US20200376564A1 - Method for producing nickel powder - Google Patents

Method for producing nickel powder Download PDF

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US20200376564A1
US20200376564A1 US16/954,357 US201816954357A US2020376564A1 US 20200376564 A1 US20200376564 A1 US 20200376564A1 US 201816954357 A US201816954357 A US 201816954357A US 2020376564 A1 US2020376564 A1 US 2020376564A1
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nickel
nickel powder
solution
manufacturing
sulfate
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Shin-ichi Heguri
Kazuyuki Takaishi
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Sumitomo Metal Mining Co Ltd
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Sumitomo Metal Mining Co Ltd
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Assigned to SUMITOMO METAL MINING CO., LTD. reassignment SUMITOMO METAL MINING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HEGURI, SHIN-ICHI, TAKAISHI, KAZUYUKI
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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
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12—Both compacting and sintering
    • B22F3/16—Both compacting and sintering in successive or repeated steps
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
    • C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a method for obtaining a high-purity nickel powder having a low sulfur grade from a nickel sulfate amine complex solution and a briquette obtained by solidifying the nickel powder.
  • the present invention can be applied to a treatment of an intermediate generating solution generated in a step in a nickel hydrometallurgical process.
  • a method for industrially manufacturing a nickel powder using a hydrometallurgical process there is a method for manufacturing a nickel powder by dissolving a raw material in a sulfuric acid solution, then removing impurities, adding ammonia to the obtained nickel sulfate solution to form a nickel amine complex, and supplying a hydrogen gas to the generated nickel sulfate amine complex solution to reduce the nickel.
  • Non Patent Literature 1 describes a nickel powder manufacturing process for adding an iron compound as a seed crystal during a reduction reaction and precipitating nickel on the iron compound.
  • this method has a disadvantage that iron derived from the seed crystal is mixed into a product.
  • Patent Literature 1 discloses a method for providing a nickel powder that is inexpensive, has excellent weather resistance, has a low electric resistance in a state of being kneaded with a resin, reduces an initial electric resistance and an electric resistance during use, can be used stably for a long time, and is suitable as a conductive particle for a conductive paste and a conductive resin, and a method for manufacturing the nickel powder.
  • the nickel powder disclosed in Patent Literature 1 contains 1 to 20% by mass of cobalt and the balance composed of nickel and unavoidable impurities, is formed of secondary particles obtained by aggregating primary particles, and contains 0.8% by mass or less of oxygen. It is stated that cobalt is preferably contained only in a surface layer of the secondary particles, and the cobalt content in the surface layer is preferably 1 to 40% by mass.
  • this nickel powder is to be obtained by the disclosed manufacturing method, cobalt coexists. This method is not suitable, for example, for an application to separate nickel and cobalt from each other when nickel and cobalt coexist as in nickel oxide ore, and to recover nickel and cobalt with high purity and economically.
  • Patent Literature 2 provides a method for manufacturing a metal powder by a liquid phase reduction method. This method has been improved such that particle aggregates are not easily generated.
  • This manufacturing method includes: a first step of preparing an aqueous solution containing metal ions derived from a metal compound by dissolving the metal compound, a reducing agent, a complexing agent, and a dispersant; and a second step of reducing the metal ions with the reducing agent by adjusting the pH of the aqueous solution to precipitate a metal powder.
  • an object is to provide a method for manufacturing, using an industrially inexpensive hydrogen gas, coarse particles of a so-called high-purity nickel powder, containing a small amount of impurities and particularly having a low sulfur grade, from a nickel sulfate amine complex solution using a fine nickel powder.
