US20200338641A1 - Method for producing nickel powder - Google Patents

Method for producing nickel powder Download PDF

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US20200338641A1
US20200338641A1 US16/082,004 US201716082004A US2020338641A1 US 20200338641 A1 US20200338641 A1 US 20200338641A1 US 201716082004 A US201716082004 A US 201716082004A US 2020338641 A1 US2020338641 A1 US 2020338641A1
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nickel
nickel powder
reactor
seed crystals
complex solution
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Yoshitomo Ozaki
Shin-ichi Heguri
Kazuyuki Takaishi
Ryo-ma Yamaguma
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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, OZAKI, YOSHITOMO, 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0433—Nickel- or cobalt-based alloys
    • 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
    • B22F2203/00—Controlling
    • B22F2203/11—Controlling temperature, temperature profile
    • 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
    • B22F2203/00—Controlling
    • B22F2203/13—Controlling pressure
    • 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
    • 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

Definitions

  • the present invention relates to a method for obtaining nickel powder from a nickel ammine sulfate complex solution, and specifically relates to a method for continuously adding a solution and hydrogen gas etc., to a high pressure container, and continuously discharging and recovering nickel powder.
  • a method for producing nickel powder disclosed in Japanese Patent Application Laid-Open No. 2015-140480 in which a raw material containing nickel is dissolved in a solution of sulfuric acid, followed by liquid-purification step of removing impurities contained in the dissolution, and thereafter ammonia is added to the resulting nickel sulfate solution to form a nickel ammine complex; and the nickel ammine sulfate complex solution is then placed into a container at high temperature and high pressure, and hydrogen gas is fed to reduce nickel in the nickel ammine sulfate complex solution.
  • batch methods for production are often used from the viewpoint of ease of handling and cost of the apparatus.
  • a series of operation to open the reactor, place the solution, tightly seal the reactor, heat the reactor, control the temperature and the pressure, blow hydrogen gas into the reactor to perform reduction, cool the reactor, and extract the reaction product should be performed at each stage.
  • the batch methods are not efficient because the methods require large amounts of labor and time, reducing the operating rate.
  • influences of heating and/or cooling before and after the reaction cannot be neglected, causing uneven precipitates called scaling or a variation in particle size during the reaction in some cases.
  • uneven nickel powder produced due to mixing of coarse nickel powder is more likely to cause wear or clog of the facility during handling, reducing the operating rate.
  • the influences of uneven nickel powder as well as the labor to remove it result in difficulties in maintaining the operating rate of the reaction and the quality of products at constant levels.
  • Nickel powder obtained by the batch method has a problem about the quality of impurities compared to the electrolytic nickel in the form of a plate (sheet) obtained by standard electrometallurgy. Specifically, the sulfur grade should be 0.01% by weight or less to obtain the certification of high purity grade in an international nickel market London Metal Exchange (LME).
  • the nickel powder obtained by the batch method may have higher sulfur grade than that in the high purity nickel of the LME grade specified in the LME, and are difficult to use in applications where the electrolytic nickel is completely replaced.
  • An object of the present invention provides a method for continuously feeding a solution, seed crystals, and hydrogen gas into a reactor kept at high temperature and high pressure to produce nickel powder, and continuously discharging and recovering the produced powder, whereby a fine nickel powder with high purity can be sufficiently grown, a variation in particle size can be reduced to maintain the quality of the nickel powder, and a high operating rate of the reaction can be maintained.
  • a first aspect of the invention relates to a method of producing nickel powder, where the method includes the steps of feeding a nickel ammine sulfate complex solution and seed crystals into a reactor, and feeding hydrogen gas into the reactor to subject a nickel complex ion in the nickel ammine sulfate complex solution to a reduction treatment and to thereby produce nickel powder having a sulfur grade of lower than 0.01% by weight, wherein, in the reduction treatment, while the nickel ammine sulfate complex solution containing polyacrylic acid in a concentration of 0.5 to 1.0 g/liter is being continuously fed into the reactor, a temperature inside the reactor is controlled within the range of 150° C. or more and 185° C.
