WO2014136487A1 - Installation hydrométallurgique pour minerai d'oxyde de nickel et procédé pour la conduite de ladite installation hydrométallurgique - Google Patents

Installation hydrométallurgique pour minerai d'oxyde de nickel et procédé pour la conduite de ladite installation hydrométallurgique Download PDF

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WO2014136487A1
WO2014136487A1 PCT/JP2014/051319 JP2014051319W WO2014136487A1 WO 2014136487 A1 WO2014136487 A1 WO 2014136487A1 JP 2014051319 W JP2014051319 W JP 2014051319W WO 2014136487 A1 WO2014136487 A1 WO 2014136487A1
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Prior art keywords
leaching
neutralization
tank
stage
solid
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PCT/JP2014/051319
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English (en)
Japanese (ja)
Inventor
諭 松原
中井　修
坂元　隆
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住友金属鉱山株式会社
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Priority to US14/773,496 priority Critical patent/US20160024614A1/en
Priority to CA2904569A priority patent/CA2904569A1/fr
Priority to EP14760507.5A priority patent/EP2975142B1/fr
Priority to AU2014227269A priority patent/AU2014227269B2/en
Publication of WO2014136487A1 publication Critical patent/WO2014136487A1/fr
Priority to PH12015501978A priority patent/PH12015501978B1/en

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    • 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
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
    • C22B23/043—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
    • 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
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
    • 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
    • C22B3/02—Apparatus therefor
    • 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
    • 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
    • C22B3/20—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

Definitions

  • the present invention relates to a nickel oxide ore wet smelting plant that recovers nickel and cobalt from nickel oxide ore, and an operation method of the wet smelting plant.
  • the hydrometallurgical method of nickel oxide ore using this high pressure acid leaching method has processes as shown in the simplified process diagram of FIG. That is, an ore processing step in which nickel oxide ore is pulverized to a predetermined size to form a slurry, a sulfuric acid is added to the ore slurry to perform a leaching treatment under high temperature and high pressure (high pressure acid), and a leaching slurry.
  • a solid-liquid separation process for solid-liquid separation into a leachate containing an impurity element together with cobalt, and a neutralized starch containing the impurity element by adjusting the pH of the obtained leachate
  • a neutralization step for obtaining a neutralized final solution containing zinc together with nickel and cobalt, and dezincification for forming a nickel sulfide by adding a sulfiding agent to the neutralized final solution to obtain a nickel recovery mother liquor Process and nickel times
  • a nickel recovery process that forms a mixed sulfide containing nickel and cobalt by adding a sulfiding agent to the mother liquor, and a neutralization treatment is performed by mixing the waste liquid (poor liquid) in the nickel recovery process and the residue from the CCD process.
  • a final neutralization step see, for example, Patent Documents 1 and 2).
  • the leaching slurry obtained from the leaching step is adjusted to a pH at which cleaning can be performed efficiently during the multi-stage cleaning process in the next CCD step.
  • the pH of the leaching slurry is adjusted by charging the leaching slurry into a neutralization tank and adding a neutralizing agent such as calcium carbonate.
  • the pre-neutralized leaching slurry is then separated into a leaching solution and an leaching residue containing impurity elements together with nickel and cobalt while being subjected to multi-stage cleaning in a CCD process.
  • the separated leachate is sent to the neutralization step to become a neutralization final solution, and the leach residue is sent to the final neutralization step for processing.
  • the neutralized final solution is charged into the sulfurization reactor, and zinc sulfide, copper, etc. in the neutralized final solution are converted to sulfide by adding a sulfurizing agent such as hydrogen sulfide gas or sodium hydrosulfide. .
  • a nickel recovery mother liquor from which zinc sulfide has been removed is obtained by solid-liquid separation using a filter press or the like.
  • Patent Document 3 in a plant having a plurality of the same processes, even if there is a trouble or the like in a predetermined process on a series of processes by connecting processing facilities in a predetermined process with piping.
  • a technique for minimizing a decrease in operation efficiency is disclosed, which is a very effective technique in actual operation.
  • the technique described in Patent Document 3 is used as it is. It cannot be applied.
  • the present invention has been proposed in view of such circumstances, and is a nickel oxide ore capable of improving productivity by increasing the amount of ore treatment without causing a reaction failure or deterioration in operation efficiency.
  • An object of the present invention is to provide a wet smelting plant and an operation method thereof.
  • the inventors of the present invention have made extensive studies in order to achieve the above-described object.
  • the neutralization tank is provided in two stages, and the first stage neutralization tanks are arranged in a plurality of series. And it discovered that the subject mentioned above could be solved by making the neutralization processing tank of a 2nd step into a single series.
  • the hydrometallurgical plant for nickel oxide ore includes at least a leaching facility including a plurality of leaching treatment tanks for leaching the nickel oxide ore and a two-stage neutralization treatment tank, and the leaching treatment described above.
  • Pre-neutralization equipment that performs pre-neutralization to adjust the pH of the leached slurry discharged from the tank to a predetermined range, and a single series, the leached slurry discharged from the pre-neutralization equipment after pH adjustment,
  • the first stage neutralization tank is a leach provided in the leaching facility.
  • a plurality of series are provided so as to correspond to each series of treatment tanks, and the second stage in which the leaching slurry adjusted in pH in each series of neutralization treatment tanks constituting the first stage consists of a single series So as to join the neutralization tank Made which are, leached slurry joins the neutralization tank of the second stage, characterized in that it is transferred to the solid-liquid separation equipment.
  • the operation method of the nickel oxide ore hydrometallurgical plant according to the present invention is an operation method of the hydrometallurgical plant for recovering nickel and cobalt from the nickel oxide ore, the hydrometallurgy of the nickel oxide ore.
  • the plant includes at least a leaching facility including a plurality of leaching treatment tanks for leaching the nickel oxide ore and a two-stage neutralization treatment tank, and the pH of the leaching slurry discharged from the leaching treatment tank is within a predetermined range.
  • a pre-neutralization facility that performs pre-neutralization to be adjusted, and a single series of leaching slurry that has been pH-adjusted and discharged from the pre-neutralization facility are separated into a leaching solution and a leaching residue in a solid-liquid separation tank.
  • a plurality of first-stage neutralization treatment tanks correspond to each series of leaching treatment tanks provided in the leaching equipment.
  • the second stage neutralization treatment tanks are arranged in a single series, and the leach slurry discharged from each neutralization treatment tank in the first stage is formed from the single series. It is made to merge with the 2nd-stage neutralization processing tank, and the leached slurry which joined is transferred to the said solid-liquid separation equipment, It is characterized by the above-mentioned.
  • the pre-neutralization equipment for pre-neutralizing the leaching slurry is constituted by a two-stage neutralization tank, and the first-stage neutralization tank Is a plurality of series so as to correspond to a plurality of leaching treatment tanks, and the second stage neutralization treatment tank is a single series.
  • FIG. 1 is a configuration diagram of a nickel oxide ore hydrometallurgical plant.
  • FIG. 2 is a process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • FIG. 3 is a diagram for explaining the flow of operation during normal operation.
  • FIG. 4 is a diagram for explaining the flow of operation for self-circulating transfer from the first-stage neutralization tank to the corresponding leaching tank.
  • FIG. 5 is a diagram for explaining an operation flow for transferring the leach slurry from the first-stage neutralization tank to the final neutralization facility.
