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WO2019203680A1 - Procédé de récupération de nickel et de cobalt à partir de minerais latéritiques ferrugineux - Google Patents

Procédé de récupération de nickel et de cobalt à partir de minerais latéritiques ferrugineux Download PDF

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Publication number
WO2019203680A1
WO2019203680A1 PCT/RU2018/000254 RU2018000254W WO2019203680A1 WO 2019203680 A1 WO2019203680 A1 WO 2019203680A1 RU 2018000254 W RU2018000254 W RU 2018000254W WO 2019203680 A1 WO2019203680 A1 WO 2019203680A1
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WIPO (PCT)
Prior art keywords
ore
nickel
cobalt
roasting
recovery
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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/RU2018/000254
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English (en)
Inventor
Guseingulu Bakhlul Ogly SADYKHOV
Leonid Borisovich TSYMBULOV
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.)
OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "VI KHOLDING"
Original Assignee
OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "VI KHOLDING"
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Priority to PCT/RU2018/000254 priority Critical patent/WO2019203680A1/fr
Publication of WO2019203680A1 publication Critical patent/WO2019203680A1/fr
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
    • C22B23/005—Preliminary treatment of ores, e.g. by roasting or by the Krupp-Renn process
    • 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

Definitions

  • the invention relates to the field of non-ferrous metallurgy, in particular to a method for recovery of nickel and cobalt from laterite ores.
  • nickel reserves are concentrated in laterite ores, which, according to their chemical and mineral composition, are divided into ferruginous (limonite) and magnesium silicate (saproiite) ores.
  • ferruginous ores accounts for about 70% of the nickel and of saproiite ores about 30%.
  • Magnesium silicate nickel ores are processed by pyrometallurgical methods, and ferruginous ores by hydrometallurgical methods.
  • Hydrometallurgical processing of laterite ores is carried out in two variants (Reznik I.D., Emiakov G.P., Shneerson Ya.M.“Nickel (Current state of hydrometallurgy of oxidized nickel ores)”. - Moscow: Science and Technology, 2001, vol.2, pp. 364-464); Dr.Sc. Ashok D. Dalvi; Dr. W. Gordon Bacon; Mr. Robert C. Osborne.“The Past and the Future of Nickel Laterites”// PDAC 2004 International Convention, Trade Show & Investors Exchange.
  • ammonium- carbonate technology which is based on the principle of selective recovery of Ni and Co from the ore.
  • the technology includes the following main steps: drying the ore, grinding, reduction of the grinded ore under conditions that ensure selective reduction of nickel and cobalt, cooling the reduced ore in an inert atmosphere, and leaching the ore in an ammonium- carbonate solution by air aeration with transfer of nickel and cobalt into a solution, and iron into an insoluble constituent.
  • the preliminary reduction roasting of the ore ensures selectivity of the dissolution of nickel and cobalt during the leaching of the cinder.
  • the cobalt and nickel are then recovered from the solution using a variety of methods.
  • the process provides for the regeneration of the main ammonium reagent and, in part, carbon dioxide.
  • a reduction roasting in industrial conditions is carried out in the Herreshoff multiple- hearth furnaces in a temperature range of 650-750°C.
  • a reducing atmosphere in the furnace is created by sub-stoichiometric combustion of fuel.
  • the rate of reduction noticeably decreases, and the temperature increasing to 800°C and higher leads to formation of forsterite, which adversely affects the results of nickel recovery during leaching.
  • the process is carried out with a minimum degree of reduction of iron in its oxides to a metal state, with its content in the reduced ore in the range 2.0-2.5%.
  • the increased content of metallic iron leads to a deterioration in the recovery of nickel and cobalt in the subsequent ammonium carbonate leaching of the cinder.
  • the ground ore is mixed with heavy oil, in particular with fuel oil, in an amount of about 2.5% of the ore mass.
  • the cinder After reduction roasting, the cinder is cooled to 150-250°C in an inert atmosphere in water refrigerators (multi-disk type), then the cinder from the refrigerator is unloaded into a chute, into which an ammonium solution containing 65-85 g/1 of N3 ⁇ 4 and 35-45 g/1 of C0 2 is fed.
  • the total leaching time is 2.0-2.5 hours.
  • the nickel- and cobalt-containing solution is separated from the ore tailings and sent to recover nickel and cobalt by known methods, in particular by distillation process or in its combination with other methods such as liquid extraction, ion exchange and precipitation.
  • the distillation process is carried out in conventional distillation multi-sectional columns by heating the solution with an acute steam to 100-1 l0°C.
  • the sublimable ammonium and carbon dioxide are absorbed by water and returned to the leaching process as a working solution.
  • the process is simple to operate, but it is very sensitive to changes in the basic leaching parameters (temperature, ammonium concentration in the solution, etc.), requires high energy costs and is environmentally unsafe.
  • An increase in the recovery of nickel and cobalt is possible if the following conditions are met: increasing the leaching temperature; increasing of concentrations of N3 ⁇ 4 and C0 2 in the ammonium-carbonate solution, increasing of the ratio of the liquid phase to the solid phase, i.e. increasing of the specific volume of the ammonium-carbonate solution with respect to the roasted ore; exclusion or minimization of sulfur content in the process scheme.