  • the feed rate of hydrogen gas is controlled to maintain an inner pressure of the reactor in the range of 2.5 to 3.5 MPa to produce a nickel powder slurry containing the nickel powder, and thereafter, when the nickel powder slurry is extracted from the reactor, a feed amount of the nickel ammine sulfate complex solution and the seed crystals and a discharge amount of the nickel powder slurry are adjusted to keep a given amount of the solution in the reactor.
  • a second aspect of the present invention relates to a method of producing nickel powder, where the method includes the steps of feeding hydrogen gas into a reactor, and feeding a nickel ammine sulfate complex solution and seed crystals into the reactor to subject a nickel complex ion in the nickel ammine sulfate complex solution to a reduction treatment and to thereby produce nickel powder having a sulfur grade of lower than 0.01% by weight, wherein, in the reduction treatment, the nickel complex ion in the nickel ammine sulfate complex solution is reduced in such a manner that a slurry containing ammonium sulfate and nickel powder are stored in the reactor to form a liquid phase portion and a gaseous phase portion in the reactor and an inner pressure of the gaseous phase portion is controlled through the feeding of the hydrogen gas into the reactor, a slurry containing seed crystals and the nickel ammine sulfate complex solution containing polyacrylic acid in a concentration of 0.5 to 1.0 g/liter are continuously fed into the liquid phase portion, a temperature
  • the feed rate of the hydrogen gas is controlled to maintain an inner pressure of the reactor in the range of 2.5 to 3.5 MPa, to produce a nickel powder slurry containing the nickel powder, and thereafter, when the nickel powder slurry is extracted from the reactor, a feed amount of the nickel ammine sulfate complex solution and the seed crystals and a discharge amount of the nickel powder slurry are adjusted to keep a given amount of the solution in the reactor.
  • Nickel powder having an average particle size in the range of 0.1 to 100 ⁇ m may be used as the seed crystals according to the first aspect of the invention or the second aspect of the invention.
  • Nickel powder having an average particle size in the range of 0.1 to 10 ⁇ m may be used as the seed crystals according to the first aspect of the invention or the second aspect of the invention.
  • the amount of the seed crystals to be added according to the above-described aspects may be in the range of 1 to 100% by weight based on the weight of nickel contained in the nickel ammine sulfate complex solution.
  • the nickel ammine sulfate complex solution that is subjected to the reduction treatment may contain polyacrylic acid in an amount in the range of 0.5 to 5% by weight based on the weight of the seed crystals in the nickel ammine sulfate complex solution.
  • the reduction treatment according to the invention may include continuously feeding into the reactor the nickel ammine sulfate complex solution containing the seed crystals such that the reaction time of the reduction treatment in the reactor takes 5 minutes or more and 120 minutes or less.
  • a nickel precipitate can be formed on seed crystals and a grown nickel powder can be formed thereon through the repeated reduction treatment with the precipitation of nickel.
  • nickel powder having a little variation in size can be continuously obtained.
  • the nickel powder having lower sulfur grade can be extracted and recovered from the solution in the form of fine powdery precipitate. Furthermore, a coarse nickel powder having a spherical shape and a smooth surface can also be obtained depending on the combination of the particle size of the nickel powder and the concentration of the dispersant.
  • the nickel powder produced in the present invention can be used in applications of nickel pastes as an inner constitutional substance of stacked ceramic capacitors.
  • This production method can grow particles through repetition of the reduction treatment with hydrogen to obtain a high purity nickel metal of high quality while maintaining a high operating rate of the reaction. This method attains an industrially remarkable effect.
  • FIG. 1 This illustrates an optical microscope photograph ( ⁇ 50) of the nickel powder according to Example 1 of the present invention.
  • FIG. 2 This illustrates an optical microscope photograph ( ⁇ 100) of the nickel powder according to Example 2 of the present invention.
  • FIG. 3 This illustrates an SEM photograph ( ⁇ 1000) of the nickel powder according to Example 3 of the present invention.
  • FIG. 4 This illustrates an SEM photograph ( ⁇ 500) of the nickel powder according to Example 4 of the present invention.
