EP3424625A1 - Procédé de production de poudre de nickel - Google Patents

Procédé de production de poudre de nickel Download PDF

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Publication number
EP3424625A1
EP3424625A1 EP17759576.6A EP17759576A EP3424625A1 EP 3424625 A1 EP3424625 A1 EP 3424625A1 EP 17759576 A EP17759576 A EP 17759576A EP 3424625 A1 EP3424625 A1 EP 3424625A1
Authority
EP
European Patent Office
Prior art keywords
nickel
slurry
nickel powder
solution
hydrogen gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP17759576.6A
Other languages
German (de)
English (en)
Other versions
EP3424625A4 (fr
Inventor
Shin-ichi HEGURI
Yoshitomo Ozaki
Osamu Ikeda
Yohei Kudo
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sumitomo Metal Mining Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Publication of EP3424625A1 publication Critical patent/EP3424625A1/fr
Publication of EP3424625A4 publication Critical patent/EP3424625A4/fr
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/01—Reducing atmosphere
    • B22F2201/013—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2301/00—Metallic composition of the powder or its coating
    • B22F2301/15—Nickel or cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2304/00—Physical aspects of the powder
    • B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention relates to a method for controlling scaling in a reaction vessel in a method for producing nickel powder from a solution containing a nickel ammine sulfate complex.
  • the present invention can be applied to a treatment of an in-process intermediate solution generated from a nickel hydrometallurgical process.
  • Methods for producing fine nickel powder have been known including atomization methods of dispersing molten nickel in gas or water to obtain fine powder, and dry processes, such as CVD processes, of volatilizing nickel, and reducing the nickel in a gaseous phase to obtain nickel powder as described in Patent Literature 1.
  • Methods for producing nickel powder by a wet process include a method of producing nickel powder using a reducing agent as described in Patent Literature 2, and an atomization thermal decomposition method of atomizing a nickel solution in a reduction atmosphere at a high temperature to obtain a nickel powder through a thermal decomposition reaction as described in Patent Literature 3.
  • Non Patent Literature 1 a method as described in Non Patent Literature 1 is industrially inexpensive and useful, in which hydrogen gas is fed to a nickel ammine sulfate complex solution to reduce nickel ions in the complex solution, obtaining a nickel powder.
  • This method involves the following process: a small amount of fine particles called seed crystals is added, and a reducing agent is fed thereto to grow the seed crystals into a powder having a predetermined particle size.
  • a reducing agent is fed thereto to grow the seed crystals into a powder having a predetermined particle size.
  • the so-called scaling which is part of nickel precipitated on the walls of the reaction container in the apparatus rather than on the seed crystals, may be formed in the reaction vessel, causing failure such as clogging of the pipes.
  • Non Patent Literature 1 " The Manufacture and properties of Metal powder produced by the gaseous reduction of aqueous solutions", Powder metallurgy, No. 1/2 (1958), pp. 40-52 .
  • the present invention provides a method for controlling the generation of scaling in a reaction vessel to reduce time and cost required for removal of the scaling in the process of producing nickel powder from a solution containing a nickel ammine sulfate complex.
  • a first aspect of the present invention to solve the above problem is a method for producing nickel powder, including: adding, to a solution containing a nickel ammine sulfate complex, seed crystals in an amount of 0.3 times or more and 3 times or less the weight of nickel in the solution to form a slurry; charging the slurry into a reaction vessel, maintaining a liquid phase portion occupied by the slurry and a gaseous phase portion other than the liquid phase portion within the reaction vessel; and blowing hydrogen gas into the slurry to reduce a nickel complex ion and to thereby form a nickel precipitate.
  • a second aspect of the present invention is a method for producing nickel powder, wherein of a polyacrylate salt dispersant is added to the slurry according to the first aspect in an amount of 0.5 to 5% based on the weight of the seed crystals added to the slurry.
  • a third aspect of the present invention is a method for producing nickel powder, wherein a solution containing a nickel ammine sulfate complex is added to the nickel precipitate according to the first and second aspects, and hydrogen gas is blown thereinto to precipitate and grow nickel on the nickel precipitate.
  • a fourth aspect of the present invention is a method for producing nickel powder, wherein the temperature of the slurry is 150 to 200°C when hydrogen gas is blown into the slurry according to the first to third aspects.
  • a fifth aspect of the present invention is a method for producing nickel powder, wherein the pressure of the gaseous phase portion in the reaction vessel is in the range of 1.0 to 4.0 MPa when hydrogen gas is blown into the slurry according to the first to fourth aspects.
  • the present invention can control the generation of scaling. For this reason, the frequency of removal of scale can be reduced, resulting in a reduction in time and cost.
  • FIG. 1 This is a diagram illustrating a relation between the amount of nickel powder to be added, the number of repetitions, and the amount of scaling generated.
  • the present invention is a method for producing nickel powder by adding seed crystals to a nickel ammine sulfate complex solution, and blowing hydrogen gas thereinto to produce a nickel powder.
  • a nickel ammine sulfate complex solution that can be used in the present invention is not particularly limited, but it is suitable to use a nickel ammine sulfate complex solution obtained by dissolving a nickel-containing material, such as an industrial intermediate including one or a mixture of two or more selected from nickel and cobalt mixed sulfide, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, and nickel powder, with sulfuric acid or ammonia to prepare a nickel-containing leachate (solution containing nickel), subjecting the nickel-containing leachate to a liquid-purification step such as solvent extraction, ion exchange, or neutralization to remove impurity elements in the solution, and adding ammonia to the resulting solution.
