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WO2018101069A1 - Procédé de métallurgie humide pour minerai d'oxyde de nickel - Google Patents

Procédé de métallurgie humide pour minerai d'oxyde de nickel Download PDF

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Publication number
WO2018101069A1
WO2018101069A1 PCT/JP2017/041381 JP2017041381W WO2018101069A1 WO 2018101069 A1 WO2018101069 A1 WO 2018101069A1 JP 2017041381 W JP2017041381 W JP 2017041381W WO 2018101069 A1 WO2018101069 A1 WO 2018101069A1
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WO
WIPO (PCT)
Prior art keywords
nickel
solution
hydrogen sulfide
neutralization
oxide ore
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/041381
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English (en)
Japanese (ja)
Inventor
智暁 米山
敬介 柴山
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Metal Mining Co Ltd
Original Assignee
Sumitomo Metal Mining Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2017002344A external-priority patent/JP6350684B2/ja
Application filed by Sumitomo Metal Mining Co Ltd filed Critical Sumitomo Metal Mining Co Ltd
Priority to AU2017369155A priority Critical patent/AU2017369155B2/en
Priority to EP17876261.3A priority patent/EP3550040A4/fr
Publication of WO2018101069A1 publication Critical patent/WO2018101069A1/fr
Priority to PH12019501187A priority patent/PH12019501187B1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a hydrometallurgical method by high-pressure acid leaching of nickel oxide ore, and particularly to a hydrometallurgical method capable of increasing the nickel recovery rate.
  • HPAL high pressure acid leach
  • the treatment is generally performed in accordance with the following steps (a) to (d).
  • a reaction vessel such as an autoclave
  • valuable materials such as nickel and cobalt contained in the nickel oxide ore are leached, and after leaching, the slurry is taken out from the reaction vessel and separated into a leaching solution containing nickel and cobalt and a leaching residue by a settling tank. Liquid separation process.
  • a dezincification step in which the added sulfurized starch (also referred to as zinc starch) is solid-liquid separated to obtain a post-dezincification solution (also referred to as dezincification final solution) by adding while controlling.
  • D A nickel recovery step of separating and recovering the mixed sulfide after adding a sulfiding agent to the post-dezinced solution to form a nickel cobalt mixed sulfide.
  • Patent Document 1 discloses a wet smelting method using the above-described high-pressure acid leaching method, and this wet smelting method was obtained by a leaching step of leaching nickel oxide ore with sulfuric acid and then solid-liquid separation.
  • a leaching residue is appropriately added to the leachate in the neutralization step, the pH of the neutralization final solution is adjusted to 3.0 to 3.5, and the neutralization final solution is further removed in the dezincing step.
  • a sulfidation reaction was carried out in a state in which a suspension of neutralized starch and leach residue remained in the neutralized final solution so that the turbidity of the solution became 100 to 400 NTU (Nephelometric Turbidity Unit).
  • the slurry containing the sulfide starch is subjected to solid-liquid separation in the filtration step in the dezincification step to obtain the sulfide starch and a final solution containing nickel and cobalt.
  • the conditions for producing a nickel sulfide starch and the conditions for producing a zinc sulfide starch in the dezincification step are close to each other.
  • nickel co-precipitated into the material, resulting in loss. Since the recovery rate of nickel greatly affects the economics of the process, it is desired to reduce the nickel loss as much as possible.
  • the present invention has been made in view of such a situation.
  • An object of the present invention is to provide a hydrometallurgical method capable of increasing the nickel recovery rate by reducing the amount of nickel to be precipitated.
  • the present inventors added a sulfidizing agent to the post-neutralization solution after neutralization of the leachate obtained by high-pressure acid leaching of nickel oxide ore, and dezincation reaction (sulfurization reaction) by sulfurization. 2), two or more reaction tanks for the dezincification reaction are provided, they are connected in series, and the distribution ratio of hydrogen sulfide gas blown into the reaction tanks is adjusted to increase the nickel recovery rate.