  • FIG. 5 This illustrates an optical microscope photograph 5 A ( ⁇ 50) and 5 B its enlarged photograph ( ⁇ 100) of the nickel powder according to Example 4 of the present invention.
  • the present invention is a method for producing nickel powder including: producing nickel powder through a reduction treatment with hydrogen gas blown into a reactor as a pressurized container while adding seed crystals to a nickel ammine sulfate complex solution and continuously feeding the seed crystals; and continuously discharging the nickel powder from the pressurized container. Moreover, a high purity, uniform fine nickel powder having lower sulfur grade can be obtained by using a dispersant.
  • 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 form a slurry, which is subjected to the reduction treatment.
  • the seed crystals added here are powder having an average particle size of preferably 0.1 ⁇ m or more and 100 ⁇ m or less, more preferably 0.1 ⁇ m or more and 10 ⁇ m or less.
  • Nickel powder is suitably used as a substance which does not become impurities in the final nickel precipitate to contaminate the precipitate.
  • the nickel powder used as the seed crystals can be prepared through addition of a reducing agent such as hydrazine to the nickel ammine sulfate complex solution, for example.
  • the weight of the seed crystals to be added is preferably 1% by weight or more and 100% by weight or less based on the weight of the nickel in the nickel ammine sulfate complex solution.
  • a content of less than 1% by weight cannot sufficiently achieve the effect of reducing uneven precipitation.
  • a content of more than 100% by weight has no influences over the effect; rather, it results in excess addition of the seed crystals.
  • a dispersant may also be then added to disperse the seed crystals in the slurry.
  • Any polyacrylate dispersant can be used without particular limitation. Suitable is sodium polyacrylate because it is industrially available at low cost.
  • the amount thereof to be added is suitably in the range of 0.5 to 5% by weight based on the weight of the seed crystals.
  • a content of less than 0.5% does not achieve any dispersing effect.
  • a content of more than 5% has no influences over the dispersing effect; rather, such an addition is excess addition of the dispersant.
  • the polyacrylic acid may be added such that the concentration thereof is 0.5 to 1.0 g/liter based on the amount of the nickel ammine sulfate complex solution.
  • the seed crystals added at this time are preferably seed crystals having an average particle size of 0.1 ⁇ m or more and 10 ⁇ m or less.
  • the slurry prepared by adding the seed crystals or the seed crystals and the dispersant in the nickel ammine sulfate complex solution is continuously placed into a reaction vessel of a container resistant to high pressure and high temperature where a slurry containing ammonium sulfate and nickel powder is stored and the inner pressure is controlled with hydrogen gas. Thereby, a liquid phase portion occupied by the slurry and a gaseous phase portion are formed within the reaction vessel.
  • the slurry containing the seed crystals or the slurry containing the seed crystals and the dispersant, and the nickel ammine sulfate complex solution are continuously charged into a reaction vessel of a container resistant to high pressure and high temperature where a slurry containing ammonium sulfate and nickel powder is stored and the inner pressure is controlled with hydrogen gas.
  • a slurry is formed, and a liquid phase portion occupied by the slurry and a gaseous phase portion having an inner pressure controlled with hydrogen gas is formed within the reaction vessel.
  • the nickel complex ion contained in the nickel ammine sulfate complex solution is reduced with hydrogen gas to precipitate nickel on the seed crystals added and grow the nickel precipitate into nickel powder.
  • the nickel powder slurry i.e., the slurry containing the grown nickel powder is simultaneously formed, ant is continuously discharged.
  • the reaction temperature at this time is preferably in the range of 150° C. or more and 185° C. or less.
  • a reaction temperature of less than 150° C. reduces the reduction efficiency.
  • a reaction temperature of more than 185° C. has no influences over the reaction; rather, it is not suitable because it increases loss of thermal energy.
  • the gaseous phase portion of the reaction vessel preferably is under a pressure maintained in the range of 2.5 to 3.5 MPa during the reaction.
  • a pressure of less than 2.5 MPa reduces the reaction efficiency.
  • a pressure of more than 3.5 MPa has no influences over the reaction; rather, it increases loss of hydrogen gas.