  • a nickel-containing material such as an industrial intermediate including one or a mixture of two or more selected from nickel and cobalt mixed sulfide, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, and nickel powder
  • sulfuric acid or ammonia to prepare
  • seed crystals are added to the nickel ammine sulfate complex solution to prepare a slurry.
  • the seed crystals added here are preferably a powder having a particle size of 20 ⁇ m or less.
  • a nickel powder is suitable as a substance which does not contaminate the final nickel precipitate.
  • the nickel powder used as the seed crystals can be prepared, for example, by adding a reducing agent such as hydrazine to the nickel ammine sulfate complex solution.
  • the weight of the seed crystals added here is preferably 0.3 times or more and 3 times or less the weight of nickel in the solution. An amount of less than 0.3 times the weight of nickel in the solution cannot achieve a sufficient effect of reducing scaling. An amount of more than 3 times has no influences over the effect; rather, this results in addition of excess crystal seeds.
  • a dispersant may be added to disperse the seed crystals in the slurry.
  • a dispersant used here is not particularly limited as long as it has polyacrylate salt, but sodium polyacrylate, which is industrially available at low cost, is preferable.
  • the amount of the dispersant to be added is preferably 0.5 to 5% based on the weight of the seed crystals. An amount of less than 0.5% cannot achieve the dispersion effect. An amount of more than 5% has no influences over the dispersion effect; rather, this results in addition of an excess dispersant.
  • the slurry prepared by the addition of the seed crystals or the seed crystals and the dispersant is charged into a reaction vessel in a container resistant to high pressure and high temperature, forming a liquid phase portion occupied by the slurry and a gaseous phase portion in the reaction vessel. Subsequently, hydrogen gas is blown into the slurry in the reaction vessel to reduce a nickel complex ion in the solution and precipitate nickel on the seed crystals added.
  • the reaction temperature is preferably in the range of 150 to 200°C.
  • a reaction temperature of less than 150°C reduces the efficiency of reduction.
  • a reaction temperature of 200°C or more has no influences over the reaction; rather, such a reaction temperature increases loss of thermal energy, and is not suitable.
  • the pressure of the gaseous phase portion in the reaction vessel during the reaction is preferably 1.0 to 4.0 MPa. If the pressure is less than 1.0 MPa, reaction efficiency will be reduced, and even if the pressure exceeds 4.0 MPa, there will be no influence on the reaction, and the loss of hydrogen gas will increase.
  • a precipitate of nickel is formed on the seed crystals through the reduction and the precipitation treatment under such conditions so that nickel can be extracted and recovered from the solution in the form of a fine powdery precipitate by the effect of the dispersant.
  • the nickel powder thus produced can be used in, for example, an application to nickel pastes as an inner constitutional substance for stacked ceramic capacitors. Besides, particles of the nickel powder can be grown through repetition of the above hydrogen reduction to produce high purity nickel metal.
  • the resulting slurry was then charged into an internal cylindrical can of an autoclave used as a reaction vessel to define a liquid phase portion and a gaseous phase portion.
  • the slurry was heated to and held at 185°C with stirring.
  • hydrogen gas was blown and fed into the slurry so that the pressure of the gaseous phase portion in the internal cylindrical can of the autoclave became 3.5 MPa, to perform a reduction treatment. Thereby, a reduced slurry was generated.
  • the feed of hydrogen gas was stopped, and the internal cylindrical can was cooled.
  • the reduced slurry in the internal cylindrical can was filtered to recover nickel powder.
  • a nickel sulfate solution containing nickel equivalent to 75 g, a solution containing 330 g of ammonium sulfate, and 191 ml of 25% aqueous ammonia were added and the total amount of the solution was adjusted to 1000 ml to prepare an adjusted slurry.
  • the adjusted slurry was reacted in the autoclave in the same manner as described above, and a thus recovered nickel precipitate was again reacted in the manner described above. This operation was repeated to grow nickel powder.
  • the reduced slurry in the internal cylindrical can was extracted, and was dried.
  • the weight of the internal cylindrical can was measured to measure a change in weight before and after the reaction.
  • the change in weight is small according to "the number of repetitions" and the generation of scaling can be reduced.
  • a nickel powder was grown under the same condition as in Example 1 except that the nickel powder as seed crystals was added in an amount of 3.0 times the weight of nickel in the mixed solution, i.e., 225 g.
  • Example 2 The results similar to those in Example 1 were obtained. Even if the number of repetitions was increased, the weight of scaling generated was 20 g or less each time.
  • the growth was repeatedly performed in the same manner as in Example 1 except that initially 15.0 g of 1 ⁇ m nickel powder (proportion of addition: 20%) and 0.3 g of sodium polyacrylate (42% solution) were added.
  • Example 2 The growth was repeatedly performed in the same manner as in Example 1 except that initially 7.5 g of 1 ⁇ m nickel powder (proportion of addition: 10%) and 0.1 g of sodium polyacrylate (42% solution) were added.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
EP17759576.6A 2016-02-29 2017-02-08 Procédé de production de poudre de nickel Withdrawn EP3424625A4 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2016038185A JP2017155265A (ja) 2016-02-29 2016-02-29 ニッケル粉の製造方法
PCT/JP2017/004499 WO2017150105A1 (fr) 2016-02-29 2017-02-08 Procédé de production de poudre de nickel