  • the present inventors have found that this can be done and have completed the present invention.
  • the method for hydrometallizing nickel oxide ore according to the present invention includes a leaching step in which leaching residue is removed after acid leaching of nickel oxide ore under high pressure to obtain a leachate, and a neutralizing agent is added to the leachate.
  • a nickel recovery process for recovering nickel as a sulfide by adding a sulfiding agent to the solution after dezincing, and the hydrogen sulfide gas in the dezincing step The second and subsequent steps from the top of the total amount of hydrogen sulfide gas blown into all the reaction tanks while the post-neutralized solution was sequentially flowed into two or more reaction tanks connected in series. 50% or more of hydrogen sulfide gas blown into the reaction tank It is characterized by adjusting below 0%.
  • the amount of nickel co-precipitated with impurities such as zinc and copper can be reduced to increase the nickel recovery rate.
  • the raw material nickel oxide ore is finely granulated by a crushing means such as a crusher, and then water is added to form a slurry. After the addition, it is charged into a pressure vessel such as an autoclave and subjected to sulfuric acid leaching treatment at a high temperature and high pressure of, for example, 240 to 280 ° C. to leach valuable nickel and cobalt.
  • the slurry obtained by the sulfuric acid leaching is washed in multiple stages, and then the leaching residue is removed from the slurry by solid-liquid separation to obtain a leachate containing nickel, cobalt, and impurity elements.
  • an alkali such as slaked lime or calcium carbonate is added to the leachate as a neutralizing agent, and the pH of the leachate is adjusted to precipitate the impurity elements as neutralized starch.
  • a flocculant (coagulant) is added to the slurry containing the neutralized starch, followed by solid-liquid separation to remove the neutralized starch, thereby obtaining a neutralized final solution containing nickel and cobalt.
  • the zinc removal step S4 hydrogen sulfide gas as a sulfiding agent is blown into the neutralized final solution to produce a sulfide containing zinc (zinc sulfide), and the slurry containing the sulfide is solidified. By separating the liquid, zinc sulfide is removed to obtain a liquid after dezincing.
  • nickel recovery step S5 a nickel-cobalt mixed sulfide containing nickel and cobalt is generated by adding a sulfiding agent such as hydrogen sulfide gas to the solution after dezincing, and a slurry containing the nickel-cobalt mixed sulfide is produced.
  • the nickel-cobalt mixed sulfide is recovered by solid-liquid separation and a post-sulfurized liquid (poor liquid) is obtained. This poor solution may be repeated in the solid-liquid separation step S2 as shown in FIG. 1 as necessary.
  • zinc is selectively precipitated and precipitated as sulfides in the dezincing step S4 to separate it from nickel and cobalt.
  • two or more reaction tanks for performing a sulfurization reaction by blowing hydrogen sulfide gas into the neutralized final liquid are provided, and the neutralized final liquid obtained in the neutralization process flows in order by connecting the plurality of reaction tanks in series.
  • the ratio of the amount of hydrogen sulfide gas blown into the reaction tanks after the first tank in the series of reaction tanks connected in series hereinafter referred to as “blowing”). (Also referred to as “compression ratio”) to an appropriate range.
  • compression ratio the amount of nickel co-precipitated with impurities such as zinc and copper can be reduced, and the nickel recovery rate can be increased.
  • the dezincing step S4 the No. 1 reaction tank, No. 2 reaction tank, No. 3 reaction tank, etc. from the top in the order in which the neutralization final solution flows through the reaction tank in which the dezincification reaction is performed.
  • the reactor is composed of n reactors in the No. n reactor, the No. 2 reactor and the subsequent reactors with respect to the total amount of hydrogen sulfide gas injected into all reactors from the No. 1 reactor to the No. n reactor.