  • a first aspect of the present invention for solving the above problems provides a method for manufacturing a nickel powder from a nickel sulfate solution, including:
  • a nickel recovery step of repeatedly supplying the recovered nickel powder to either or both of the complexation step (2) and the reduction step (3), adding a sulfurizing agent to the recovered final reduction solution, precipitating nickel sulfide, and subjecting it to solid/liquid separation to generate nickel sulfide and a nickel post-reduction solution;
  • a second aspect of the present invention provides a method for manufacturing a nickel powder, in which sieving the nickel powder recovered in the solid/liquid separation step (4) in the first aspect of the present invention according to a particle size, selecting a nickel powder having a smaller size than a predetermined particle size, and adding the selected nickel powder to either or both of the complexation step (2) and the reduction step (3) as a seed crystal are repeatedly performed to obtain a nickel powder having a larger particle size than the nickel powder as the seed crystal.
  • a third aspect of the present invention provides a method for manufacturing a nickel powder, in which the seed crystal added in either or both of the complexation step (2) and the reduction step (3) in the second aspect of the present invention has an average particle size of 0.1 to 100 ⁇ m.
  • a fourth aspect of the present invention provides a method for manufacturing a nickel powder, in which when the mixed slurry containing a nickel sulfate amine complex solution, a seed crystal, and nickel hydroxide is formed in the complexation step (2) in the first to third aspects of the present invention, a dispersant is further added to the mixed slurry.
  • a fifth aspect of the present invention provides a method for manufacturing a nickel powder, in which the seed crystal is added in an amount of 1 to 100% with respect to the weight of nickel in the nickel sulfate amine complex solution in the complexation step (2) in the first to fourth aspects of the present invention.
  • a sixth aspect of the present invention provides a method for manufacturing a nickel powder, in which the reduced slurry in the first to fifth aspects of the present invention is sieved, and the sieved nickel powder and the sieved reduced slurry as a final reduction solution are repeatedly used as a part of the final reduction solution and the nickel powder as a seed crystal in the complexation step (2).
  • a seventh aspect of the present invention provides a method for manufacturing a nickel powder, in which the complexation step (2) in the sixth aspect of the present invention includes two steps of a dissolving step of adding a final reduction solution to obtain a nickel sulfate amine complex solution, and a seed crystal adding step of adding a nickel powder or a mixed slurry containing a nickel powder and a final reduction solution.
  • An eighth aspect of the present invention provides a method for manufacturing a nickel powder, in which the nickel sulfate solution in the first aspect of the present invention is obtained by dissolving at least one selected from a mixed sulfide of nickel and cobalt recovered by leaching nickel oxide ore, nickel sulfide, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, and a nickel metal powder, in a sulfuric acid acidic solution.
  • a ninth aspect of the present invention provides a method for manufacturing a nickel powder, in which the nickel sulfate solution in the first aspect of the present invention is obtained through a leaching step of dissolving a nickel-containing material containing cobalt as impurities, and a solvent extraction step of adjusting the 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 recovery solution by a solvent extraction method.
  • a tenth aspect of the present invention provides a method for manufacturing a nickel powder, in which the ammonium sulfate concentration in the nickel sulfate amine complex solution in the first aspect of the present invention is 100 to 500 g/L, and the ammonium concentration is 1.9 or more in a molar ratio with respect to the nickel concentration in the complex solution.
  • An eleventh aspect of the present invention provides a method for manufacturing a nickel powder, in which blowing of a hydrogen gas is performed, while the temperature is maintained in a range of 100 to 200° C. and the pressure is maintained in a range of 0.8 to 4.0 MPa in the reduction step (3) in the first aspect of the present invention.
  • a twelfth aspect of the present invention provides a method for manufacturing a nickel powder, in which the dispersant in the fourth aspect of the present invention contains a polyacrylate.
  • a thirteenth aspect of the present invention provides a method for manufacturing a nickel powder, further including: a nickel powder briquetting step of processing the nickel powder obtained through the reduction step (3) in the first aspect of the present invention into a massive nickel briquette using a briquetting machine; and a briquette sintering step of sintering the obtained massive nickel briquette in a hydrogen atmosphere under a holding condition of a temperature of 500 to 1200° C. to form a nickel briquette as a sintered body.
