WO2017150105A1 - Procédé de production de poudre de nickel - Google Patents

Procédé de production de poudre de nickel Download PDF

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Publication number
WO2017150105A1
WO2017150105A1 PCT/JP2017/004499 JP2017004499W WO2017150105A1 WO 2017150105 A1 WO2017150105 A1 WO 2017150105A1 JP 2017004499 W JP2017004499 W JP 2017004499W WO 2017150105 A1 WO2017150105 A1 WO 2017150105A1
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WO
WIPO (PCT)
Prior art keywords
nickel
mixed slurry
nickel powder
added
powder
Prior art date
Application number
PCT/JP2017/004499
Other languages
English (en)
Japanese (ja)
Inventor
伸一 平郡
佳智 尾崎
修 池田
陽平 工藤
Original Assignee
住友金属鉱山株式会社
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 住友金属鉱山株式会社 filed Critical 住友金属鉱山株式会社
Priority to CN201780013765.0A priority Critical patent/CN108698131A/zh
Priority to CA3016924A priority patent/CA3016924A1/fr
Priority to US16/080,363 priority patent/US20210197266A1/en
Priority to EP17759576.6A priority patent/EP3424625A4/fr
Priority to AU2017227099A priority patent/AU2017227099A1/en
Publication of WO2017150105A1 publication Critical patent/WO2017150105A1/fr
Priority to PH12018501840A priority patent/PH12018501840A1/en