  • the amount of hydrogen sulfide gas blown into (n-1) reactors ie, the blow ratio) is adjusted within the range of 50% to 90%. Thereby, the amount of nickel co-precipitated with impurities such as zinc and copper can be reduced.
  • the particle size of the sulfide starch can be increased.
  • the particle size of a sulfide starch becomes large by setting a blowing ratio high as above-mentioned, filterability improves.
  • the blowing ratio in order to improve solid-liquid separation in addition to improving the nickel recovery rate, it is preferable to adjust the blowing ratio within the range of 60 to 90%, and within the range of 60 to 85%. More preferably.
  • the liquid passing capacity of the filtration device is improved, so that productivity can be increased.
  • the reason why the particle size of the dezincified starch grows large by increasing the blowing ratio in this way is that when the blowing ratio is increased, in the No.
  • the impurities including zinc generated at the early stage of the sulfurization reaction This is because the number of fine particles made of sulfide decreases, and as a result, sulfide grows with these few fine particles as nuclei (also referred to as “seed”) in the No. 2 reaction tank and later.
  • the proportion of hydrogen sulfide gas blown into the No. 1 reaction tank is relatively high, and as a result, fine zinc sulfide particles that serve as nuclei in the No. 1 reaction tank Is excessively generated, and after the No. 2 reactor, the sulfide grows with these many fine particles as nuclei, so it is difficult to obtain a zinc sulfide having a large particle size.
  • the blowing ratio exceeds 90%, the production of fine zinc sulfide as a nucleus in the No. 1 reaction tank is suppressed, so the number of seeds is insufficient. Growth may be insufficient.
  • seeds can be stably generated by blowing more than 10% and less than 40% of the hydrogen sulfide gas supplied to the entire reaction tank into the No. 1 reaction tank.
  • the specific blowing ratio may be appropriately adjusted so that the particles grow to such an extent that the filter cloth is not easily clogged during the subsequent filtration process.
  • the reaction tank located at the end may serve as a buffer tank without blowing hydrogen sulfide gas so much.
  • the reaction time can be ensured in the buffer tank even if a short path of the processing liquid occurs in the reaction tank located upstream of the reaction tank. , A decrease in the overall reaction efficiency can be suppressed.
  • the waste of equipment costs and energy costs increases, and the slurry retained in these excess reaction tanks is oxidized by the entrained air and dezinced.
  • the number of reaction tanks for performing the dezincification reaction is preferably 3 tanks or less because problems such as re-dissolution of starch may occur. Further, separately prepared zinc sulfide or zinc sulfide recovered by solid-liquid separation may be supplied as seed to the No. 1 reaction tank, whereby a coarser zinc sulfide can be generated.
  • the dezincing reaction in the range of pH 2.5 to 3.5.
  • pH 2.5 zinc once converted to sulfide may be redissolved and separation of zinc may be insufficient.
  • the pH exceeds 3.5 elements that are not subject to removal, such as iron and nickel, may precipitate, increasing the starch load on the filter cloth and filter during the subsequent filtration process, In the case of iron or the like, a lot of fine starch is generated, so that the filter cloth is clogged. Therefore, it is necessary to backwash the filter cloth frequently in order to ensure a sufficient flow rate, and the production efficiency decreases. There is a fear.
  • the nickel oxide ore was hydrometallized by high-temperature and high-pressure leaching along the process flow shown in FIG. 1, and nickel was recovered in the form of sulfide. Specifically, nickel oxide ore consisting of laterite, saprolite, and limonite ore is put together with sulfuric acid into an autoclave as a pressurized vessel, heated to a temperature of 240-260 ° C with a steam heater, and high pressure pressurized leaching is performed. Thereafter, the leaching residue was solid-liquid separated from the obtained leaching slurry to obtain a leaching solution.
  • a neutralized starch is produced by adding slaked lime as a neutralizing agent to the leachate and adjusting the pH to a range of 3.0 to 3.5, and then adding an anionic flocculant to the neutralized starch. The product was removed by solid-liquid separation to obtain a neutralized final solution.
