Method for producing nickel powder

Patent metadata

Field	Value
Publication number	US-10118224-B2
Application number	US-201515114218-A
Country	US
Kind code	B2
Filing date	Jan 27, 2015
Priority date	Jan 30, 2014
Publication date	Nov 6, 2018
Grant date	Nov 6, 2018

Abstract

Provided is a method for producing nickel powder from a nickel ammine sulfate complex solution, comprising treatment steps of: (1) a seed crystal production step of producing nickel powder having an average particle size of 0.1 to 5 μm; (2) a seed crystal addition step of adding the nickel powder obtained in the step (1) as seed crystals to form a mixed slurry; (3) a reduction step of forming a reduced slurry containing nickel powder formed by precipitation of a nickel component in the mixed slurry on the seed crystals; and (4) a growth step of performing solid-liquid separation to separate and recover the nickel powder as a solid phase component and then blowing hydrogen gas into a solution prepared by adding the nickel ammine sulfate complex solution to the recovered nickel powder to grow the nickel powder to form high purity nickel powder.

First claim

The invention claimed is:

1. A method for producing nickel powder from a nickel ammine sulfate complex solution, the method comprising treatment steps of:
(1) a seed crystal production step of mixing a nickel sulfate solution and hydrazine to produce nickel powder having an average particle size of 0.1 to 5 μm serving as seed crystals;
(2) a seed crystal addition step of adding the nickel powder having an average particle size of 0.1 to 5 μm obtained in the step (1) as seed crystals to the nickel ammine sulfate complex solution to form a mixed slurry;
(3) a reduction step of blowing hydrogen gas into the mixed slurry obtained in the seed crystal addition step (2) to form a reduced slurry by precipitation of a nickel component in the mixed slurry on the seed crystals; and
(4) a growth step of subjecting the reduced slurry formed in the reduction step (3) to solid-liquid separation to separate the nickel component in the reduced slurry to form a recovered nickel powder as a solid phase component and then blowing hydrogen gas into a solution prepared by adding the nickel ammine sulfate complex solution to the recovered nickel powder and thereby causing the recovered nickel powder to grow and form high purity nickel powder.

2. The method for producing nickel powder according to claim 1 , wherein an alkali is further mixed when a nickel sulfate solution and hydrazine are mixed in the seed crystal production step (1).

3. The method for producing nickel powder according to claim 2 , wherein a dispersant is further added to the mixed slurry when the seed crystals are added to the nickel ammine sulfate complex solution to form a mixed slurry in the seed crystal addition step (2).

4. The method for producing nickel powder according to claim 3 , wherein, in the seed crystal addition step (2), an amount of the seed crystals added is 1 to 100% based on a weight of nickel in the nickel ammine sulfate complex solution.

5. The method for producing nickel powder according to claim 4 , wherein the dispersant contains a sulfonate.

6. The method for producing nickel powder according to claim 2 the nickel ammine sulfate complex solution is obtained by:
a leaching step of dissolving a nickel-containing material containing cobalt as an impurity;
a solvent extraction step of adjusting pH of a leachate containing nickel and cobalt obtained in the leaching step and then separating the leachate into a nickel sulfate solution and a cobalt-recovering solution by solvent extraction; and
a complexing step of subjecting the nickel sulfate solution to complexing treatment with ammonia.

7. The method for producing nickel powder according to claim 6 , wherein the nickel-containing material is at least one powder of nickel and cobalt mixed sulfide, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, and metallic nickel.

8. The method for producing the nickel powder according to claim 6 , wherein 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester or di-(2,4,4-trimethylpentyl)phosphinic acid is used in the solvent extraction.

9. The method for producing nickel powder according to claim 6 , wherein a concentration of ammonium sulfate in the nickel ammine sulfate complex solution is 100 to 500 g/l, and an ammonium concentration is 1.9 or more in a molar ratio based on a concentration of nickel in the complex solution.

10. The method for producing nickel powder according to claim 6 , wherein the nickel sulfate solution produced by the solvent extraction step is the nickel sulfate solution in the seed crystal production step (1).

11. The method for producing nickel powder according to claim 6 , further comprising at least one ammonia recovery step of adding an alkali to at least one post-reaction solution obtained in the reduction step (3) and/or in the growth step (4) and heating the resulting mixture to volatilize and recover ammonia gas.

12. The method for producing nickel powder according to claim 11 , wherein the ammonia recovered in the ammonia recovery step is recycled as ammonia used for producing the nickel ammine sulfate complex solution used in the solvent extraction step and the complexing step, and as ammonia as an alkali used for mixing in the seed crystal production step (1).

13. The method for producing nickel powder according to claim 1 , wherein the reduction step (3) and the growth step (4) are each performed by maintaining a temperature of 150 to 200° C. and a pressure of 1.0 to 4.0 MPa.

14. The method for producing nickel powder according to claim 1 , further comprising:
a nickel powder briquetting step of processing the high purity nickel powder obtained in the growth step (4) into nickel briquettes in a massive form using a briquetting machine; and
a briquette sintering step of sintering the resulting nickel briquettes in a massive form under holding conditions at a temperature of 500 to 1200° C. in a hydrogen atmosphere to form nickel briquettes as a sintered body.

15. The method for producing nickel powder according to claim 1 , further comprising at least one ammonium sulfate recovery step of concentrating at least one post-reaction solution obtained in the reduction step (3) and/or in the growth step (4) to precipitate ammonium sulfate and to recover ammonium sulfate crystals.

16. The method for producing nickel powder according to claim 1 , wherein a dispersant is further added to the mixed slurry when the seed crystals are added to the nickel ammine sulfate complex solution to form a mixed slurry in the seed crystal addition step (2).

17. The method for producing nickel powder according to claim 1 , wherein, in the seed crystal addition step (2), an amount of the seed crystals added is 1 to 100% based on a weight of nickel in the nickel ammine sulfate complex solution.

18. The method for producing nickel powder according to claim 1 the nickel ammine sulfate complex solution is obtained by:
a leaching step of dissolving a nickel-containing material containing cobalt as an impurity;
a solvent extraction step of adjusting pH of a leachate containing nickel and cobalt obtained in the leaching step and then separating the leachate into a nickel sulfate solution and a cobalt-recovering solution by solvent extraction; and
a complexing step of subjecting the nickel sulfate solution to complexing treatment with ammonia.

19. The method for producing nickel powder according to claim 1 , comprising at least one ammonia recovery step of adding an alkali to at least one post-reaction solution obtained in the reduction step (3) and/or in the growth step (4) and heating the resulting mixture to volatilize and recover ammonia gas.

Assignees

• Kochi Univ National Univ Corporation
• Sumitomo Metal Mining Co

Inventors

• Yanagisawa Kazumichi
• Zhang Junhao
• HEGURI Shin-ichi
• Ohara Hideki
• Ikeda Osamu
• Yoneyama Tomoaki
• Kudo Yohei
• Ozaki Yoshitomo

Classifications

• B22F1/00

  Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties · CPC title

• B22F3/10 Primary

  Sintering only · CPC title

• B22F2201/013

  Hydrogen · CPC title

• B22F1/0003

  Operations & Transport · mapped topic

• C22B23/0461

  by chemical methods · CPC title