  • a fourteenth aspect of the present invention provides a method for manufacturing a nickel powder, further including an ammonium sulfate recovery step of concentrating the final reduction solution in the solid/liquid separation step (4) in the first aspect of the present invention, crystallizing ammonium sulfate, and recovering an ammonium sulfate crystal.
  • a fifteenth aspect of the present invention provides a method for manufacturing a nickel powder, further including an ammonia recovery step of adding an alkali to the final reduction solution in the solid/liquid separation step (4) in the first aspect of the present invention, heating the resulting mixture, volatilizing an ammonia gas, and recovering ammonia.
  • the present invention provides a method for manufacturing a nickel powder from a nickel sulfate amine complex solution using a hydrogen gas, in which a high-purity nickel powder with a small amount of impurities can be easily obtained, and an industrially remarkable effect is exhibited.
  • FIG. 1 is a flowchart for manufacturing a nickel powder according to the present invention.
  • the present invention provides a method for manufacturing a nickel powder from a nickel sulfate amine complex solution, in which by subjecting a process liquid in a hydrometallurgical process to the following steps (1) to (6), a high-purity nickel powder with a smaller amount of impurities is manufactured from a nickel amine sulfate complex solution.
  • a leaching step is for dissolving, with a sulfuric acid, one selected from the group consisting of a mixed sulfide of nickel and cobalt, crude nickel sulfate, nickel oxide, nickel hydroxide, nickel carbonate, a nickel powder, and the like which are starting raw materials, or a nickel-containing material such as an industrial intermediate containing a mixture of a plurality of substances, and for leaching nickel to generate a leachate (a sulfuric acid solution containing nickel).
  • This leaching step is performed by a known method disclosed in JP 2005-350766 A or the like.
  • the pH of the leachate is adjusted, and the leachate is subjected to a solvent extraction step.
  • the leachate adjusted in pH after being obtained in the leaching step is brought into contact with an organic phase, and the components in the phases are exchanged to increase the concentration of a certain component in the aqueous phase and to decrease the concentration of another component.
  • an impurity element in the leachate, particularly cobalt is selectively extracted as a cobalt recovery solution to obtain a nickel sulfate solution having a low cobalt concentration.
  • ammonia water used for pH adjustment in this step ammonia water generated in an ammonia recovery step described later can also be used.
  • an alkali is added to a nickel sulfate solution obtained, for example, through the above-described steps to generate a precipitate of nickel hydroxide, and the precipitate as a solid component and a liquid component are separated from each other.
  • alkali to be added it is preferable to use one that can be prepared industrially at low cost and in large quantities, such as sodium hydroxide or calcium hydroxide.
  • This complexation step specifically includes two steps of a dissolving step and a seed crystal adding step.
  • a dissolving step to nickel hydroxide which is the precipitate obtained in the hydroxylation step (1), ammonia in a form of a final reduction solution obtained by solid/liquid separation of the reduced slurry obtained in the reduction step (3) is added to form a mixed solution of nickel hydroxide and the final reduction solution.
  • the mixed solution is thereby subjected to a complexation treatment to generate a nickel sulfate amine complex which is an amine complex of nickel, and thus forming a nickel amine complex solution.
  • an ammonia concentration can be adjusted by adding an ammonia gas or ammonia water.
  • ammonia is added such that the ammonia concentration is 1.9 or more in a molar ratio with respect to a nickel concentration in the solution.
  • the ammonium concentration of ammonia added is less than 1.9, nickel does not form an amine complex, and a precipitate of nickel hydroxide is generated.
  • ammonium sulfate in order to adjust an ammonium sulfate concentration, ammonium sulfate can be added in this step.
  • the ammonium sulfate concentration is preferably 100 to 500 g/L.
  • the ammonium sulfate concentration exceeds 500 g/L, the ammonium sulfate concentration exceeds a solubility, and crystals are precipitated. It is difficult to attain that the ammonium sulfate concentration is less than 100 g/L due to a metal balance in the process.
  • ammonia gas or the ammonia water used in this step an ammonia gas or ammonia water generated in an ammonia recovery step described later can be used.