  • the set of the above-mentioned disadvantages does not offer the possibility of significant improving of parameters of ammonium-carbonate technology.
  • US Pat. No. 3,656,934 proposes a selective reduction of limonite ore containing from 38 to 46% Fe total and approximately 1.5% Ni in a rotary furnace, followed by leaching of the reduced ore with an ammonium-carbonate solution.
  • Reduction roasting of the ore is carried out with additives of up to 5% coal and 1% pyrite (sulfur-containing additive) when a gaseous reducing agent is supplied in several places along the furnace.
  • pyrite sulfur-containing additive
  • the closest in terms of technical essence is the method of recovery of nickel and cobalt from laterite ores (patent RU 2333972).
  • the dried and ground laterite ore consisting of either limonite ore or saprolite ore, or a mixture of these two ores is fed to a rotary furnace which is heated by sub-stoichiometric combustion of fuel (oil fuel or gas) to create a reducing atmosphere in the furnace.
  • the reducing atmosphere in the rotary kiln is maintained by controlling the hydrogen and carbon monoxide content in the gas mixture.
  • the temperature in the reduction zone of the roasting furnace can be varied within the range of 600-850°C, preferably 700-8 l0°C.
  • the total residence time of the ore in the furnace can vary from 65 to 260 minutes, depending on the rotational speed of the furnace, and the residence time in the reduction zone at a temperature above 600°C can vary from 13 to 52 minutes. It is allowed to use up to 2.5% (by weight of ore) reducing agent, in particular heavy oil, as additives in grinded ore to intensify the reduction of nickel and cobalt at lower temperatures (600-650°C).
  • the reduced ore After roasting, the reduced ore is cooled to a temperature of 150 to 300°C in a nonoxidizing atmosphere, then passivated with an ammonium-carbonate solution.
  • the reduced ore with air aeration is leached in an ammonium- carbonate solution containing 70-150 g/l of NH 3 and 50-100 g/l of C0 2 , at atmospheric pressure and temperatures from 35 to 60°C.
  • for leaching was used a solution only with a concentration of 100 g/l of NH 3 and 80 g/l of CO2, and the leaching temperature was not indicated.
  • the solution is separated from the ore tailings and sent to the recovery of nickel and cobalt using known methods. It was noted that in the optimal conditions for the recovery of limonite ore and ammonium-carbonate leaching, the degree of nickel recovery can reach 92-93%, and cobalt - 66-69%.
  • the reduced ore is leached in an ammonium-carbonate solution with a high concentration of NH 3 (100 g/l) in the temperature range 35-60°C at atmospheric pressure.
  • an increase in the ammonium concentration above 85 g/l is considered impractical, due to a significant increase in ammonium loss even at relatively low temperatures of 30-40°C.
  • the invention solves the problem of providing with a method for recovering nickel and cobalt from laterite ores with high technical and economic parameters (high recovery rate, reducing reagent consumption, environmental safety) by replacing the ammonium-carbonate leaching technology with the sulfuric acid leaching of the reduced ore.
  • the inventors carried out numerous diverse studies and found out that nickel and cobalt can be leached with sulfuric acid from laterite ore cinder produced after reduction roasting of the ore.
  • a method including ore grinding, roasting of ore in a reducing atmosphere for the selective reduction of nickel and cobalt, cooling the reduced ore in a nonoxidizing atmosphere to a temperature of l50-300°C, and leaching the cooled cinder with transferring nickel and cobalt into the solution
  • the roasting the ore in a reducing atmosphere is carried out in the temperature range 700-800°C, preferably at 725-775°C
  • the cooled cinder is leached with sulfuric acid in a weakly acidic medium at a pH of 1.4-3.5, preferably at a pH of 2.5-3.0, at a temperature of 30-l00°C, preferably at 85-95°C for 45-120 minutes, preferably 60-90 minutes.
  • the ore Before the roasting, the ore is preferably mixed with a reducing agent, for which is used brown (subbituminous) coal in an amount of 3-3.5% of the mass of the ore.
  • a reducing agent for which is used brown (subbituminous) coal in an amount of 3-3.5% of the mass of the ore.
  • petroleum fuel such as fuel oil
  • fuel oil can be used as a reducing agent.
  • the ore roasting process is carried out in a tubular rotary furnace or in a vertical multiple-hearth furnace.
  • a reducing atmosphere can be created by controlling the H 2 and CO content in the gas atmosphere in the furnace.
  • Reduction roasting of laterite ore is a well-known process in the industry.
  • roasting of laterite ore in reducing atmosphere at lower temperatures of 700-800°C practically eliminates formation of the phase of wustite FeO, (Fe 2 0 3 is reduced to Fe30 4 ), which is readily soluble in weakly acidic solutions of the phase, and this process substantially limits the consumption of sulfuric acid in the leaching.
  • the specific consumption of sulfuric acid is 90-130 kg per 1 ton of ore at pH 2.5-3.0, then at a temperature of 850°C and 900°C consumption of acid increases to 180 kg and 215 kg, respectively.
