Process for producing nickel powder

Patent metadata

Field	Value
Publication number	US-10850330-B2
Application number	US-201615769521-A
Country	US
Kind code	B2
Filing date	Oct 14, 2016
Priority date	Oct 19, 2015
Publication date	Dec 1, 2020
Grant date	Dec 1, 2020

Abstract

A process for producing nickel powder capable of obtaining inexpensive, and also, high-performance nickel powder, even when using wet process. A process for producing nickel powder, including a crystallization step for obtaining nickel crystal powder by reductive reaction in reaction solution in which at least water-soluble nickel salt, metal salt of metal more noble than nickel, reducing agent, alkali hydroxide, amine compound, and water are mixed, wherein the reducing agent to be mixed in the crystallization step is hydrazine, the amine compound is autolysis inhibitor of hydrazine, and contains two or more primary amino groups in molecule, or contains one primary amino group and one or more secondary amino groups in molecule, and ratio of molar number of the amine compound with respect to molar number of nickel in the reaction solution is in a range of 0.01 mol % to 5 mol %.

First claim

The invention claimed is:

1. A process for producing nickel powder, comprising a crystallization step including obtaining nickel crystal powder formed by a reductive reaction in a reaction solution in which at least a water-soluble nickel salt, a metal salt of a metal more noble than nickel, hydrazine (N 2 H 4 ), an alkali hydroxide, an amine compound, a sulfide compound, and water are mixed,
wherein:
the amine compound is an autolysis inhibitor of the hydrazine,
the amine compound contains two or more primary amino groups (—NH 2 ) in the molecule, or contains one primary amino group (—NH 2 ) and one or more secondary amino groups (—NH—) in the molecule,
a ratio of a molar number of the amine compound with respect to a molar number of nickel in the reaction solution is in a range of from 0.01 mol % to 5 mol %,
the sulfide compound is an autolysis inhibition adjuvant of the hydrazine,
the sulfide compound contains one or more sulfide group (—S—) in the molecule, and
a ratio of a molar number of the sulfide compound with respect to the molar number of the nickel in the reaction solution is in a range of from 0.01 mol % to 5 mol %.

2. The process for producing nickel powder according to claim 1 , wherein the amine compound is at least one of an alkylene amine and an alkylene amine derivative.

3. The process for producing nickel powder according to claim 2 , wherein the alkylene amine or the alkylene amine derivative is at least one compound having a structure represented by formula A, in which nitrogen atoms of the amino group in the molecule are bonded via a carbon chain with two carbons

4. The process for producing nickel powder according to claim 3 , wherein
the alkylene amine is one or more selected from the group consisting of ethylene diamine (H 2 NC 2 H 4 NH 2 ), diethylene triamine (H 2 NC 2 H 4 NHC 2 H 4 NH 2 ), triethylene tetramine (H 2 N(C 2 H 4 NH) 2 C 2 H 4 NH 2 ), tetraethylene pentamine (H 2 N(C 2 H 4 NH) 3 C 2 H 4 NH 2 ), pentaethylene hexamine (H 2 N(C 2 H 4 NH) 4 C 2 H 4 NH 2 ), and propylene diamine (CH 3 CH(NH 2 )CH 2 NH 2 ), and
the alkylene amine derivative is one or more selected from the group consisting of tris (2-aminoethyl) amine (N(C 2 H 4 NH 2 ) 3 ), N-(2-aminoethyl) ethanol amine (H 2 NC 2 H 4 NHC 2 H 4 OH), N-(2-aminoethyl) propanol amine (H 2 NC 2 H 4 NHC 3 H 6 OH), 2, 3-diaminopropionic acid (H 2 NCH 2 CH(NH)COOH), and 1, 2-cyclohexane diamine (H 2 NC 6 H 10 NH 2 ).

5. The process for producing nickel powder according to claim 1 , wherein the sulfide compound is a carboxy group-containing sulfide compound or a hydroxyl group-containing sulfide compound further containing at least one or more carboxy group (—COOH) or hydroxyl group (—OH) in the molecule.

6. The process for producing nickel powder according to claim 5 , wherein the carboxy group-containing sulfide compound or the hydroxyl group-containing sulfide compound is one or more selected from the group consisting of methionine (CH 3 SC 2 H 4 CH(NH 2 )COOH), ethionine (C 2 H 5 SC 2 H 4 CH(NH 2 )COOH), thiodipropionic acid (HOOCC 2 H 4 SC 2 H 4 COOH), thiodiglycolic acid (HOOCCH 2 SCH 2 COOH), and thiodiglycol (HOC 2 H 5 SC 2 H 5 OH).