  • the ratio of the amount of hydrogen sulfide gas blown into the No. 2 reaction vessel and No. 3 reaction vessel that is, the blowing ratio, with respect to the amount of hydrogen sulfide gas blown into all three reaction vessels. It was gradually changed within the range from 5.1% to 86.3%.
  • the sulfidized liquid extracted from the No. 3 reaction tank at the end was supplied to a Buchner funnel having a filter cloth on a 60 cm diameter filter panel provided with a large number of filtration holes, and the filtrate side was evacuated. Solid-liquid separation was performed by suction.
  • zinc sulfides (dezincified starches) of Samples 1 to 46 produced under conditions with different blowing ratios were obtained. Note that most of the hydrogen sulfide gas was blown into the No. 2 reaction tank and No. 3 reaction tank, and the zinc sulfide grown in the No. 2 reaction tank was in a dissolved state.
  • the No. 3 reaction tank was used as a place for finishing the growth by reacting with the residual hydrogen sulfide gas. Specifically, the amount of injection into the No. 3 reaction tank was adjusted appropriately as long as the injection ratio was not changed in accordance with the growth state of the sampled zinc sulfide particle diameter.
  • Table 1 below shows the blowing ratio when the zinc sulfides of Samples 1 to 46 are generated and the particle sizes of the zinc sulfides generated under these conditions. Moreover, the graph which plotted the relationship between these blowing ratio and the particle size of zinc sulfide is shown in FIG.
  • the particle size of zinc sulfide was measured using a microtrack while observing a sample collected during steady operation with a microscope. During the production of zinc sulfide of these samples 1 to 46, the pH of the slurry in the reaction vessel was maintained within the range of 2.7 to 2.9 and the liquid temperature within the range of 60 to 67 ° C.
  • composition of this neutralized final solution was within the range of nickel concentration of 3.5 to 4.0 g / L, iron concentration of 0.7 to 1.4 g / L, and zinc concentration of 60 to 140 mg / L. It was.
  • the zinc concentration in the solution after dezincing was reduced to about 5 to 12 mg / L.
  • the nickel quality in the zinc sulfide can be reduced to 1% or less by setting the blowing ratio to 50% or more.
  • the particle size of zinc sulfide should be approximately 10 ⁇ m or more, and this indicates that the blowing ratio of hydrogen sulfide gas is approximately from Table 1 and FIG. It can be seen that it should be 60% or more.
  • the effect of improving the filterability is also obtained.

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  • Manufacturing & Machinery (AREA)
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  • Environmental & Geological Engineering (AREA)
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Abstract

La présente invention améliore le taux de récupération de nickel dans une étape de dézingage pour éliminer le zinc contenu dans un minerai d'oxyde de nickel dans la métallurgie humide, qui utilise une lixiviation acide à haute pression du minerai. Un procédé de métallurgie humide comprend : une étape de lixiviation S1 consistant à lixivier par voie acide un minerai d'oxyde de nickel sous haute pression pour obtenir un lixiviat ; une étape de neutralisation S3 consistant à éliminer un précipité de neutralisation généré par l'addition d'un agent neutralisant audit lixiviat et à obtenir une solution de postneutralisation ; une étape de dézingage S4 consistant à éliminer le précipité de zinc généré par le soufflage de sulfure d'hydrogène gazeux dans ladite solution de postneutralisation pour obtenir une solution de postdézingage ; et une étape de récupération de nickel S5 consistant à ajouter un agent de sulfuration à ladite solution de postdézingage et à récupérer le nickel sous la forme d'un sulfure. Lorsque le sulfure d'hydrogène gazeux est insufflé, ladite solution de postneutralisation passe successivement à travers de multiples cuves de réaction qui sont reliées en série tandis que le volume de sulfure d'hydrogène gazeux soufflé dans la deuxième cuve de réaction à partir du dessus et dans les cuves de réaction subséquentes est ajusté à 50 % jusqu'à 90 % du volume total du sulfure d'hydrogène gazeux soufflé dans toutes les cuves de réaction.
