerke Birgit

Classifications

• C22B23/065 Primary

  carbonyl methods · CPC title

• C22B23/021

  by reduction in solid state, e.g. by segregation processes · CPC title

• C22B5/12

  by gases · CPC title

• C22B1/005

  Preliminary treatment of scrap (C22B1/02 - C22B1/26 take precedence) · CPC title

• C01G53/02

  Carbonyls · CPC title