  • FIG. 6 is a diagram for explaining an operation flow for transferring the leach slurry from the first-stage neutralization tank to the solid-liquid separation tank.
  • FIG. 7 is a simplified process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • FIG. 8 is a simplified process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • FIG. 9 is a simplified process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • FIG. 10 is a simplified process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • the nickel oxide ore hydrometallurgical plant according to the present embodiment includes, for example, a leaching process by a high-pressure acid leaching method, a preliminary neutralization process, and a solid-liquid separation. It is for performing the hydrometallurgical operation of the nickel oxide ore which consists of a process (CCD process), a neutralization process, a dezincification process, a sulfurization process, and a final neutralization process (detoxification process).
  • the hydrometallurgical plant 10 includes at least a leaching treatment tank 11 (1 to n) for leaching nickel oxide ore. ) With a plurality of (n) series leaching equipment 11 and a two-stage neutralization tank, and preliminary neutralization to adjust the pH of the leaching slurry discharged from the leaching tank 11 (1 to n) to a predetermined range.
  • the first stage neutralization treatment tank 12 A (1 to n) in the preliminary neutralization equipment 12 is the leaching treatment tank 11 (1 to n ) provided in the leaching equipment.
  • a plurality of (n) series are provided so as to correspond to each series, and a single leaching slurry whose pH is adjusted in each series of neutralization treatment tanks 12A (1 to n) constituting the first stage is provided. It is comprised so that it may join to the neutralization processing tank 12B of the 2nd step
  • stage which consists of a series.
  • the leached slurry that has joined the second-stage neutralization tank 12B is transferred to the solid-liquid separation facility 13.
  • the hydrometallurgical plant 10 includes two or more reaction tanks in a series of treatment facilities in a process before the preliminary neutralization process (hereinafter also referred to as “upper process”).
  • a series of processing equipment is configured from a single series (one series) of reaction vessels. In this way, it is possible to increase the amount of nickel oxide ore while reducing the number of parts and suppressing the equipment cost, using a leaching treatment facility of a size that has been used in the past. The production amount of mixed sulfide (product) can be stably increased.
  • the hydrometallurgical plant 10 even when the leaching slurry obtained from a plurality of series of treatment facilities has a variation in pH or the like, it is made to merge in the second-stage neutralization treatment tank 12B. Therefore, the variation can be eliminated, and solid-liquid separation processing can be performed in the solid-liquid separation facility 13 as a uniform leaching slurry.
  • the hydrometallurgical plant 10 by appropriately providing piping for connecting the first-stage neutralization treatment tank 12A (1 to n) and the reaction tank of the treatment equipment in other processes, for example, plant operation It is possible to prevent the leaching slurry at the stage where the leaching process, such as immediately after the start, has not progressed sufficiently, from being transferred to the solid-liquid separation process or a subsequent process. Thereby, generation
  • the nickel oxide ore wet smelting plant and the operation method of the wet smelting plant according to the present embodiment will be described more specifically.
  • This nickel oxide ore wet smelting method is a hydrometallurgical method of leaching and recovering nickel and cobalt from nickel oxide ore using, for example, a high-pressure acid leaching method (HPAL method).
  • HPAL method high-pressure acid leaching method
  • FIG. 2 shows an example of a process diagram of a hydrometallurgical method using high pressure acid leaching of nickel oxide ore.
  • the hydrometallurgical method of nickel oxide ore is a leaching step S1 in which sulfuric acid is added to a slurry of nickel oxide ore and leaching is performed under high temperature and high pressure, and the pH of the obtained leaching slurry is set to a predetermined value.
  • the zinc sulfide is generated by the above, and the zinc sulfide is separated and removed to obtain the nickel recovery mother liquor containing nickel and cobalt, and the sulfur recovery agent is added to the nickel recovery mother liquor.
  • a nickel recovery step S6 described form a mixed sulfide containing Kell and cobalt. Furthermore, this hydrometallurgy method has a final neutralization step S7 for recovering and detoxifying the leaching residue separated in the solid-liquid separation step S3 and the poor liquid discharged in the nickel recovery step S6.
  • Leaching process (1-1) About leaching process
  • a leaching process using, for example, a high-pressure acid leaching method is performed on the nickel oxide ore. Specifically, sulfuric acid is added to the ore slurry obtained by pulverizing the nickel oxide ore used as a raw material, and the ore slurry is stirred by pressurization under a high temperature condition of 220 to 280 ° C. A leach slurry consisting of the residue is formed.
  • Nickel oxide ores used in the leaching step S1 are mainly so-called laterite ores such as limonite or saprolite ores.
  • Laterite ore usually has a nickel content of 0.8 to 2.5% by weight and is contained as a hydroxide or siliceous clay (magnesium silicate) mineral.
  • the iron content is 10 to 50% by weight and is mainly in the form of trivalent hydroxide (goethite), but partly divalent iron is contained in the siliceous clay.
  • an oxidized ore containing valuable metals such as nickel, cobalt, manganese, and copper, for example, a manganese nodule that exists in the deep sea bottom is used.
  • a leaching reaction represented by the following formulas (1) to (3) and a high temperature thermal hydrolysis reaction represented by the following formulas (4) and (5) occur, and nickel, cobalt, etc.
  • Leaching as a sulfate and immobilizing the leached iron sulfate as hematite since the immobilization of iron ions does not proceed completely, the leaching slurry obtained usually contains divalent and trivalent iron ions in addition to nickel, cobalt and the like.
  • the amount of sulfuric acid added in the leaching step S1 is not particularly limited, and an excessive amount that allows iron in the ore to be leached is used. For example, 300 to 400 kg per ton of ore. If the amount of sulfuric acid added per ton of ore exceeds 400 kg, the sulfuric acid cost increases, which is not preferable.
  • the pH of the obtained leaching solution is adjusted to 0.1 to 1.0 from the viewpoint of filterability of the leaching residue containing hematite produced in the subsequent solid-liquid separation step S3. It is preferable to do.
  • the leaching process (high pressure acid leaching facility) 11 performs the leaching process in the leaching step S1 described above.
  • the leaching equipment 11 in the hydrometallurgical plant 10 includes a plurality of (n) series of leaching treatment tanks 11 (1 to n) for leaching nickel oxide ore (for example, FIG. 1).
  • (N 2 series) as shown in FIG.
  • the leaching treatment tank is referred to as “leaching treatment tank 11 (n) ” when the number of series is not specified.
  • a first-stage neutralization tank 12A (1 to n) which will be described later, is also expressed as “neutralization tank 12A (n) ”.
  • each series of leaching treatment tanks 11 (n) constituting the leaching equipment 11 for example, a high-temperature pressurized container (autoclave) is used.
  • the leaching treatment tank 11 (n) for example, ore slurry transferred from the ore treatment process, that is, a predetermined amount of ore slurry obtained by pulverizing ore to a predetermined particle size is loaded from each charging section. Entered.
  • the leaching processing tank 11 (n) which consists of an autoclave etc.
  • size comparable as what has been conventionally used for operation can be used.
  • a leaching slurry having a production amount of 1 million tons / year to 2 million tons / year in terms of nickel can be used.
  • the amount of nickel oxide ore can be increased, and the nickel-cobalt mixed sulfide obtained through a subsequent process Production volume can be increased.
  • the first stage of the neutralization treatment tank 12A constituting its leaching vessel 11 (n) a preliminary neutralizing facility 12 (n) and can be connected to pipe 21 (n) connecting the.