  • a seed crystal adding step is performed in which a nickel powder having an average particle size of 0.1 to 100 ⁇ m is added as a seed crystal in a form of a nickel powder slurry to the generated nickel sulfate amine complex solution to form a mixed slurry containing the seed crystal, the nickel sulfate amine complex solution, and nickel hydroxide.
  • the weight of the seed crystal added at this time is preferably 1 to 100% with respect to the weight of nickel in the nickel sulfate amine complex solution.
  • reaction efficiency is significantly reduced at the time of reduction in a subsequent step.
  • the above ratio exceeds 100%, the amount used is large, and manufacture of the seed crystal is costly and not economical.
  • a dispersant may be added at the same time. Since the seed crystals are dispersed by adding the dispersant, the efficiency can be increased in a subsequent reduction step.
  • the dispersant used here is not particularly limited as long as containing a sulfonate, but a lignin sulfonate is preferable because the lignin sulfonate can be obtained industrially at low cost.
  • a hydrogen gas is blown into the obtained mixed slurry, a nickel component in the solution is reduced, and the nickel component is precipitated on the seed crystal to form a reduced slurry containing a nickel powder.
  • the reaction temperature is preferably 100 to 200° C.
  • the temperature is lower than 100° C., more preferably lower than 150° C., reduction efficiency decreases. Even when the temperature is higher than 200° C., there is no influence on the reaction, and a loss in thermal energy or the like increases.
  • the pressure during the reaction is preferably 0.8 to 4.0 MPa.
  • the pressure is less than 0.8 MPa, reaction efficiency is reduced. Even when the pressure exceeds 4.0 MPa, there is no influence on the reaction, and a loss in hydrogen gas increases.
  • a magnesium ion, a sodium ion, a calcium ion, a sulfate ion, and an ammonium ion are mainly present as impurities, but all of these ions remain in the solution. Therefore, a high-purity nickel powder can be generated.
  • nickel hydroxide in the liquid of the mixed slurry reacts with an ammonium ion generated by the reduction reaction, is dissolved as a nickel amine complex in the solution, and is reduced by reacting with a hydrogen gas to precipitate nickel on the seed crystal.
  • the reduced slurry generated in the previous reduction step (3) is solid/liquid separated to recover a high-purity nickel powder with a small amount of impurities and a final reduction solution.
  • the high-purity nickel powder is repeatedly supplied to the complexation step (2) and/or the reduction step (3), in which the high-purity nickel powder is used as a seed crystal in the complexation step (2), and is used as a nickel powder to be subjected to particle growth in the reduction step (3).
  • the recovered final reduction solution is repeatedly supplied as a substitute for ammonia water in the complexation step (2).
  • a small-sized nickel powder or a nickel powder having a reduced size by grinding or the like is repeatedly supplied as a seed crystal to the complexation step (2).
  • the nickel powder is further added to the nickel sulfate amine complex solution obtained in the complexation step (2).
  • a hydrogen gas is supplied thereto, and nickel is thereby further reduced and precipitated on the high-purity nickel powder. Therefore, the particles can be grown.
  • a high-purity nickel powder having a higher bulk density and a larger particle size can also be generated.
  • the obtained high-purity nickel powder may be processed into a briquette shape which is coarser, hardly oxidized, and easily handled through the following nickel powder briquetting step or briquette firing step.
  • An ammonia recovery step may be further provided.
  • the high-purity nickel powder manufactured by the present invention is dried and then formed into a massive nickel briquette as a product form by a briquetting machine or the like.
  • a substance that does not contaminate a product quality such as water, may be added to the nickel powder as a binder in some cases.
  • the nickel briquette prepared in the briquetting step is roasted and sintered in a hydrogen atmosphere to prepare a briquette sintered body. This treatment increases the strength and removes trace amounts of residual ammonia and sulfur components.