PCT/JP2017/041381 2016-11-30 2017-11-16 Procédé de métallurgie humide pour minerai d'oxyde de nickel Ceased WO2018101069A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2017369155A AU2017369155B2 (en) 2016-11-30 2017-11-16 Wet metallurgy method for nickel oxide ore
EP17876261.3A EP3550040A4 (fr) 2016-11-30 2017-11-16 Procédé de métallurgie humide pour minerai d'oxyde de nickel
PH12019501187A PH12019501187B1 (en) 2016-11-30 2019-05-29 Hydrometallurgical method for nickel oxide ore

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2016-232416 2016-11-30
JP2016232416 2016-11-30
JP2017-002344 2017-01-11
JP2017002344A JP6350684B2 (ja) 2016-11-30 2017-01-11 ニッケル酸化鉱石の湿式製錬方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2023031095A (ja) * 2021-08-24 2023-03-08 住友金属鉱山株式会社 濾過設備の運転方法、脱亜鉛処理方法、及び、ニッケル酸化鉱石の製錬方法
WO2025129468A1 (fr) * 2023-12-19 2025-06-26 宜昌邦普宜化新材料有限公司 Procédé et appareil d'élimination de chrome d'un lixiviat de ferronickel

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004305917A (ja) * 2003-04-07 2004-11-04 Sumitomo Metal Mining Co Ltd 硫酸ニッケル水溶液からの亜鉛の除去方法
JP2010031302A (ja) * 2008-07-25 2010-02-12 Sumitomo Metal Mining Co Ltd ニッケル酸化鉱石の湿式製錬方法
JP2010037626A (ja) 2008-08-07 2010-02-18 Sumitomo Metal Mining Co Ltd 亜鉛硫化物の分離方法
JP2015028219A (ja) * 2009-10-19 2015-02-12 住友金属鉱山株式会社 ニッケル酸化鉱石の湿式精錬プラントおよびその操業方法
WO2016139858A1 (fr) * 2015-03-05 2016-09-09 住友金属鉱山株式会社 Procédé pour la production de sulfure de nickel et procédé hydrométallurgique pour minerai d'oxyde de nickel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004305917A (ja) * 2003-04-07 2004-11-04 Sumitomo Metal Mining Co Ltd 硫酸ニッケル水溶液からの亜鉛の除去方法
JP2010031302A (ja) * 2008-07-25 2010-02-12 Sumitomo Metal Mining Co Ltd ニッケル酸化鉱石の湿式製錬方法
JP2010037626A (ja) 2008-08-07 2010-02-18 Sumitomo Metal Mining Co Ltd 亜鉛硫化物の分離方法
JP2015028219A (ja) * 2009-10-19 2015-02-12 住友金属鉱山株式会社 ニッケル酸化鉱石の湿式精錬プラントおよびその操業方法
WO2016139858A1 (fr) * 2015-03-05 2016-09-09 住友金属鉱山株式会社 Procédé pour la production de sulfure de nickel et procédé hydrométallurgique pour minerai d'oxyde de nickel

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of EP3550040A4 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2023031095A (ja) * 2021-08-24 2023-03-08 住友金属鉱山株式会社 濾過設備の運転方法、脱亜鉛処理方法、及び、ニッケル酸化鉱石の製錬方法
JP7700576B2 (ja) 2021-08-24 2025-07-01 住友金属鉱山株式会社 濾過設備の運転方法、脱亜鉛処理方法、及び、ニッケル酸化鉱石の製錬方法
WO2025129468A1 (fr) * 2023-12-19 2025-06-26 宜昌邦普宜化新材料有限公司 Procédé et appareil d'élimination de chrome d'un lixiviat de ferronickel

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