  • the pipe 21 (n) is a pipe that connects the leaching treatment tank 11 (n) and the first-stage neutralization treatment tank 12A (n) in the same series.
  • This piping 21 (n) causes the transfer pump 31 to circulate (self-circulate) the leaching slurry discharged from the first neutralization treatment tank 12A (n) to the same leaching treatment tank 11 (n). This is so-called self-circulation piping. The operation for self-circulation will be described in detail later.
  • Pre-neutralization step S2 Pre-neutralization treatment
  • the pH of the leaching slurry obtained in the leaching step S1 is adjusted to a predetermined range.
  • excess sulfuric acid is added from the viewpoint of improving the leaching rate. Therefore, the obtained leaching slurry contains free sulfuric acid (excess sulfuric acid not involved in the leaching reaction), and its pH is very low. Therefore, in the pre-neutralization step S2, the pH of the leaching slurry is adjusted to a predetermined range so that the washing is efficiently performed at the time of the multi-stage washing in the next solid-liquid separation step S3.
  • the leaching slurry used for the cleaning treatment is adjusted to a pH of about 2 to 6.
  • a pH When the pH is lower than 2, a cost for making the subsequent process equipment acid-resistant is required.
  • nickel leached in the leaching solution (slurry) may remain as a residue in the washing process (precipitate) and the washing efficiency may be reduced.
  • a set value may be selected depending on conditions such as the operation status of the leaching process in the leaching step S1 and the pH of the washing water used in the solid-liquid separation step S3 (about 5 if it is acid rain) in the pH range described above.
  • a set value may be selected.
  • the pH adjustment method is not particularly limited, but can be adjusted to a predetermined range by adding a neutralizing agent such as calcium carbonate slurry.
  • the pre-neutralization facility 12 performs the pre-neutralization process in the pre-neutralization step S2.
  • the preliminary neutralization equipment 12 in the hydrometallurgical plant 10 includes two stages of neutralization treatment tanks 12A and 12B as shown in FIG.
  • the first-stage neutralization tank 12A (n) corresponds to each series of the leaching tank 11 (n) provided in the leaching equipment 11 described above.
  • a plurality (n) series are provided to correspond.
  • the second stage neutralization treatment tank 12B is composed of a single series, and the leached slurry discharged from each of the first stage neutralization treatment tanks 12A (n) is the second stage neutralization treatment. It is comprised so that it may join the tank 12B.
  • the leaching equipment 11 includes two series of leaching treatment tanks (leaching treatment tank 11 (1) and leaching treatment tank 11 (2) ), the leaching treatment tanks 11 (1) and 11 (2) Correspondingly, a neutralization tank 12A (1) and a neutralization tank 12A (2) are provided as the first-stage neutralization tank 12A.
  • the second stage neutralization treatment tank 12B is composed of a single series of treatment tanks, and the neutralization treatment tank 12A (1) and the neutralization treatment tank 12A (2) constituting the first stage.
  • the leaching slurries discharged from each of the first and second wastewaters are joined to the second neutralization treatment tank 12B.
  • the slurry after pre-neutralization obtained by pre-neutralizing the leaching slurry with a plurality of series of neutralization treatment tanks is likely to vary in terms of pH, for example.
  • the leaching slurry obtained from the neutralization tank is not uniform.
  • the reaction varies and the like, and the efficient operation cannot be performed.
  • the preliminary neutralization facility 12 is provided with the two-stage neutralization treatment tanks 12A and 12B, and the upper process and the lower process are performed between the first stage and the second stage.
  • variation will be eliminated, and it transfers to the next solid-liquid separation process S3 as a uniform leaching slurry.
  • the second-stage neutralization treatment tank 12B can function as a retention tank (buffer), the flow rate of the leaching slurry can be accurately adjusted and stably transferred to the solid-liquid separation step S3. it can.
  • the processing amount of nickel oxide ore can be increased effectively, reducing a number of parts and reducing equipment cost effectively.
  • the low-pH leaching slurry obtained from the leaching treatment tanks 11 (n) of each series is subjected to the first stage neutralization treatment corresponding to each series.
  • the tank 12A (n) is charged and the leaching slurry is neutralized by adding a neutralizing agent such as a calcium carbonate slurry.
  • a neutralizing agent such as a calcium carbonate slurry.
  • the leaching slurry neutralized in each series of neutralization treatment tanks 12A (n) constituting the first stage is joined to the second stage neutralization treatment tank 12B, and leaching after preliminary neutralization.
  • a slurry is obtained.
  • a neutralizing agent may be added to finely adjust the pH of the leaching slurry.
  • the leaching slurry whose pH has been adjusted can be subjected to the solid-liquid separation process more stably.
  • the pipe 21 (n) is a pipe that connects the first-stage neutralization treatment tank 12A (n) and the charging section of the leaching treatment tank 11 (n) in the same series.
  • This pipe 21 (n) causes the leach slurry to be circulated (self-circulated) from the first stage neutralization tank 12A (n) to the leaching tank 11 (n) of the same series by the transfer pump 31.
  • This is so-called self-circulation piping.
  • the arrangement configuration of the pipe 21 (n) and the self-circulating operation will be described in detail later.
  • the first neutralization treatment tank 12A (n) in the preliminary neutralization equipment 12 includes the neutralization treatment tank 12A (n) and the final neutralization equipment 14 in the final neutralization step (detoxification step) S7. Can be connected to each other.
  • This pipe 22 is connected to the charging section of the final neutralization equipment 14 independently from each series of the first stage neutralization tank 12A (n) or integrated at a predetermined location from each series.
  • the leaching slurry discharged from the first-stage neutralization tank 12A (n) can be transferred to the final neutralization facility 14 by the transfer pump 31 provided in the pipe 22.
  • the arrangement configuration of the piping 22 and the operation of transferring the leaching slurry from the first-stage neutralization treatment tank 12A (n) to the final neutralization facility 14 will be described in detail later.
  • the piping 23 which connects each solid-liquid separation tank can be connected.
  • This pipe 23 is provided for each of the solid-liquid separation tanks provided in multiple stages independently from each series of the first stage neutralization treatment tank 12A (n) or integrated at a predetermined location from each series.
  • the leaching slurry discharged from the first stage neutralization tank 12A (n) is transferred to a predetermined solid-liquid separation tank by a transfer pump 31 provided in the pipe 23 and connected to the charging section. Make it possible.
  • the arrangement configuration of the piping 23 and the operation of transferring the leaching slurry from the first-stage neutralization treatment tank 12A (n) to the predetermined solid-liquid separation tank will be described in detail later.
  • FIG. 1 although the piping 21, 22, 23 mentioned above are made into common piping in part, and the transfer pump for transferring the leaching slurry is shown in common, it is limited to this. is not.
  • Each of the pipes 21, 22, and 23 may be provided individually and a transfer pump may be installed in each of the pipes 21, 22, and 23.
  • Solid-liquid separation step (3-1) Solid-liquid separation treatment
  • nickel and cobalt were washed while washing the leached slurry after pH adjustment obtained in the preliminary neutralization step S2 in multiple stages.
  • a leaching solution crude nickel sulfate aqueous solution
  • zinc as an impurity element is separated from a leaching residue.
  • the solid-liquid separation process is performed by the solid-liquid separation equipment such as a thickener using the flocculant supplied from the flocculant supply equipment. Specifically, the leaching slurry is first diluted with a cleaning liquid, and then the leaching residue in the slurry is concentrated as a thickener sediment. Thereby, the nickel content adhering to the leaching residue can be reduced according to the degree of dilution.