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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 suppressing scaling in a reaction tank in a method for producing nickel powder from a solution containing a nickel sulfate ammine complex.
  • it can be applied to the treatment of an intermediate product solution in a process generated from a wet nickel smelting process.
  • Patent Document 1 As a method for producing a fine nickel powder, an atomizing method in which molten nickel is dispersed in gas or water to obtain a fine powder, or nickel is volatilized and reduced in the gas phase as disclosed in Patent Document 1. A dry method such as a CVD method for obtaining nickel powder is known.
  • Non-Patent Document 1 a method for obtaining nickel powder by supplying hydrogen gas to a nickel sulfate ammine complex solution and reducing nickel ions in the complex solution as shown in Non-Patent Document 1 is industrially inexpensive and useful.
  • a method is used in which a small amount of fine particles called seed crystals coexist, a reducing agent is supplied thereto, and seed crystals are grown to obtain a powder having a predetermined particle size.
  • a so-called scaling is formed in which a part of nickel is deposited not on the seed crystal but on the reaction vessel wall in the apparatus in the reaction tank, which may cause problems such as blockage of piping.
  • the present invention provides a method for suppressing the generation of scaling in the reaction tank and reducing the labor and cost required for removal in the process of producing nickel powder from a solution containing a nickel sulfate ammine complex. It is to provide.
  • the first invention of the present invention for solving the above-mentioned problem is that a seed crystal of 0.3 to 3 times the weight of nickel in the solution is added to a solution containing a nickel sulfate ammine complex.
  • the formed mixed slurry is charged into a reaction tank, and the reaction tank is maintained in a liquid phase part occupied by the mixed slurry and a gas phase part other than the liquid phase part, and then hydrogen gas is added to the mixed slurry.
  • nickel complex ions are reduced to form nickel precipitates, thereby producing a nickel powder.
  • a polyacrylate dispersion agent is added to the mixed slurry in the first invention, and 0.5 to 5% is added to the seed crystal weight of the seed crystal added to the mixed slurry. This is a method for producing nickel powder.
  • a solution containing a nickel sulfate ammine complex is added to the nickel deposits in the first and second inventions, hydrogen gas is blown, and nickel is deposited and grown on the nickel deposits. This is a method for producing nickel powder.
  • a method for producing nickel powder characterized in that the temperature of the mixed slurry when hydrogen gas is blown into the mixed slurry according to the first to third aspects is 150 to 200 ° C. It is.
  • the pressure in the gas phase portion in the reaction vessel when hydrogen gas is blown into the mixed slurry in the first to fourth aspects is in the range of 1.0 to 4.0 MPa. This is a method for producing nickel powder.
  • the occurrence of scaling can be suppressed. Therefore, the frequency of descaling is reduced, and labor and cost can be saved.
  • the present invention is a method for producing nickel powder characterized by producing nickel powder by adding seed crystals to a nickel sulfate ammine complex solution and blowing hydrogen gas.
  • the manufacturing method of the nickel powder of this invention is demonstrated.
  • the nickel sulfate ammine complex solution used in the present invention is not particularly limited, but one or a mixture selected from nickel and cobalt mixed sulfide, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, nickel powder and the like.
  • nickel-containing materials such as industrial intermediates
  • nickel leaching solution solution containing nickel
  • a solution obtained by adding ammonia to a solution obtained by removing impurity elements from the solution to form a nickel sulfate ammine complex solution is suitable.
  • seed crystals are added to the nickel sulfate ammine complex solution to form a mixed slurry.
  • the seed crystal added here is preferably a powder having a particle size of 20 ⁇ m or less, and nickel powder is suitable as a substance that does not contaminate the final nickel deposit.
  • the nickel powder used as the seed crystal can be produced, for example, by adding a reducing agent such as hydrazine to the nickel sulfate ammine complex solution.
  • the weight of the seed crystal added here is preferably 0.3 to 3 times the weight of nickel in the solution. If the amount is less than 0.3 times, the effect of suppressing the scaling cannot be sufficiently obtained, and even if an amount exceeding 3 times is added, the effect is not affected, and the addition is excessive.
  • a dispersant can be added in order to disperse the seed crystals in the mixed slurry.
  • the dispersant used here is not particularly limited as long as it is a polyacrylate, but sodium polyacrylate is preferred as an industrially available product.
  • the amount of the dispersant added is preferably 0.5 to 5% based on the seed crystal weight. If it is less than 0.5%, the dispersion effect cannot be obtained, and even if added over 5%, the dispersion effect is not affected, and the addition is excessive.
  • the slurry formed by adding seed crystals or seed crystals and a dispersing agent is charged into a reaction tank of a high pressure resistant high temperature vessel, and a liquid phase part and a gas phase part occupied by the slurry are formed in the reaction tank. To do. Thereafter, hydrogen gas is blown into the slurry in the reaction tank to reduce nickel complex ions in the solution and deposit nickel on the added seed crystals.
  • the reaction temperature at this time is preferably in the range of 150 to 200 ° C. If it is less than 150 degreeC, reduction efficiency will fall, and even if it is 200 degreeC or more, there is no influence on reaction, rather, since loss, such as a heat energy, increases, it is not suitable.
  • the pressure in the gas phase part of the reaction tank during the reaction is preferably 1.0 to 4.0 MPa. If it is less than 1.0 MPa, the reaction efficiency decreases, and even if it exceeds 4.0 MPa, there is no influence on the reaction, and the loss of hydrogen gas increases.
  • nickel precipitates are formed on the seed crystals, and nickel can be extracted and recovered from the solution as fine powdery precipitates by the effect of the dispersant.
  • the nickel powder produced as described above can be used, for example, as a nickel paste, which is an internal constituent material of a multilayer ceramic capacitor.
  • the above-mentioned hydrogen reduction is repeated to grow particles to produce high-purity nickel metal. can do.
  • the reducing slurry in the inner cylinder can was filtered to recover nickel powder.
  • a nickel sulfate solution containing 75 g of nickel, a solution containing 330 g of ammonium sulfate, and 191 ml of 25% aqueous ammonia were added to the collected nickel deposits to prepare a mixed slurry adjusted to a total liquid volume of 1000 ml.
  • the adjusted mixed slurry was reacted in an autoclave in the same manner as described above, and the operation of reacting the recovered nickel precipitates again in the above manner was repeated to grow nickel powder.
  • the reduced slurry in the inner cylinder can was taken out and dried, and the weight of the inner cylinder can was measured to measure the change in weight before and after the reaction.
  • the results are shown in FIG. 1 (see legend 22.5g).
  • the “number of repetitions” when the seed crystal nickel powder is 22.5 g (addition ratio 30%), it is understood that the change in weight is small and the occurrence of scaling can be suppressed.
  • Nickel powder was grown under the same conditions as in Example 1 except that 225 g of nickel powder as a seed crystal was added, which was 3.0 times the weight of nickel in the mixed solution. The result was similar to that of Example 1, and the weight of the generated scaling was 20 g or less each time even when the number of repetitions was increased.
  • Example 2 The growth was repeated in the same manner as in Example 1 except that 7.5 g of 1 ⁇ m nickel powder (addition ratio 10%) and 0.1 g of sodium polyacrylate (42% solution) were added initially. As a result, as shown in FIG. 1 (refer to legend 7.5g), it can be seen that a large increase in the amount of scaling was observed in the second repeated reaction, and the trend continued thereafter.