  • the roasting and sintering temperature is preferably 500 to 1200° C. When the temperature is lower than 500° C., sintering is insufficient. Even when the temperature is higher than 1200° C., efficiency hardly changes, and a loss in energy increases.
  • Nickel remains in the final reduction solution generated in the solid/liquid separation step (4).
  • the nickel may be mixed into an ammonium sulfate crystal generated in a subsequent ammonium sulfate recovery step to contaminate the quality of the ammonium sulfate crystal. Therefore, it is necessary to remove the residual nickel in advance.
  • a sulfurizing agent used here may be an industrially used sulfurizing agent such as a hydrogen sulfide gas or sodium hydrogen sulfide, but is preferably a hydrogen sulfide gas in order to further improve the quality of the ammonium sulfate crystal.
  • Nickel sulfide precipitated by adding a sulfurizing agent is solid/liquid separated and recovered. Thereafter, the recovered nickel sulfide can be leached again, and repeatedly supplied to the system.
  • nickel sulfide recovered in the previous nickel recovery step is leached dedicatedly and singly, there are few disadvantages such as impurities, and high efficiency is preferably obtained.
  • nickel sulfide recovered in the previous nickel recovery step is repeatedly supplied to the above [leaching step] as one of the starting raw materials described above, equipment saving can be achieved, which is preferable. Note that a nickel post-reduction solution in the aqueous phase is sent to a subsequent step.
  • the nickel post-reduction solution generated in the above [nickel recovery step] contains ammonium sulfate and ammonia.
  • the solution after reaction is heated and concentrated through an ammonium sulfate recovery step to crystallize ammonium sulfate, and ammonium sulfate can be recovered as an ammonium sulfate crystal.
  • the alkali used here is not particularly limited, but caustic soda, slaked lime, and the like are industrially inexpensive and suitable.
  • ammonia water can be generated, and the obtained ammonia water can be repeatedly used in a step.
  • the nickel hydroxide was added to 1700 ml of a mixed solution of a nickel sulfate solution having a nickel concentration of 30 g/L and an ammonium sulfate solution having an ammonia concentration of 40 g/L together with 12.8 g of nickel powder having an average particle size of 2 ⁇ m as a seed crystal, and the resulting mixture was stirred to prepare a mixed slurry.
  • This mixed slurry was heated to 185° C. while being stirred in an autoclave.
  • a hydrogen gas was blown and supplied into the autoclave such that the pressure in the autoclave became 3.5 MPa to be subjected to the reduction step.
  • the resulting product was subjected to the solid/liquid separation step by filtration, and a nickel powder with particle growth was recovered.
  • the recovered nickel powder had an average particle size of 65 ⁇ m and a recovery amount of 119 g.
  • the recovered nickel powder was washed with pure water, and then the impurity grade of the nickel powder was analyzed.
  • Results thereof are illustrated in Table 1.
  • Mg or Na was not mixed into the nickel powder, and a high-purity nickel powder could be generated.
  • the 116 g of nickel hydroxide was mixed with a nickel sulfate amine complex solution having a nickel concentration of 30 g/L, 232 ml of 25% ammonia water, and 225 g of ammonium sulfate, and pure water was added thereto to prepare 1000 ml of mixed slurry.
  • 20 g of nickel powder having an average particle size of 1 ⁇ m was added as a seed crystal to prepare a mixed slurry.
  • the prepared mixed slurry was heated to 120° C. while being stirred in an autoclave.
  • a hydrogen gas was blown and supplied into the autoclave such that the pressure in the autoclave became 3.5 MPa to perform a nickel powder generation treatment which is a reduction treatment.
  • the reduced slurry obtained after cooling was subjected to the solid/liquid separation treatment by filtration, and a high-purity and small-size nickel powder was recovered.
  • the recovered nickel powder at this time was 70 g.
  • the mixed slurry was heated to 120° C. while being stirred in an autoclave.
  • a hydrogen gas was blown and supplied into the autoclave such that the pressure in the autoclave became 3.5 MPa.