  • this solid-liquid separation step S3 it is preferable to perform solid-liquid separation while using multiple stages of solid-liquid separation tanks such as thickeners and washing the leach slurry in multiple stages.
  • a continuous countercurrent cleaning method CCD method: Counter-Current Decantation
  • a cleaning liquid is brought into contact with the leaching slurry in countercurrent
  • the cleaning liquid newly introduced into the system can be reduced, and the recovery rate of nickel and cobalt can be improved to 95% or more.
  • the cleaning liquid is not particularly limited, but it is preferable to use a liquid that does not include nickel and does not affect the process. Among them, it is preferable to use an aqueous solution having a pH of 1 to 3. When the pH of the cleaning liquid is high, a bulky aluminum hydroxide is produced when aluminum is contained in the leachate, which causes poor settling of the leach residue. For this reason, as the cleaning liquid, it is preferable to repeatedly use a low pH (pH of about 1 to 3) poor liquid obtained in the nickel recovery step S6 as a subsequent step.
  • the flocculant to be used is not particularly limited, and for example, an anionic flocculant can be used.
  • (3-2) Solid-liquid separation facility In the hydrometallurgical plant 10 according to the present embodiment, the solid-liquid separation facility 13 performs the solid-liquid separation process in the solid-liquid separation step S3 described above.
  • the solid-liquid separation facility 13 in the hydrometallurgical plant 10 is configured by connecting, for example, six-stage thickeners (solid-liquid separation tanks) (CCD1 to CCD6) as shown in FIG.
  • the leaching slurry after the pre-neutralization in the pre-neutralization step S2 (pH adjusted) is transferred by a transfer pump and charged into the first stage thickener (CCD 1).
  • the cleaning liquid cleaning water
  • the sixth-stage thickener CCD 6 at the final stage via a pipe (not shown).
  • the cleaning liquid charged in the CCD 6 at the final stage takes in the moisture adhering to the residue in the leaching slurry in the process of being transferred from the CCD 6 to the CCD 5, CCD 4,.
  • the concentration of valuable metals such as nickel in the cleaning liquid increases, and is finally discharged from the CCD 1 as a leachate and transferred to the neutralization step S4 of the next step.
  • the concentration of valuable metals in the cleaning liquid charged in the CCD 6 is, for example, approximately 0 g / L at the time of charging when the nickel concentration is 0.5 g in the transfer process from the CCD 6 to the CCD 5.
  • the leachate discharged from the CCD 1 has a nickel concentration of about 3 g / L.
  • the first-stage neutralization constituting each solid-liquid separation tank and the preliminary neutralization equipment 12 is provided in each charging portion of the solid-liquid separation tank such as thickener provided in multiple stages.
  • a pipe 23 connecting the treatment tank 12A (n) can be connected. This pipe 23 is provided for each of the solid-liquid separation tanks provided in multiple stages independently from each series of the first stage neutralization treatment tank 12A (n) or integrated at a predetermined location from each series.
  • the leaching slurry discharged from the first stage neutralization tank 12A (n) is transferred to a predetermined solid-liquid separation tank by a transfer pump 31 provided in the pipe 23 and connected to the charging section. Make it possible.
  • the arrangement configuration of the piping 23 and the operation of transferring the leaching slurry from the first-stage neutralization treatment tank 12A (n) to the predetermined solid-liquid separation tank will be described in detail later.
  • Neutralization step S4 the pH of the leachate (crude nickel sulfate aqueous solution) separated in the solid-liquid separation step S3 is adjusted, and the neutralized starch containing the impurity element is separated, and nickel and A neutralized final solution containing zinc together with cobalt is obtained.
  • the pH of the resulting neutralized final solution is 4 or less, preferably 3.0 to 3.5, more preferably 3.1 to 3, while suppressing oxidation of the separated leachate.
  • a neutralizing agent such as calcium carbonate is added to the leachate so as to be 3.2 to form a neutralized final solution and a neutralized starch slurry containing trivalent iron as an impurity element.
  • impurities such as trivalent iron ions and aluminum ions remaining in the solution are removed as neutralized starch in this way, and a neutralized final solution serving as a base for the nickel recovery mother liquor is generated. .
  • the neutralization process in neutralization process S4 is performed by the neutralization equipment.
  • the neutralization facility include a neutralization reaction tank that performs a neutralization reaction, and a separation treatment tank such as a thickener that separates the neutralized starch obtained by the neutralization reaction and the neutralized final solution.
  • This neutralization equipment consists of a single series.
  • the neutralization reaction tank in the neutralization facility the leachate (crude nickel sulfate aqueous solution) discharged from the CCD 1 in the solid-liquid separation facility 13 is charged, and a neutralizing agent such as calcium carbonate is charged for neutralization. A reaction occurs.
  • the separation treatment tank the slurry after the neutralization reaction is charged, and the slurry is separated into a neutralized final solution that becomes a mother liquor for nickel recovery and a neutralized starch slurry that contains trivalent iron as an impurity element. To do.
  • the neutralized starch slurry is extracted from the bottom of the separation treatment tank.
  • the neutralized final solution from which the neutralized starch has been separated overflows and is stored in a storage tank or the like, and is then transferred to the next dezincing step S5.
  • a zinc sulfide is generated by adding a sulfiding agent such as hydrogen sulfide gas to the neutralized final solution obtained from the neutralizing step S4 and subjecting it to a sulfiding treatment.
  • the zinc sulfide is separated and removed to obtain a nickel recovery mother liquor (dezincing final solution) containing nickel and cobalt.
  • a neutralized final solution containing zinc and nickel and cobalt is introduced into a pressurized container, and hydrogen sulfide gas or the like is blown into the gas phase, so that zinc is made against nickel and cobalt.
  • hydrogen sulfide gas or the like is blown into the gas phase, so that zinc is made against nickel and cobalt.
  • the dezincing process in the dezincing step S5 is performed in a dezincing facility.
  • the dezincification equipment includes, for example, a sulfidation reaction tank that performs a sulfidation reaction by blowing hydrogen sulfide gas or the like into the final neutralized solution, and a filter device that separates and removes zinc sulfide from the solution after the sulfidation reaction.
  • This dezincification equipment consists of a single series.
  • the neutralized final solution transferred through the above-described neutralization step S4 is charged, and a sulfiding agent such as hydrogen sulfide gas is blown to cause a sulfidation reaction.
  • the filter device is constituted by a filter cloth (filter cloth) or the like, and separates zinc sulfide from the post-sulfurization reaction solution containing zinc sulfide to generate a nickel recovery mother liquor. The obtained nickel recovery mother liquor is transferred to the next nickel recovery step S6.
  • Nickel recovery step S6 a sulfur recovery agent such as hydrogen sulfide gas is blown into the nickel recovery mother liquor obtained by separating and removing zinc, which is an impurity element, as zinc sulfide in the zinc removal step S5. A sulfurization reaction is caused to produce a sulfide (nickel / cobalt mixed sulfide) containing nickel and cobalt and a poor solution.
  • a sulfur recovery agent such as hydrogen sulfide gas is blown into the nickel recovery mother liquor obtained by separating and removing zinc, which is an impurity element, as zinc sulfide in the zinc removal step S5.
  • a sulfurization reaction is caused to produce a sulfide (nickel / cobalt mixed sulfide) containing nickel and cobalt and a poor solution.