  • a reduction treatment accompanied by the precipitation of nickel under such conditions can form a nickel precipitate on seed crystals and thus a grown nickel powder, continuously yielding nickel powder having a little variation in size.
  • nickel having lower sulfur grade can be extracted and recovered from the solution in the form of a fine powdery precipitate.
  • a coarse nickel powder having a spherical shape and a smooth surface can also be yielded depending on the combination of the particle size of the nickel powder and the concentration of the dispersant.
  • the nickel powder produced as described above can be used in applications of nickel pastes as an inner constitutional substance of stacked ceramic capacitors. Besides, particles can be grown through repetition of the reduction with hydrogen to produce fine nickel metal with high purity and uniformity which has a particle size of 20 ⁇ m or less and is suitable for handling.
  • a pressurized container having an inner volume of 190 liter was used as a reaction vessel.
  • a solution slurry (90 liter) containing ammonium sulfate (269 g/L) and nickel powder (100 g/L) was placed into the reaction vessel.
  • the reaction vessel was covered with a lid to maintain the temperature at 185° C. Hydrogen gas was then blown into the reaction vessel to control the pressure to 3.5 MPa.
  • the starting solution containing 150 g/liter of ammonium sulfate and a nickel ammine sulfate complex solution (concentration of nickel: 110 g/L) was added to the pressurized container at a flow rate of 1 liter per minute, and further a nickel seed crystal slurry (concentration of slurry: 300 g/L) was added at a flow rate of 0.25 liter per minute to advance a reduction treatment.
  • the nickel powder used here as the seed crystals forming the nickel seed crystal slurry had an average particle size of 1 ⁇ m. Hydrogen gas was blown into the reaction vessel such that the inner pressure of the pressurized container was maintained at 3.5 MPa.
  • the following operation was continued for four hours: while the amount of the solution stored in the pressurized container was being controlled in the range of 90 liter ⁇ 5 liter, the nickel powder slurry containing the nickel powder produced in the reduction treatment was continuously extracted from the pressurized container.
  • the reaction time in the reduction treatment in the reactor was 75 minutes from the charge of the starting solution and the seed crystal slurry to the extraction of the nickel powder slurry.
  • the extracted nickel powder slurry contained 0.28 g/L of nickel, and the reduction rate (reaction rate), namely, the proportion of hydrogen gas used in the precipitation reaction of the nickel powder was 99.6%.
  • the proportion of particles having a particle size of more than 300 ⁇ m was less than 0.1%
  • the proportion of particles having a particle size of more than 150 ⁇ m and 300 ⁇ m or less was 91%
  • the proportion of particles having a particle diameter of more than 100 ⁇ m and 150 ⁇ m or less was 8.3%
  • the proportion of particles having a particle diameter of more than 75 ⁇ m and 100 ⁇ m or less and the proportion of particles having a particle diameter of more than 45 ⁇ m and 75 ⁇ m or less both were less than 0.1%
  • the proportion of particles having a particle diameter of 45 ⁇ m or less was 0.7%.
  • Example 2 The same reactor as in Example 1 was used. A solution slurry (90 liter) containing ammonium sulfate (205 g/L), polyacrylic acid (concentration: 1 g/L), and nickel powder (concentration: 105 g/L) was placed into the reactor. The reaction vessel was covered with a lid to maintain the inner temperature at 185° C.
  • Hydrogen gas was then blown into the gaseous phase portion in the reactor to control the inner pressure of the container to 3.5 MPa.
  • a starting solution containing a nickel ammine sulfate complex solution (concentration of nickel: 83 g/L) and ammonium sulfate at a concentration of 120 g/L was fed into the reactor at a flow rate of 1 liter per minute, and simultaneously the nickel seed crystal slurry (concentration of slurry: 150 g/L) was continuously fed into the reactor at a flow rate of 0.5 liter per minute to advance the reduction treatment.
  • Nickel powder having an average particle size of 1 ⁇ m was used as the nickel powder forming the nickel seed crystal slurry. Hydrogen gas was blown such that the inner pressure of the reactor was maintained at 3.5 MPa.
