IP Library › Granted Patent US 12,403,427
Granted Patent B2
US 12,403,427 · App. 17/928,262 · Granted Sep 2, 2025

Method of separating and recovering cobalt salt and nickel salt

Inventors: Tomoya Yoshizaki (Otsu, JP); Takanori Soya (Otsu, JP); Masakazu Koiwa (Otsu, JP); Shigehisa Hanada (Otsu, JP)
Assignee: Toray Industries, Inc.
B01D61/0271B01D61/025B01D61/029B01D61/04B01D69/02B01D69/10B01D69/12B01D71/56C01G51/10C01G53/10C02F9/00C22B3/06C22B3/22C22B23/0407C22B23/0453B01D2311/04B01D2311/06B01D2317/025C02F1/441C02F1/442C02F1/66C02F2101/20C02F2301/08
View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 12,403,427
App. No.
17/928,262
Granted
Sep 2, 2025
Kind
B2
Abstract

A method of separating and recovering a cobalt salt and a nickel salt includes a separation step of separating, by using a nanofiltration membrane, a cobalt salt and a nickel salt from a rare metal-containing aqueous solution containing at least both the cobalt salt and the nickel salt as rare metals, in which the nanofiltration membrane has a glucose permeability of 3 times or more a sucrose permeability, the sucrose permeability of 10% or less, and an isopropyl alcohol permeability of 50% or more when a 1,000 mg/L glucose aqueous solution, a 1,000 mg/L sucrose aqueous solution, and a 1,000 mg/L isopropyl alcohol aqueous solution, each having a pH of 6.5 and a temperature of 25° C., individually permeate through the nanofiltration membrane at an operating pressure of 0.5 MPa.

Claims (23)

1. A method of separating and recovering a cobalt salt and a nickel salt, the method comprising a separation step of separating, by using a nanofiltration membrane, a cobalt salt and a nickel salt from a rare metal-containing aqueous solution containing at least both the cobalt salt and the nickel salt as rare metals,

wherein the nanofiltration membrane has a glucose permeability of 3 times or more a sucrose permeability, the sucrose permeability of 10% or less, and an isopropyl alcohol permeability of 50% or more when a 1,000 mg/L glucose aqueous solution, a 1,000 mg/L sucrose aqueous solution, and a 1,000 mg/L isopropyl alcohol aqueous solution, each having a pH of 6.5 and a temperature of 25° C., individually permeate through the nanofiltration membrane at an operating pressure of 0.5 MPa.

2. The method according to claim 1 , wherein the nanofiltration membrane comprises a base material, a support membrane on the base material, and a separation function layer on the support membrane, and

the separation function layer comprises a polyamide having a structure derived from a polyfunctional aliphatic amine and a structure derived from a polyfunctional acid halide.

3. The method according to claim 2 , wherein the polyfunctional aliphatic amine is a compound represented by formula (1),

provided that R 1 and R 2 each independently represent an alkyl group having 1 to 6 carbon atoms, a phenyl group, a benzyl group, COOR 5 , CONHR 5 , CON(R 5 ) 2 , or OR 5 , and R 5 represents a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, a phenyl group, or a benzyl group; and R 3 and R 4 each independently represent hydrogen, an alkyl group having 1 to 6 carbon atoms, a phenyl group, a benzyl group, COOR 6 , CONHR 6 , CON(R 6 ) 2 , or OR 6 , and R 6 represents a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, a phenyl group, or a benzyl group.

4. The method according to claim 2 , wherein the polyamide is a crosslinked aromatic polyamide having a structure represented by formula (2),

provided that R 1 and R 2 each independently represent an alkyl group having 1 to 6 carbon atoms, a phenyl group, a benzyl group, COOR 5 , CONHR 5 , CON(R 5 ) 2 , or OR 5 , and R 5 represents a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, a phenyl group, or a benzyl group; R 3 and R 4 each independently represent hydrogen, an alkyl group having 1 to 6 carbon atoms, a phenyl group, a benzyl group, COOR 6 , CONHR 6 , CON(R 6 ) 2 , or OR 6 , and R 6 represents a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, a phenyl group, or a benzyl group; R 7 is an aliphatic chain or an aliphatic ring comprising only a carbon atom and a hydrogen atom as a constituent element; and Ar 8 is an aromatic ring having 6 to 14 carbon atoms which may have a substituent.

5. The method according to claim 1 , further comprising a complex forming step of adding a complex forming agent to the rare metal-containing aqueous solution before the separation step,

wherein the complex forming agent has a solubility in water of 100 mg/L or more.

6. The method according to claim 5 , wherein the complex forming step comprises a step of adjusting a pH of the rare metal-containing aqueous solution to 1 or more and 9 or less.

7. The method according to claim 5 , wherein the complex forming step comprises a step of adding an amine-based ligand as the complex forming agent.

8. The method according to claim 1 , further comprising, before the separation step, an acid treatment step of bringing a material containing at least both cobalt and nickel as rare metals into contact with an acid aqueous solution to obtain the rare metal-containing aqueous solution.