  • the mother liquid for nickel recovery is a sulfuric acid solution in which impurity components are reduced from the leachate of nickel oxide ore through the neutralization step S4 and the dezincing step S5.
  • the nickel recovery mother liquor may contain several g / L of iron, magnesium, manganese, etc. as impurity components. These impurity components are sulfides with respect to nickel and cobalt to be recovered. As a result, the resulting sulfide is not contained.
  • Nickel recovery processing in the nickel recovery step S6 is executed in a nickel recovery facility.
  • the nickel recovery facility includes, for example, a sulfurization reaction tank that performs a sulfurization reaction by blowing hydrogen sulfide gas or the like into a nickel recovery mother liquor, and a solid-liquid separation tank that separates and recovers nickel-cobalt mixed sulfide from the liquid after the sulfurization reaction.
  • This nickel recovery facility consists of a single series. In the sulfidation reaction tank in the nickel recovery facility, the nickel recovery mother liquor transferred through the dezincing step S5 described above is charged, and a sulfidizing agent such as hydrogen sulfide gas is blown to cause a sulfidation reaction. Mixed sulfide is formed.
  • the solid-liquid separation tank is constituted by, for example, a thickener or the like, and is subjected to sedimentation treatment on the slurry after the sulfidation reaction containing nickel / cobalt mixed sulfide, so that nickel / cobalt mixed sulfide which is a precipitate is formed. Is recovered from the bottom of the thickener. On the other hand, the aqueous solution component overflows and is recovered as a poor solution.
  • the recovered poor solution is a solution having a very low concentration of valuable metals such as nickel, and contains impurity elements such as iron, magnesium, and manganese remaining without being sulfided. This poor solution is transferred to the final neutralization step S7 and detoxified.
  • Final neutralization step (7-1) Final neutralization treatment
  • the final stage of the solid-liquid separation tank provided in multiple stages in the solid-liquid separation process in the solid-liquid separation step S3 described above (for example, During the adjustment of the leaching residue discharged from the CCD 6) and the poor solution containing impurity elements such as iron, magnesium, manganese, etc. recovered in the nickel recovery step S6 to a predetermined pH range satisfying the discharge standard A summation process (detoxification process) is performed.
  • the pH adjustment method is not particularly limited, but can be adjusted to a predetermined range by adding a neutralizing agent such as calcium carbonate slurry.
  • the final neutralization facility 14 performs the neutralization process in the above-described final neutralization step S7.
  • a final neutralization treatment tank is provided in a single series.
  • the final neutralization facility 14 is charged with the leaching residue transferred from the solid-liquid separation step S3 and the poor solution transferred from the nickel recovery step S6.
  • the reaction tank the leaching residue and the poor liquid are mixed, and the pH is adjusted to a predetermined pH range by the neutralizing agent to become a waste slurry (tailing).
  • generated in this reaction tank is transferred to a tailing dam (waste storage place).
  • the charging section of the final neutralization facility 14 includes the final neutralization facility 14 and the first-stage neutralization treatment tank 12A (n) constituting the preliminary neutralization facility 12.
  • the pipe 22 to be connected can be connected. This pipe 22 is connected to the charging section of the final neutralization equipment 14 independently from each series of the first stage neutralization tank 12A (n) or integrated at a predetermined location from each series.
  • the leaching slurry discharged from the first-stage neutralization tank 12A (n) can be transferred to the final neutralization facility 14 by the transfer pump 31 provided in the pipe 22.
  • the arrangement of the piping 22 and the operation of transferring the leached slurry from the first stage neutralization tank 12A (n) to the final neutralization facility 14 will be described in detail later.
  • the hydrometallurgical plant 10 includes at least a leaching facility 11 including a plurality (n) of leaching treatment tanks 11 (n) for performing leaching treatment on nickel oxide ore, and two stages.
  • the neutralization treatment tanks 12A and 12B are provided, and the pre-neutralization equipment 12 for performing the pre-neutralization for adjusting the pH of the leaching slurry discharged from the leaching treatment tank 11 (n) to a predetermined range, and a single series, It comprises a solid-liquid separation facility 13 for solid-liquid separation of the leached slurry that has been adjusted in pH and discharged from the preliminary neutralization facility 12 in a solid-liquid separation tank (FIG. 1).
  • the first stage neutralization treatment tank 12 ⁇ / b > A (n) is a leaching treatment tank 11 provided in the leaching equipment 11.
  • a plurality of series are provided so as to correspond to each series of (n), and the leaching slurry whose pH is adjusted in each series of neutralization treatment tanks 12A (n) constituting the first stage consists of a single series.
  • the second stage neutralization tank 12B is configured to join, and the leachate that has joined the second stage neutralization tank is transferred to a solid-liquid separation facility.
  • the hydrometallurgical plant 10 configured in this way, by using a plurality of series of leaching treatment facilities having a size that has been conventionally operated (for example, the amount of leachate produced is 1 to 20,000 tons / year in terms of nickel).
  • the amount of nickel oxide ore can be increased.
  • the subsequent processes that is, the processes subsequent to the preliminary neutralization process, are integrated into one series, the number of parts can be reduced as a whole plant, and the equipment cost can be reduced.
  • each leaching slurry obtained from a plurality of series of treatment equipment has pH and the like. Even when there is a variation in properties, the leaching slurry discharged from each series is merged in the second stage neutralization treatment tank 12B, so that the variation can be eliminated and uniform.
  • a solid-liquid separation process can be performed as a leach slurry.
  • paragraph, and the reaction tank in the processing equipment in another process. 23 can be provided as appropriate.
  • the leaching slurry at a stage where the leaching process such as immediately after the start of plant operation is not sufficiently progressed can be prevented from being transferred to the solid-liquid separation step S3 or a later step, Generation
  • production of the reaction failure in a process, the fall of operational efficiency, etc. can be suppressed effectively.
  • FIG. 3 shows a diagram for explaining the flow of operation during normal operation.
  • nickel oxide ore slurry (ore slurry) that has been crushed to a predetermined size in an ore treatment process or the like is supplied to the leaching treatment facility 11.
  • the first series of leaching treatment tanks 11 (1) and the second series of leaching treatment tanks 11 (2), which are provided, are ores in the leaching treatment tanks 11 (1) and 11 (2) of each series. A leaching treatment is applied to the slurry.
  • the leaching slurry obtained by the leaching treatment in the leaching treatment tanks 11 (1) and 11 (2) is transferred to the preliminary neutralization equipment 12.
  • the leaching slurry discharged from the leaching treatment tanks 11 (1) and 11 (2) is stored in the first stage corresponding to each series of the leaching treatment tanks 11 (1) and 11 (2). It charges to sum processing tank 12A (1) , 12A (2) , respectively.
  • a neutralizing agent is added to the leached slurry charged to adjust the pH to a predetermined pH range.
  • the leaching slurry whose pH has been adjusted in the first stage neutralization tanks 12A (1) and 12A (2) is transferred to the second stage neutralization tank 12B and charged. That is, the leaching slurry whose pH is adjusted in each of the first and second series of neutralization treatment tanks 12A (1) and 12A (2) is used as a second stage neutralization treatment tank 12B composed of a single series. To join. In this way, in the second stage neutralization treatment tank 12B, the leaching slurries from each series are merged, so that variations in properties such as pH can be eliminated, and the uniform leaching slurry is transferred to the subsequent process. can do. In the second-stage neutralization treatment tank 12B, a neutralizing agent may be added to the combined leaching slurry to finely adjust the pH.