  • the slurry subjected to the reduction treatment was continuously extracted. This operation was continued for hours.
  • the extracted slurry subjected to the reduction treatment was subjected to solid liquid separation using a Nutsche funnel into nickel powder and filtrate.
  • the resulting nickel powder was washed, and was vacuum dried.
  • the reaction time in the reduction treatment in the reactor was 60 minutes from the charge of the starting solution and the seed crystal slurry to the extraction of the nickel powder slurry.
  • reaction rate namely, the proportion of hydrogen gas used in the precipitation reaction of the nickel powder was 98.9%.
  • the resulting nickel powder had a finer average particle size D50 of 5.2 ⁇ m but had a less variation in size than those of Example 1 (see FIG. 2 ). Furthermore, the sulfur grade was 0.003%, which indicates that a high purity nickel powder having a low sulfur grade lower than the sulfur quality (0.01%) specified as the LME grade was obtained.
  • a solution (90 liter) containing ammonium sulfate (205 g/L), nickel powder (105 g/L), and polyacrylic acid (1 g/L) was placed into a reactor having the same structure as in Example 1 and having a volume of 90 liter to maintain the temperature at 185° C. Hydrogen gas was blown into the reaction vessel to control the pressure at 3.5 MPa.
  • a starting solution containing a nickel ammine sulfate complex solution (concentration of nickel: 83 g/L) and ammonium sulfate at a concentration of 120 g/L was added to this pressurized container at a rate of 1 liter/min, and simultaneously a nickel seed crystal slurry (slurry content: 150 g/L) was added at a rate of 0.5 liter/min.
  • a nickel seed crystal slurry slurry content: 150 g/L
  • polyacrylic acid at a concentration of 1 g/L was added to the nickel ammine sulfate complex solution in the starting solution, which was fed to the reactor. Hydrogen gas was blown into the pressurized container such that its pressure became 3 . 5 MPa.
  • the extracted nickel powder forming the nickel powder slurry had an average particle size of 5.9 ⁇ m.
  • the nickel powder slurry was continuously extracted. This operation was continued for 12 hours.
  • the reaction time in the reduction treatment in the reactor was 60 minutes from the charge of the starting solution and the seed crystal slurry to the extraction of the nickel powder slurry.
  • the sulfur grade was 0.003%, which was lower than the sulfur grade (0.01%) specified as the LME grade.
  • the nickel powder had a particle size D50 of 6.4 ⁇ m, which indicates that a very fine powder could be stably obtained as shown in FIG. 3 .
  • a starting solution (90 liter) containing ammonium sulfate (200 g/L), nickel powder (11 g/L), and polyacrylic acid (0.1 g/L) was placed into the 90 liter reactor the same as that in Example 1 to maintain the temperature at 185° C. Hydrogen gas was blown thereinto to control the pressure at 3.5 MPa.
  • a starting solution having a composition containing a nickel ammine sulfate complex solution (concentration of nickel: 83 g/L) and 360 g/L of ammonium sulfate was added to the reactor at a flow rate of 1 liter/min, and a nickel seed crystal slurry (concentration: 33 g/L) was added at a rate of 0.5 liter/min.
  • Hydrogen gas was blown into the pressurized container such that its pressure was maintained at 3.5 MPa, to advance the reduction treatment.
  • the nickel powder slurry subjected to the reduction treatment was continuously extracted from the reactor. This operation was continued for 6 hours.
  • the nickel powder forming the 33 g/L nickel seed crystal slurry had an average particle size of 53 ⁇ m.
  • the reaction time in the reduction treatment in the reactor was 60 minutes from the charge of the starting solution and the seed crystal slurry to the extraction of the nickel powder slurry.
  • the reduction rate or the reaction rate was 89.0%.
  • the recovered nickel powder has a sulfur grade of 0.01%, which satisfied the sulfur grade (0.01%) specified as the LME grade.
  • the nickel powder had a particle size D50 of 78.0 ⁇ m, which indicates that a sufficiently grown nickel powder was obtained. As shown in FIGS. 4 and 5 , the nickel powder was obtained in the form of particles having very smooth surfaces and having a true spherical shape.