7. The process for producing nickel powder according to claim 1 , wherein a ratio of a used amount of a molar number of the hydrazine with respect to the molar number of the nickel is less than 2.0, in the crystallization step.

8. The process for producing nickel powder according to claim 1 , wherein a ratio of a used amount of a molar number of the hydrazine with respect to the molar number of the nickel is less than 1.3, in the crystallization step.

9. The process for producing nickel powder according to claim 1 , wherein the water-soluble nickel salt is one or more selected from the group consisting of nickel chloride (NiCl 2 ), nickel sulfate (NiSO 4 ), and nickel nitrate (Ni(NO 3 ) 2 ).

10. The process for producing nickel powder according to claim 1 , wherein the metal salt of metal more noble than nickel is one or more selected from the group consisting of a copper salt, a gold salt, a silver salt, a platinum salt, a palladium salt, a rhodium salt, and an iridium salt.

11. The process for producing nickel powder according to claim 1 , wherein the alkali hydroxide is one or more selected from the group consisting of sodium hydroxide (NaOH) and potassium hydroxide (KOH).

12. The process for producing nickel powder according to claim 1 , wherein the crystallization step further includes:
(i) preparing:
(1) a nickel salt solution by dissolving at least the water soluble nickel salt and the metal salt of metal more noble than nickel in water, and
(2) a reducing agent solution by mixing at least the reducing agent, the alkali hydroxide, and water,

(ii) adding the amine compound to at least one of the nickel salt solution and the reducing agent solution,
(iii) adding the sulfide compound to at least one of the nickel salt solution and the reducing agent solution, and then
(iv) mixing the nickel salt solution and the reducing agent solution.

13. The process for producing nickel powder according to claim 1 , wherein the crystallization step further includes:
(i) preparing:
(1) a nickel salt solution by dissolving at least the water soluble nickel salt and the metal salt of metal more noble than nickel in water, and
(2) a reducing agent solution by mixing at least the reducing agent, the alkali hydroxide, and water,

(ii) mixing the nickel salt solution and the reducing agent solution to form a first mixture, and then
(iii) mixing the first mixture and the amine compound to form a second mixture, and
(iv) mixing the second mixture and the sulfide compound.

14. The process for producing nickel powder according to claim 1 , wherein the crystallization further includes:
(i) preparing:
(1) a nickel salt solution by dissolving at least the water soluble nickel salt and the metal salt of metal more noble than nickel in water, and
(2) a reducing agent solution by mixing at least the reducing agent, the alkali hydroxide, and

(ii) adding the sulfide compound to at least one of the nickel salt solution and the reducing agent solution, followed by
(iii) mixing the nickel salt solution and the reducing agent solution to form a mixture, and then
(iv) mixing the mixture and the amine compound.

15. The process for producing nickel powder according to claim 1 , wherein the crystallization step further includes:
(i) preparing:
(1) a nickel salt solution by dissolving at least the water soluble nickel salt and the metal salt of metal more noble than nickel in water,
(2) a reducing agent solution by mixing at least the reducing agent and water, and
(3) an alkali hydroxide solution by mixing at least the alkali hydroxide and water, are prepared,

(ii) adding the amine compound to at least one of the nickel salt solution, the reducing agent solution, and the alkali hydroxide solution,
(iii) adding the sulfide compound to at least one of the nickel salt solution, the reducing agent solution, and the alkali hydroxide solution, and then
(iv) mixing the nickel salt solution and the reducing agent solution to obtain a nickel salt/reducing agent-containing solution, and
(v) mixing the alkali hydroxide solution and the nickel salt/reducing agent-containing solution.

16. The process for producing nickel powder according to claim 1 , wherein the crystallization step further includes:
(i) preparing:
(1) a nickel salt solution by dissolving at least the water solub

Assignees

• Sumitomo Metal Mining Co

Inventors

• Ishii Junji
• Tanaka Hiroyuki
• Murakami Shingo
• Kumagai Yuki
• Yukinobu Masaya
• Matsumura Yoshiaki

Classifications

• B22F1/145

  Chemical treatment, e.g. passivation or decarburisation · CPC title

• B22F1/052

  characterised by a mixture of particles of different sizes or by the particle size distribution · CPC title

• B22F1/07

  Metallic powder characterised by particles having a nanoscale microstructure (nanosized particles B22F1/054) · CPC title

• B22F9/002

  amorphous or microcrystalline · CPC title

• B22F9/04

  starting from solid material, e.g. by crushing, grinding or milling ({C22C1/1084 takes precedence}; crushing, grinding or milling, in general, see the relevant subclasses, e.g. B02C) · CPC title