  • each of the first stage neutralization tanks 12A (1) and 12A (2) and the second stage neutralization tank It is transported by overflowing the leached slurry via the pipes 24 (1) and 24 (2) connecting to 12B.
  • the leaching slurry is discharged from the second-stage neutralization treatment tank 12B, and the leaching slurry is transferred to the solid-liquid separation facility 13.
  • the solid-liquid separation facility 13 can be a facility in which six stages of thickeners (CCD1 to CCD6) are connected, and the transferred leach slurry is used as the first stage thickener (CCD1).
  • CCD1 to CCD6 the first stage thickener
  • the discharge section of the second-stage neutralization tank 12B and the piping 25 connecting the charging section to the first-stage thickener (CCD 1) are used. Then, transfer is performed using a transfer pump 32 provided in the pipe 25.
  • the leaching slurry charged is contacted countercurrently with the cleaning liquid charged in the final stage CCD 6 in the process of transferring the leached slurry sequentially from the CCD 1 to the CCD 6.
  • the residue in the slurry is agglomerated.
  • a leachate (crude nickel sulfate aqueous solution) having a high concentration of valuable metals such as nickel is discharged from the CCD 1.
  • the leaching residue having a low concentration of valuable metals such as nickel is discharged from the CCD 6 at the final stage, transferred to the final neutralization equipment 14 and detoxified.
  • the process of leaching valuable metals from the ore slurry has hardly started, and the leaching process is performed from the leaching treatment tanks 11 (1) and 11 (2) constituting the leaching equipment 11. Insufficient leaching slurry is discharged.
  • the first stage neutralization treatment tanks 12A (1) and 12A (2) in the preliminary neutralization facility 12, and leaching Pipes 21 (1) and 21 (2) connecting the leaching treatment tanks 11 (1) and 11 (2) in the facility 11 are connected.
  • the pipes 21 (1) and 21 (2) are connected to the first stage neutralization tanks 12A (1) and 12A (2) and the charging sections of the leaching tanks 11 (1) and 11 (2). It is a pipe connected by the same series. That is, for example, the pipe 21 (2) connecting the second series of leaching treatment tank 11 (2) and the second series of neutralization treatment tank 12A (2) .
  • These pipes 21 (1) and 21 (2) are used for the process liquid (temperature increase ) for raising the temperature of the leaching treatment tanks 11 (1) and 11 (2) at the time of start-up after the start of operation as described above.
  • liquid) and leaching tank 11 (1), 11 (a leach slurry low nickel concentration discharged from the 2) leaching tank 11 (1), 11 (2) and neutralization tank 12A (1), 12A It is possible to circulate between (2) .
  • the pipes 21 (1) and 21 (2) are the same series of leaching treatment tanks for leaching slurry and process liquid discharged from the first stage neutralization treatment tanks 12A (1) and 12A (2).
  • 11 (1) and 11 (2) are self-circulating pipes that can be self-circulated.
  • the pipes 21 (1) and 21 (2) extend from the first-stage neutralization treatment tanks 12A (1) and 12A (2) , respectively, and then extend to predetermined locations (see FIG. 1 and FIG. 4 may be combined at the transfer pump 31 location), branched again, and connected to the respective leaching treatment tanks 11 (1) and 11 (2) , or completely for each series. It is good also as separate piping.
  • a transfer pump 31 is provided in the pipes 21 (1) and 21 (2) , and the leaching slurry discharged from the neutralization tanks 12A (1) and 12A (2) is transferred to the transfer pump 31. To the leaching treatment tanks 11 (1) and 11 (2) .
  • the transfer of the leach slurry is controlled between the neutralization tanks 12A (1) and 12A (2) and the transfer pump 31 described above.
  • ON / OFF valves 42 (1) and 42 (2) are provided.
  • the ON / OFF valves 42 (1) and 42 (2) are set in the ON state (“open” state) so that the discharged leached slurry can be transferred. In the normal operation described above, this for self circulation pipe 21 (1), 21 (2) to provided the ON / OFF valve 42 (1), 42 (2) the OFF state ( "closed” ).
  • the leaching process for the ore slurry is performed in the leaching treatment tank 11 (2) in the leaching equipment 11 in the initial stage such as immediately after the start of operation, that is, immediately after the start of the operation of the second system .
  • the obtained leaching slurry has an insufficient leaching state.
  • a process liquid temperature rising liquid
  • warm water is charged and the temperature rising process is performed.
  • the leaching slurry or the process liquid is discharged from the leaching treatment tank 11 (2), and the middle of the first stage of the same series. It is made to transfer to sum processing tank 12A (2) . Thereafter, the neutralization treatment tank 12A (2) and the leaching tank 11 (2) and via a pipe 21 (2) connecting the leaching treatment tank 11 from the first-stage neutralization treatment tank 12A (2) ( The leaching slurry or process liquid is self-circulated for 2) .
  • the self-circulation pipe 21 (2) connecting the first stage neutralization treatment tank 12A (2) and the leaching treatment tank 11 (2) is connected.
  • the provided ON / OFF valve 42 (2) is turned on (“open” state).
  • the leaching slurry or process liquid is circulated from the neutralization tank 12A (2) to the leaching tank 11 (2) by the transfer pump 31 provided in the self-circulation pipe 21 (2) .
  • This self-circulating operation is performed, for example, until the leaching treatment tank 11 (2) is sufficiently heated.
  • the supply of ore slurry and the supply of sulfuric acid to the leaching treatment tank 11 (2) are stopped. Therefore, when circulating the leaching slurry, the valuable metal concentration of the leaching slurry is substantially 0 g / L in terms of nickel.
  • the first stage neutralization treatment tanks 12A (1) and 12A (2) and the leaching treatment tanks 11 (1) and 11 (2) By providing the pipes 21 (1) and 21 (2) for connecting the leaching slurry and the process liquid for raising the temperature in the initial stage such as immediately after the start of operation, the self-circulation is enabled. Thereby, it is possible to prevent the leaching slurry and process liquid containing almost no nickel from being transferred to the subsequent solid-liquid separation process S3 or the like.
  • the first stage neutralization treatment tanks 12A (1) and 12A (2) in the preliminary neutralization facility 12 and leaching A pipe 22 connecting the leaching treatment tanks 11 (1) , 11 (2) and the final neutralization equipment 14 in the equipment 11 is connected.
  • the pipe 22 is independent from each series of the first stage neutralization treatment tanks 12A (1) and 12A (2) , or is integrated at a predetermined location from each series, so that the final neutralization equipment 14 Connected to the charging section.
  • the pipe 22 is provided with a transfer pump 31, and the leach slurry discharged from the first-stage neutralization tanks 12 A (1) and 12 A (2) is finally neutralized by the transfer pump 31. 14 to transfer.
  • an ON / OFF valve 42 (1) which controls the transfer of the leach slurry, for example, between the neutralization tanks 12A (1) , 12A (2) and the above-described transfer pump is provided inside the pipe 22. 42 (2) is provided.
  • the ON / OFF valve 42 ( 1) , 42 (2) is turned on (“open” state) to allow the discharged leach slurry to be transferred.
  • the ON / OFF valves 42 (1) and 42 (2) provided in the pipe for transferring to the final neutralization facility 14 are in the OFF state (“closed” state). ing.
  • the leaching process proceeds little by little in the leaching treatment tank 11 (2) .