Abstract

L'invention concerne un procédé de production de poudre de nickel à partir d'une solution contenant un complexe d'ammine et de sulfate de nickel, le procédé selon l'invention permettant de supprimer les dépôts dans un réacteur et de réduire le temps et le coût consacrés à leur élimination. Ce procédé de production de poudre de nickel est caractérisé en ce que, dans une solution contenant un complexe d'ammine et de sulfate de nickel, un germe cristallin est ajouté à raison de 0,3 à 3 fois le poids de nickel dans la solution pour former une suspension épaisse mélangée, un gaz contenant de l'hydrogène est soufflé dans la suspension épaisse mélangée et les ions du complexe de nickel sont réduits pour former un précipité de nickel.
PCT/JP2017/004499 2016-02-29 2017-02-08 Procédé de production de poudre de nickel WO2017150105A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
CN201780013765.0A CN108698131A (zh) 2016-02-29 2017-02-08 镍粉的制造方法
CA3016924A CA3016924A1 (fr) 2016-02-29 2017-02-08 Procede de production de poudre de nickel
US16/080,363 US20210197266A1 (en) 2016-02-29 2017-02-08 Method for producing nickel powder
EP17759576.6A EP3424625A4 (fr) 2016-02-29 2017-02-08 Procédé de production de poudre de nickel
AU2017227099A AU2017227099A1 (en) 2016-02-29 2017-02-08 Nickel powder production method
PH12018501840A PH12018501840A1 (en) 2016-02-29 2018-08-29 Method for producing nickel powder

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
JP2016-038185 2016-02-29

Publications (1)

Publication Number Publication Date
WO2017150105A1 true WO2017150105A1 (fr) 2017-09-08

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Application Number Title Priority Date Filing Date
PCT/JP2017/004499 WO2017150105A1 (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

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005505695A (ja) 2001-10-18 2005-02-24 カナディアン・エレクトロニック・パウダーズ・コーポレーション・（シーイーピーシー） 積層セラミックコンデンサ電極内部用粉末
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
JP2010242143A (ja) 2009-04-02 2010-10-28 Sumitomo Electric Ind Ltd 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
JP2015166489A (ja) * 2014-02-17 2015-09-24 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
JP2016033255A (ja) * 2014-03-26 2016-03-10 国立大学法人高知大学 ニッケル粉の製造方法

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Publication number Priority date Publication date Assignee Title
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
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
US10471514B2 (en) * 2014-02-21 2019-11-12 Kochi University, National University Corporation Method for producing nickel powder
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005505695A (ja) 2001-10-18 2005-02-24 カナディアン・エレクトロニック・パウダーズ・コーポレーション・（シーイーピーシー） 積層セラミックコンデンサ電極内部用粉末
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
JP2010242143A (ja) 2009-04-02 2010-10-28 Sumitomo Electric Ind Ltd 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
JP2015166489A (ja) * 2014-02-17 2015-09-24 国立大学法人高知大学 ニッケル粉の製造方法
JP2016033255A (ja) * 2014-03-26 2016-03-10 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

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"The Manufacture and properties of Metal powder produced by the gaseous reduction of aqueous solutions", POWDER METALLURGY, 1958, pages 40 - 52
See also references of EP3424625A4

Also Published As

Publication number Publication date
AU2017227099A1 (en) 2018-09-13
EP3424625A4 (fr) 2019-11-20
JP2017155265A (ja) 2017-09-07
US20210197266A1 (en) 2021-07-01
CN108698131A (zh) 2018-10-23
EP3424625A1 (fr) 2019-01-09
PH12018501840A1 (en) 2019-05-15
CA3016924A1 (fr) 2017-09-08

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