9. The method according to claim 8 , further comprising a mixing step of mixing a permeated water generated in a concentration step with the rare metal-containing aqueous solution obtained in the acid treatment step,

wherein, in the separation step, the permeated water and a concentrated water are obtained from a mixed water obtained in the mixing step.

10. The method according to claim 1 , wherein the separation step comprises at least a first separation step and a 2a-th separation step which use the nanofiltration membrane, and

a permeated water obtained in the first separation step is treated in the 2a-th separation step.

11. The method according to claim 10 , wherein the permeated water obtained in the first separation step is diluted to be treated in the 2a-th separation step.

12. The method according to claim 1 , wherein the separation step comprises at least a first separation step and a 2b-th separation step which use the nanofiltration membrane, and

a non-permeated water obtained in the first separation step is treated in the 2b-th separation step.

13. The method according to claim 12 , wherein the non-permeated water obtained in the first separation step is diluted to be treated in the 2b-th separation step.

14. The method according to claim 1 , further comprising, before the separation step, a pre-separation step of separating an alkali metal salt and a polyvalent rare metal salt by using the nanofiltration membrane, to obtain a permeated water in which an alkali metal ion concentration (mg/L) is 100 times or more a polyvalent rare metal ion concentration (mg/L).

15. The method according to claim 1 , further comprising a concentration step of concentrating an aqueous solution obtained in the separation step with a reverse osmosis membrane.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 28, 2022
From: YOSHIZAKI, TOMOYA; SOYA, TAKANORI; KOIWA, MASAKAZU; HANADA, SHIGEHISA
To: TORAY INDUSTRIES, INC.
Reel/Frame 061896/0611 →
Priority Claims (1)
JP 2020-094338 · May 29, 2020 · national
Continuity (1)
Related Publication 20230219040A1 · Jul 13, 2023
References Cited (31)
US 6843917B1 · Guy et al. · 2005 [cited by applicant]
US 10308523B1 · Chow · 2019 [cited by examiner]
US 11905180B2 · Yoshizaki · 2024 [cited by examiner]
US 20100150802A1 · Gilliam et al. · 2010 [cited by applicant]
US 20170136422A1 · Ogawa · 2017 [cited by examiner]
US 20180155208A1 · Chow et al. · 2018 [cited by applicant]
EP 4141135A1 · 2023 [cited by applicant]
JP 62201606A · 1987 [cited by applicant]
JP 411928B2 · 1992 [cited by applicant]
JP 11226366A · 1999 [cited by applicant]
JP 2003500542A · 2003 [cited by applicant]
JP 2019173063A · 2019 [cited by applicant]
JP 2020513397A · 2020 [cited by applicant]
KR 20060086209A · 2006 [cited by applicant]
WO 2013026093A1 · 2013 [cited by applicant]
WO 2014094003A2 · 2014 [cited by applicant]
WO 2019018333A1 · 2019 [cited by applicant]
Dupont Product Data Sheet FilmTec NF270 Element. No date. Retrieved from internet 2025. [cited by examiner]
Dupont Product Data Sheet FilmTec NF270-400/34i Element. No date. Retrieved from internet 2025. [cited by examiner]
Office Action dated Mar. 22, 2024, of counterpart Canadian Patent Application No. 3,185,166. [cited by applicant]
International Preliminary Report on Patentability dated Nov. 17, 2022, of corresponding International Application No. PCT/JP2021/020477 along with an English translation of Written Opinion of the International Searching… [cited by applicant]
Extended European Search Report dated May 21, 2024, of counterpart European Patent Application No. 21812490.7. [cited by applicant]
“FilmTec™ Membranes, FilmTec™ NF270 Nanofiltration Elements for Commercial Systems,” Dupont, XP093159661, Aug. 1, 2021, Product Worksheet retrieved from the internet on May 6, 2024: http://www.dupont.com/products/filmte… [cited by applicant]
International Search Report dated Aug. 10, 2021, of corresponding International Application No. PCT/JP2021/020477 along with an English translation. [cited by applicant]
Lin, Su-Hsia et al., “Metal Rejection by Nanofiltration from Diluted Solutions in the Presence of Complexing Agents,” [cited by applicant]
Belkhouche, Nasr-Eddine et al., “Separation of cobalt and nickel by nanofiltration using a FilmTec membrane,” [cited by applicant]
Nguyen, Nguyen Cong et al., “Separation of three divalent cations (Cu [cited by applicant]
“Exploration Project for Promoting the Development of Mineral Resources in FY2017: Report on a study on mineral resource infrastructure development (basic study for the formulation of a strategy to secure mineral resour… [cited by applicant]
Office Action dated Feb. 12, 2025, from counterpart Japanese Application No. 2021-531280. [cited by applicant]
Office Action dated Jun. 16, 2025, from counterpart Korean Patent Application No. 10-2022-7041416. [cited by applicant]
Yali Zhao et al., “Preparation of a highly permeable nanofiltration membrane using a novel acyl chloride monomer with -PO(CI)2 group,” Desalination 431, 2018, pp. 56-65. [cited by applicant]