  • the nickel concentration in the discharged leaching slurry is low.
  • the leaching slurry is discharged from the leaching treatment tank 11 (2) , and the first stage neutralization treatment tank of the same series. Transfer to 12A (2) . Then, via a pipe 22 which connects the neutralization tank 12A and (2) and a final neutralization equipment 14, transferring the leached slurry from the neutralization tank 12A (2) to a final neutralization equipment 14.
  • the leaching slurry is transferred to the final neutralization equipment 14, the above-described self-circulation piping (first stage neutralization treatment tank 12A (2) and leaching treatment tank 11 (2) are connected. Piping) 21
  • the ON / OFF valve 43 provided in (2) is turned off (“closed” state).
  • the ON / OFF valve 42 (2) provided in the pipe 22 connecting the first-stage neutralization treatment tank 12A (2) and the final neutralization equipment 14 is turned on ("open” state). To do.
  • the leach slurry is transferred from the neutralization tank 12A (2) to the final neutralization facility 14 by the transfer pump 31 provided in the pipe 22.
  • the transfer operation of the leaching slurry to the final neutralization equipment 14 is performed, for example, by the nickel concentration of the leaching slurry discharged from the leaching treatment tank 11 (2) among the thickeners provided in multiple stages in the solid-liquid separation equipment 13. This is performed when the nickel concentration in the liquid phase in the stage thickener (CCD 6) is lower.
  • the valuable metal concentration of the leaching slurry at this stage that is, the stage of carrying out the transfer operation to the final neutralization facility 14 is, for example, about 0 to 5 g / L in terms of nickel.
  • the piping 22 that connects the first-stage neutralization treatment tanks 12A (1) , 12A (2) and the final neutralization equipment 14 is provided.
  • the leaching slurry discharged at the stage where the leaching process is not sufficiently advanced at the start of operation can be transferred to the final neutralization facility 14.
  • the leaching slurry having a low nickel concentration from being transferred to the solid-liquid separation step S3 or the like in the subsequent step.
  • the first stage neutralization treatment tanks 12A (1) and 12A (2) in the preliminary neutralization facility 12 are In the liquid separation equipment 13, pipes 23 that connect the respective solid-liquid separation tanks (thickeners) provided in multiple stages are connected.
  • This pipe 23 is independent from each series of the first-stage neutralization treatment tanks 12A (1) and 12A (2) , or is integrated at a predetermined location from each series, so that each solid-liquid separation tank Connected to the charging section. More specifically, the pipe 23 extends from the first-stage neutralization treatment tanks 12A (1) and 12A (2) toward the solid-liquid separation facility 13 and has multiple stages constituting the solid-liquid separation facility 13. It branches so that it may be connected with each connected solid-liquid separation tank (CCD1, CCD2, ... CCD6).
  • CCD1 solid-liquid separation tank
  • the pipe 23 is provided with a transfer pump 31, and the leaching slurry discharged from the first-stage neutralization tanks 12 A (1) and 12 A (2) is solid-liquid separated by the transfer pump 31. 13 is transferred to a predetermined solid-liquid separation tank.
  • an ON / OFF valve 42 (1) for controlling the transfer of the leaching slurry between the neutralization tanks 12A (1) , 12A (2) and the above-described transfer pump 31, for example, is provided inside the pipe 23. , 42 (2) are provided.
  • the ON / OFF valve is used.
  • 42 (1) and 42 (2) are turned on (“open” state), and the discharged leached slurry can be transferred.
  • the ON / OFF valves 42 (1) and 42 (2) provided in the pipe 23 for transferring to a predetermined solid-liquid separation tank are in an OFF state (“closed” state). It has become.
  • the pipe 23 is provided with an ON / OFF valve 44 for controlling the transfer of the leaching slurry at each branch point toward the solid-liquid separation tanks connected in multiple stages.
  • an ON / OFF valve 44 for controlling the transfer of the leaching slurry at each branch point toward the solid-liquid separation tanks connected in multiple stages.
  • the leaching process tank 11 Since the nickel concentration of the leaching slurry discharged from 2) is low, it cannot be transferred to the next step. Specifically, for example, even when the leaching treatment proceeds and the valuable metal concentration in the leaching slurry exceeds 5 g / L in terms of nickel, the leaching slurry to be transferred to the second stage neutralization treatment tank 12B. If it is lower than the desired nickel concentration, it cannot be transferred to the next step.
  • the leaching slurry is discharged from the leaching treatment tank 11 (2) , and the first stage neutralization treatment tank of the same series. Transfer to 12A (2) . Then, via a pipe 23 for connecting the the solid-liquid separation equipment 13 neutralization treatment tank 12A (2), the leach slurry is transferred from the neutralization tank 12A (2) to solid-liquid separation equipment 13.
  • the valuable metal concentration in the leaching slurry is 2.5 g / L in terms of nickel
  • the second stage where the nickel equivalent concentration in the liquid phase during normal operation (steady state) is about 2.5 g / L. It is made to transfer to the solid-liquid separation tank (CCD2) of eyes. In this way, by appropriately controlling the transfer destination according to the valuable metal concentration in the leaching slurry, it is possible to prevent the first system during normal operation from being affected, and efficient operation is possible.
  • CCD2 solid-liquid separation tank
  • the above-described self-circulation piping (first stage neutralization treatment tank 12A (2) and leaching treatment tank 11 (2) , 21 )
  • the ON / OFF valve 43 provided in (2) is turned off (“closed” state).
  • the OFF valve 45 is turned off (“closed” state).
  • the ON / OFF valve 42 (2) provided in the pipe 23 connecting the first stage neutralization treatment tank 12A (2) and the solid-liquid separation facility 13 is turned on ("open" state). To do. Then, the leaching slurry is transferred from the first-stage neutralization tank 12A (2) to the solid-liquid separation facility 13 by the transfer pump 31 provided in the pipe 23. At this time, the ON / OFF valve 44 provided at each branch point for branching to each solid-liquid separation tank in the solid-liquid separation facility 13 is controlled so that the leached slurry is transferred to the CCD 2.
  • the ON / OFF valve 44 at the branch point to the CCD 2 is turned on (“open” state), and the ON / OFF valves 44 at the other branch points to the CCD 1 and CCD 3 to CCD 6 are turned off (“ Closed state).
  • the piping 23 that connects the first-stage neutralization tanks 12A (1) and 12A (2) and the solid-liquid separation facility 13 is provided.
  • the leaching process after the start of operation is not yet sufficient and the leaching slurry having a low nickel concentration can be transferred to a predetermined solid-liquid separation tank.
  • the amount of nickel oxide ore is increased and the production amount of nickel / cobalt mixed sulfide is improved while reducing the equipment cost. Can do. Further, even if the leaching slurries obtained from a plurality of series of treatment facilities have variations in properties such as pH, the leaching slurries discharged from the respective series are merged in the second stage neutralization treatment tank 12B. Therefore, the variation can be eliminated, and the solid-liquid separation process can be performed as a uniform leaching slurry.
  • the leaching slurry having a low nickel concentration is transferred to a subsequent process at an abnormal time such as when the processing equipment is started up. This can be prevented. Thereby, the reaction failure in a post process and the fall of operational efficiency can be suppressed.
  • the leaching slurry is self-circulated or transferred to the final neutralization facility 14 or the solid-liquid separation facility 13 while In the first series, it is possible to perform a normal operation as shown by a black arrow.