  • Example 1 Using the final reduction solution obtained in the solid/liquid separation step in Example 1 as a part of an ammonia source, a mixed slurry was prepared, subjected to the reduction step under the same conditions as in Example 1, and subjected to the solid/liquid separation step, and a nickel powder with particle growth was recovered. A nickel powder similar to that in Example 1 was recovered.
  • Example 2 To a solution containing a nickel powder prepared under the same conditions as in Example 1, 336 g of nickel sulfate, and 330 g of ammonium sulfate, 191 ml of 25% ammonia water was added, and a total liquid volume was adjusted to 1000 ml. Thereafter, the resulting solution was again subjected to the reduction step under the same conditions as in Example 1 and the solid/liquid separation step to prepare a nickel powder with particle growth. Using the nickel powder thus prepared, the same operation was repeated 10 times to cause particle growth of the nickel powder.
  • the average particle size of the recovered nickel powder was 111 ⁇ m, and the nickel powder caused particle growth so as to be 1.7 times larger than the nickel powder in Example 1.
  • the nickel powder obtained by these repeated operations had a sulfur grade of 0.04%.
  • the amount of each of sodium and magnesium was below a lower quantification limit as in Table 1 above.
  • the obtained nickel powder was heated to 1000° C. in a 2% hydrogen atmosphere and held for 60 minutes.
  • the nickel powder obtained after being thus held had a sulfur grade of 0.008%, and the sulfur grade could be further reduced by roasting.
  • Mg or Na was not mixed into the nickel powder, and a high-purity nickel powder could be generated.
  • nickel hydroxide 75 g was added to a nickel sulfate amine complex solution prepared by mixing 135 g of nickel sulfate hexahydrate, 191 ml of 25% ammonia water, 169 g of ammonium sulfate, and pure water, and pure water was added thereto such that the liquid volume became 1000 ml.
  • 15 g of nickel powder having an average particle size of 1 ⁇ m was added thereto as a seed crystal to prepare a mixed slurry.
  • the mixed slurry was heated to 100° C. while being stirred in an autoclave.
  • a hydrogen gas was supplied into the autoclave such that the pressure in the autoclave became 3.5 MPa to perform a nickel powder generation treatment.
  • Example 6 Using the same mixed slurry as in Example 6, the same operation as in Example 6 was performed under the conditions of a temperature of 100° C. and a pressure in the autoclave of 0.8 MPa. At this time, a nickel reduction ratio was 56%.
  • Example 6 Using the same mixed slurry as in Example 6, the same operation as in Example 6 was performed under the conditions of a temperature of 120° C. and a pressure in the autoclave of 3.5 MPa. At this time, a nickel reduction ratio was 74%.
  • Example 6 Using the same mixed slurry as in Example 6, the same operation as in Example 6 was performed under the conditions of a temperature of 120° C. and a pressure in the autoclave of 2.0 MPa. At this time, a nickel reduction ratio was 74%.
  • Example 6 Using the same mixed slurry as in Example 6, the same operation as in Example 6 was performed under the conditions of a temperature of 120° C. and a pressure in the autoclave of 1.5 MPa. At this time, a nickel reduction ratio was 74%.
  • Example 6 100 3.5 58
  • Example 7 100 0.8 56
  • Example 8 120 3.5 74
  • Example 9 120 2.0 74
  • Example 10 120 1.5 74
  • a nickel powder was prepared under the same conditions as in Example 1 except that without performing the hydroxylation step in Example 1, 7.5 g of nickel powder having an average particle size of 1 ⁇ m was added, as a seed crystal, to a solution prepared by adding 191 ml of 25% ammonia water to a solution containing a nickel sulfate solution containing 75 g of nickel and 330 g of ammonium sulfate, and adjusting the total liquid volume to 1000 ml, to prepare a mixed slurry.
  • the recovered nickel powder was washed with pure water, and then the impurity grade of the nickel powder was analyzed.