Publications (2)

Publication Number Publication Date
EP3424625A1 true EP3424625A1 (fr) 2019-01-09
EP3424625A4 EP3424625A4 (fr) 2019-11-20

Family

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EP17759576.6A Withdrawn EP3424625A4 (fr) 2016-02-29 2017-02-08 Procédé de production de poudre de nickel

Country Status (8)

Country Link
US (1) US20210197266A1 (fr)
EP (1) EP3424625A4 (fr)
JP (1) JP2017155265A (fr)
CN (1) CN108698131A (fr)
AU (1) AU2017227099A1 (fr)
CA (1) CA3016924A1 (fr)
PH (1) PH12018501840A1 (fr)
WO (1) WO2017150105A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP7007650B2 (ja) * 2018-07-31 2022-01-24 住友金属鉱山株式会社 ニッケル粉の製造方法

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2359347A1 (fr) 2001-10-18 2003-04-18 Cesur Celik Materiau electrode interne de condensateur en stratifie ceramiqu
JP4286220B2 (ja) 2002-08-28 2009-06-24 東邦チタニウム株式会社 金属ニッケル粉末及びその製造方法
JP2009079239A (ja) * 2007-09-25 2009-04-16 Sumitomo Electric Ind Ltd ニッケル粉末、またはニッケルを主成分とする合金粉末およびその製造方法、導電性ペースト、並びに積層セラミックコンデンサ
CN101428349B (zh) * 2008-07-29 2011-06-22 张建玲 一种镍钴金属粉末的制备方法
JP5407495B2 (ja) 2009-04-02 2014-02-05 住友電気工業株式会社 金属粉末および金属粉末製造方法、導電性ペースト、並びに積層セラミックコンデンサ
JP5828923B2 (ja) * 2014-01-30 2015-12-09 国立大学法人高知大学 ニッケル粉の製造方法
JP5881091B2 (ja) * 2014-02-17 2016-03-09 住友金属鉱山株式会社 ニッケル粉の製造方法
JP5936783B2 (ja) * 2014-02-21 2016-06-22 国立大学法人高知大学 ニッケル粉の製造方法
JP6442298B2 (ja) * 2014-03-26 2018-12-19 国立大学法人高知大学 ニッケル粉の製造方法
JP5796696B1 (ja) * 2015-01-22 2015-10-21 住友金属鉱山株式会社 ニッケル粉の製造方法
JP6610425B2 (ja) * 2015-08-31 2019-11-27 住友金属鉱山株式会社 ニッケル粉の製造方法

Also Published As

Publication number Publication date
JP2017155265A (ja) 2017-09-07
CN108698131A (zh) 2018-10-23
US20210197266A1 (en) 2021-07-01
AU2017227099A1 (en) 2018-09-13
EP3424625A4 (fr) 2019-11-20
WO2017150105A1 (fr) 2017-09-08
CA3016924A1 (fr) 2017-09-08
PH12018501840A1 (en) 2019-05-15

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