  • a two-stage neutralization tank is provided, and only one first-stage neutralization tank is provided as a plurality of lines, so that one of the lines is not affected.
  • the start-up operation at the start of operation can be performed.
  • FIGS. 3 to 6 show a configuration in which some of the pipes 21, 22, and 23 used in the non-normal operation are shared pipes.
  • the transfer pump 31 for transferring the leaching slurry through the pipes 21, 22, 23 is also common.
  • the present invention is not limited to this, and it goes without saying that the pipes 21, 22, and 23 may be provided completely individually, and a transfer pump may be provided for each of them.
  • this hydrometallurgical plant 10 what is necessary is just to determine the installation method of piping suitably in consideration of a transfer route. In addition, it is preferable because the number of equipment and the cost can be reduced by sharing the sharable parts in the piping.
  • FIGS. 3 to 6 show an embodiment in which all of the pipes 21, 22, and 23 used in the non-normal operation are shown, but one or two pipes are provided. May be.
  • a leaching facility 11 having two series of leaching treatment tanks 11 (1) and 11 (2) and a two-stage neutralization treatment tank are provided, and the first-stage neutralization treatment tanks 12A (1) and 12A ( The operation is performed by the hydrometallurgical plant 10 including the pre-neutralization facility 12 in which 2) corresponds to the leaching treatment tank and the second stage neutralization treatment tank 12B is a single series. It was.
  • the solid-liquid separation equipment 13 as shown in FIG. 1, six stages of thickeners (CCD1 to CCD6) are connected to perform multi-stage cleaning.
  • the production amount of the nickel / cobalt mixed sulfide obtained in this operation was 2500 tons in terms of nickel, and there was no problem in the product quality.
  • the set values of valuable metals in the liquid phase of the CCD of each stage in the solid-liquid separation equipment 13 are nickel equivalent concentrations, CCD1: 3 g / L, CCD 2: 2.5 g / L, CCD 3: 2 g / L, CCD 4: 1.5 g / L, CCD 5: 1 g / L, CCD 6: 0.5 g / L or less.
  • the amount of nickel-cobalt mixed sulfide produced was 2075 tons (about 83% of Operation Example 1), and there was no problem in product quality.
  • the leaching failure occurred in the leaching treatment tanks 11 (1) and 11 (2) in the first series or the second series five times. For this reason, the series where the leaching failure occurred was stopped and started up five times.
  • the leaching slurry discharged from the leaching treatment tanks 11 (1) and 11 (2) being started up that is, the leaching slurry having a low nickel concentration due to insufficient leaching treatment is used as it is. It was made to transfer to the neutralization processing tank 12B of the 2nd step via the neutralization processing tank 12A (1) , 12A (2) of the step. In such start-up operation, the average time from stop to return was 2 days.
  • the production amount of the obtained nickel-cobalt mixed sulfide was 2250 tons (about 90% of the operation example 1), but the product quality deteriorated. Specifically, the ratio of valuable metals in the nickel / cobalt mixed sulfide decreased, and it became a defective product that could not be shipped as a product, which had to be disposed of.
  • Table 1 below shows the transition of the nickel concentration (g / L) in the overflow from the first-stage solid-liquid separation tank (CCD1) when operated as described above. As shown in Table 1, it can be seen that in this operation example 5, the nickel concentration is extremely stable from the start of operation. In the sulfidation reaction in the subsequent sulfidation process using this overflow liquid as a treatment target, the reaction occurred stably without causing a reaction failure or the like.
  • Table 1 below shows the transition of the nickel concentration (g / L) in the overflow from the first-stage solid-liquid separation tank (CCD1) when operated as described above. As shown in Table 1, it can be seen that the nickel concentration decreased extremely over about half a day from the start of operation. As a result, in the subsequent sulfidation step, due to the extremely low nickel concentration, adjustment of the sulfidation reaction becomes very difficult, resulting in poor sulfidation reaction and excessive sulfidation reaction.

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Abstract

La présente invention porte sur une installation hydrométallurgique permettant d'augmenter la capacité de production en traitement de minerai et donc d'atteindre une productivité accrue sans provoquer une faible réaction ou une dégradation du rendement de production. Cette installation hydrométallurgique (10) est pourvue de : un système de lixiviation (11) qui est composé de multiples lignes de lixiviation qui ont des cuves de lixiviation (11(n)) respectivement et dans lesquelles la lixiviation d'un minerai est effectuée; un système de neutralisation préliminaire (12) qui est pourvu de cuves de première neutralisation et de seconde neutralisation et dans lequel le pH d'une pulpe de lixiviation est ajusté; et un système de séparation solide-liquide (13) qui est composé d'une ligne de séparation et dans lequel la pulpe de lixiviation à pH ajusté sortant du système de neutralisation préliminaire (12) est séparée en un solide et un liquide. Le système de neutralisation préliminaire (12) est conçu de façon à ce que : de multiples cuves de première neutralisation (12A(n)) soient disposées de façon à correspondre respectivement aux cuves de lixiviation (11(n)) des multiples lignes de lixiviation; et les courants de pulpe de lixiviation, dont les valeurs de pH ont été ajustées dans les cuves de première neutralisation (12A(n)), soient réunis dans une seule ligne qui est composée d'une cuve de seconde neutralisation (12B). Les courants de pulpe de lixiviation réunis sont transférés vers le système de séparation solide-liquide (13).
PCT/JP2014/051319 2013-03-08 2014-01-23 Installation hydrométallurgique pour minerai d'oxyde de nickel et procédé pour la conduite de ladite installation hydrométallurgique WO2014136487A1 (fr)

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US14/773,496 US20160024614A1 (en) 2013-03-08 2014-01-23 Hydrometallurgical plant for nickel oxide ore and method for operating the hydrometallurgical plant
CA2904569A CA2904569A1 (fr) 2013-03-08 2014-01-23 Installation hydrometallurgique pour minerai d'oxyde de nickel et procede pour la conduite de ladite installation hydrometallurgique
EP14760507.5A EP2975142B1 (fr) 2013-03-08 2014-01-23 Installation hydrométallurgique pour minerai d'oxyde de nickel et procédé pour la conduite de ladite installation hydrométallurgique
AU2014227269A AU2014227269B2 (en) 2013-03-08 2014-01-23 Hydrometallurgical plant for nickel oxide ore and method for operating said hydrometallurgical plant
PH12015501978A PH12015501978B1 (en) 2013-03-08 2015-09-07 Hydrometallurgical plant for nickel oxide ore and method for operating said hydrometallurgical plant

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JP2013046986A JP5569611B1 (ja) 2013-03-08 2013-03-08 ニッケル酸化鉱石の湿式製錬プラント、並びにその湿式製錬プラントの操業方法

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JP5679372B2 (ja) 2013-07-03 2015-03-04 住友金属鉱山株式会社 製鉄用ヘマタイトの製造方法
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CN205810815U (zh) * 2016-07-13 2016-12-14 京东方科技集团股份有限公司 一种有机发光显示面板
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AU2014227269B2 (en) 2018-05-10
AU2014227269A1 (en) 2015-09-24
JP2014173136A (ja) 2014-09-22
PH12015501978A1 (en) 2016-01-18
PH12015501978B1 (en) 2016-01-18
EP2975142A1 (fr) 2016-01-20
JP5569611B1 (ja) 2014-08-13
US20160024614A1 (en) 2016-01-28
CA2904569A1 (fr) 2014-09-12
EP2975142A4 (fr) 2016-12-07

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