  • Example 3 Using the same method as in Comparative Example 1, a nickel powder was prepared without performing the hydroxylation step. The operation was performed on the nickel powder repeatedly 10 times in the same manner as in Example 3 to particle growth. The nickel powder obtained by these repeated operations had a sulfur grade of 0.1%. It was not possible to obtain such a high-purity nickel powder having a sulfur grade of about 0.04% as obtained in Example 3 of the present invention.
  • the final reduction solution was put in an airtight vessel, heated to 60° C., and sulfurated by blowing a hydrogen sulfide gas thereinto in a total volume of 1.0 L while being stirred. Thereafter, the resulting solution was solid/liquid separated to obtain nickel sulfide and a nickel post-reduction solution.
  • the nickel concentration in the obtained nickel post-reduction solution was reduced to 0.01 g/L, and it is found that that most of nickel was recovered as nickel sulfide.

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* Cited by examiner, † Cited by third party
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US20250011898A1 (en) * 2021-11-30 2025-01-09 Umicore A method for iron and copper removal from solution using metallic reagents
US20250066877A1 (en) * 2023-08-25 2025-02-27 Korea Zinc Co., Ltd. All-in-one nickel recovering method for nickel hydroxide recovery from raw materials containing nickel
US12325894B2 (en) 2023-08-25 2025-06-10 Korea Zinc Co., Ltd. All-in-one nickel recovering method for nickel metal recovery from raw materials containing nickel

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4538399A4 (en) * 2023-08-25 2025-11-19 Korea Zinc Co Ltd ALL-IN-ONE NICKEL METALLURGICAL METALLURGICAL METALLING PROCESS FOR NICKEL RECOVERY FROM NICKEL-CONTAINING RAW MATERIALS
KR102789618B1 (ko) * 2023-08-25 2025-04-03 고려아연 주식회사 니켈을 함유하는 원료로부터 니켈을 회수하기 위한 올인원 니켈 제련 방법
CN120513310A (zh) * 2023-08-25 2025-08-19 高丽亚铅株式会社 从含镍原料制备硫酸镍水溶液的方法
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Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA950681A (en) * 1971-06-30 1974-07-09 Donald R. Weir Production of nickel powder from basic nickel carbonate
JP2005240164A (ja) 2004-02-27 2005-09-08 Sumitomo Metal Mining Co Ltd ニッケル粉およびその製造方法
JP4525428B2 (ja) 2004-05-13 2010-08-18 住友金属鉱山株式会社 ニッケル酸化鉱石の湿式製錬方法
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
JP6188222B2 (ja) * 2013-12-26 2017-08-30 日本放送協会 トピック抽出装置、及びプログラム
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
JP6099601B2 (ja) * 2014-02-17 2017-03-22 国立大学法人高知大学 ニッケル粉の製造方法
EP3108987A4 (en) * 2014-02-21 2018-02-07 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
JP6726396B2 (ja) * 2016-02-22 2020-07-22 住友金属鉱山株式会社 ニッケル粉の製造方法
JP6641632B2 (ja) * 2016-03-04 2020-02-05 住友金属鉱山株式会社 ニッケル粉の製造方法
CN107116228B (zh) * 2017-06-20 2019-01-04 中南大学 一种固相还原制备超细镍粉的方法

Cited By (4)

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Publication number Priority date Publication date Assignee Title
US20250011898A1 (en) * 2021-11-30 2025-01-09 Umicore A method for iron and copper removal from solution using metallic reagents
US20250066877A1 (en) * 2023-08-25 2025-02-27 Korea Zinc Co., Ltd. All-in-one nickel recovering method for nickel hydroxide recovery from raw materials containing nickel
US12325894B2 (en) 2023-08-25 2025-06-10 Korea Zinc Co., Ltd. All-in-one nickel recovering method for nickel metal recovery from raw materials containing nickel
US12385108B2 (en) * 2023-08-25 2025-08-12 Korea Zinc Co., Ltd. All-in-one nickel recovering method for nickel hydroxide recovery from raw materials containing nickel

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