  • a pressurized container having an inner volume of 190 liter and having inner walls lined with titanium was used as a reactor (reaction vessel).
  • a solution slurry (90 liter) containing 205 g/liter of ammonium sulfate, 1 g/liter of polyacrylic acid, and 105 g/liter of nickel powder was placed into this reactor.
  • the reactor was covered with a lid to maintain the temperature at 185° C.
  • Hydrogen gas was then blown into the gaseous phase portion of the reactor to control the inner pressure of the container to 3.5 MPa.
  • a nickel ammine sulfate complex solution concentration of nickel: g/liter
  • a solution containing 120 g/liter of ammonium sulfate were fed into this reactor at a flow rate of 1 liter per minute, and simultaneously 150 g/liter of nickel powder slurry was continuously fed into the reactor at a flow rate of 0.5 liter per minute.
  • Nickel powder having an average particle size of 1 ⁇ m was used for forming the nickel powder slurry. Hydrogen gas was blown into the reactor such that the inner pressure was maintained at 3.5 MPa.
  • the nickel powder slurry was continuously extracted. This operation was continued for hours.
  • the extracted nickel powder slurry was subjected to solid liquid separation using a Nutsche funnel into nickel powder and a filtrate.
  • the resulting nickel powder was washed, and was vacuum dried.
  • reaction rate namely, the proportion of hydrogen gas used in the precipitation reaction of the nickel powder was 98.9%.
  • the resulting nickel powder had an average particle size D50 of 5.2 ⁇ m. A fine nickel powder could be stably obtained.
  • a solution having the same composition as in Example 1 was continuously fed, at the same flow rate, into the same reactor as in Example 1 without containing polyacrylic acid, and was reduced with hydrogen gas under the same condition as that in Example 1 to obtain a nickel powder slurry.
  • the nickel powder slurry was subjected to solid liquid separation to obtain nickel powder.
  • the reduction rate or the reaction rate was 99.6%.
  • the proportion of particles having a particle size of 100 ⁇ m to 300 ⁇ m was 99% or more.
  • the proportion of particles having a particle size of more than 300 ⁇ m was less than 0.1%
  • the proportion of particles having a particle size of more than 150 ⁇ m and 300 ⁇ m or less was 91%
  • the proportion of particles having a particle size of more than 100 ⁇ m and 150 ⁇ m or less was 8.3%
  • the proportion of particles having a particle size of more than 75 ⁇ m and 100 ⁇ m or less and the proportion of particles having a particle size of more than 45 ⁇ m and ⁇ m or less both were less than 0.1%
  • the proportion of particles having a particle size of 45 ⁇ m or less was 0.7%.
  • the resulting nickel powder was not fine as the nickel powder according to the present invention.

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  • Chemical Kinetics & Catalysis (AREA)
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US16/082,004 2016-03-04 2017-03-03 Method for producing nickel powder Abandoned US20200338641A1 (en)

Applications Claiming Priority (9)

Application Number Priority Date Filing Date Title
JP2016041665 2016-03-04
JP2016-041665 2016-03-04
JP2016-075530 2016-04-05
JP2016075529 2016-04-05
JP2016-075529 2016-04-05
JP2016075530 2016-04-05
JP2016251266 2016-12-26
JP2016-251266 2016-12-26
PCT/JP2017/008562 WO2017150717A1 (ja) 2016-03-04 2017-03-03 ニッケル粉の製造方法

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US (1) US20200338641A1 (de)
EP (1) EP3424627A4 (de)
JP (1) JP6816755B2 (de)
CN (1) CN108778578A (de)
AU (1) AU2017226381B2 (de)
CA (1) CA3016390A1 (de)
PH (1) PH12018501870A1 (de)
WO (1) WO2017150717A1 (de)

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JP6816755B2 (ja) 2021-01-20
EP3424627A1 (de) 2019-01-09
AU2017226381B2 (en) 2019-12-12
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CA3016390A1 (en) 2017-09-08

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