  • the reduction rate is markedly reduced, and in order to achieve the required degree of reduction of nickel and cobalt, it is necessary to increase the duration of the process, which is economically unprofitable due to an increase in energy costs.
  • brown coal In the case of using brown coal, the step of mixing ore with a reducing agent before roasting is simplified.
  • Reducing atmosphere is created by controlling the content of H 2 and CO, which are produced during the combustion of fuel (methane) in the gas atmosphere of the furnace.
  • Carrying out roasting without reducing agent additives requires creating conditions for additional supply of the gas reducing agent to the low-temperature (400-650°C) zone of the rotary kiln, which significantly complicates its design.
  • the total residence time of the ore in the reduction zone of the rotary kiln, where the temperature is above 400°C, can be from 60 to 120 minutes, and above 600°C from 30 to 60 minutes, depending on the speed of rotation of the kiln, the types and composition of laterite ores used and the roasting temperature.
  • Reduction roasting of laterite ore can be carried out in multiple-hearth furnaces. Although these furnaces do not always ensure sufficient conversion efficiency of nickel and cobalt due to poor contact of gas and solids, internal“breakthrough” of solids and reducing gas, and also due to poor temperature control, it is easier to regulate the reducing atmosphere in multiple-hearth furnaces than in rotating kilns.
  • Leaching after cooling of laterite ore cinder, reduced under optimal conditions, with sulfuric acid in a weakly acidic medium at pH of 1.5-3.0 permits, firstly, to achieve a high degree of selective extraction of nickel (up to 87-99%) and cobalt (up to 75 -80%) to the solution, and secondly, to significantly improve the conditions of the hydrometallurgical processing: carry out the leaching at sufficiently low ratios of L:S (2.5-3): 1 and without air aeration, remove the hard restriction of the upper limit of the leaching temperature and expand it temperature range from 30-40 to 30-l00°C, to simplify the separation of leached solution from ore tailings and the operations of separation of metals from the solution, and, at the same time, to minimize the environmental load due to elimination of ammonium from the process cycle.
  • the proposed method eliminates the negative effect of sulfur in the reduced cinder on the recovery of cobalt and other parameters of the leaching process, i.e. there are no special requirements for the reducing agent and fuel for the
  • the advantage of using weak solutions of sulfuric acid for leaching of the reduced laterite ore cinder is due to the following main factors.
  • First, unlike ammonium or ammonium- carbonate solutions, diluted solutions of sulfuric acid are practical for leaching in a wide temperature range from 30 to 100°C due to the absence of the release of aggressive and environmentally harmful gases, and second, in sulfuric acid solutions, iron, nickel and cobalt ions are more stable than in ammonium-carbonate solutions, which allows leaching to be carried out at essentially low ratios of L:S (2.5-3): 1 (2-2.5 times less than during ammonium-carbonate leaching in the known analogues) without loss of nickel and cobalt.
  • Ni + Fe 2 (S0 ) 3 NiS0 + 2FeS0 4
  • Co + Fe 2 (S0 4 ) 3 CoS0 4 + 2FeS0 4
  • the amount of iron that passes into the solution essentially depends on pH and leaching temperature, it increases with increasing pH and increasing temperature. Therefore, to limit the dissolution of magnetite, leaching is carried out with a certain combination of these parameters. It was found that when the pH is raised from 1.5 to 2.5-3.0, the optimum leaching temperature is from 30 to 85-95°C. A decrease in pH below 1.5 results in an increase in the amount of dissolved iron in the solution and in the consumption of sulfuric acid. At pH above 3.0, hydrolysis of Fe 2 (S0 4 ) 3 in the solution can occur with the release of iron hydroxide, which is accompanied by co-precipitation of nickel and cobalt from the solution. In the proposed method leaching at higher temperatures (about 90°C) is more preferable.
  • This choice is related to the conditions for passivation of the reduced ore by a recycled solution and with the specialty of the leaching with sulfuric acid.
  • First, during the passivation of the cinder cooled to l50-300°C by recycled solution, especially at low ratios L:S (2.5-3):l, the temperature of the solution is substantially increased.
  • the most preferable ratio is in the range (2.5-3): 1.
  • the results on recovery of metals practically do not change, but the product flows increase, which is considered undesirable in industrial conditions, and at L:S below 2.5: 1, the concentration of iron in the solution increases, which may promote hydrolysis of ferric sulfate under leaching conditions, particularly at an elevated pH (at pH-3).
  • the sulfuric acid leaching of the reduced ferruginous laterite ore at specified pH values is carried out for 45-120 minutes, preferably 60-90 minutes. Decreasing of the leaching time, although it allows a little decrease in the consumption of sulfuric acid, does not always ensure the maximum degree of recovery of metals into the solution. Increasing the leaching time for more than 90 minutes does not lead to a noticeable improvement in the recovery results, but the consumption of acid slightly increases, which is not very acceptable.
  • the method of recovery of nickel and cobalt can be used for both ferruginous (limonite) and mixed (mixture of ferruginous and magnesium-silicate) laterite ores.
  • the presence of silicate ore in the mixture leads to an increase in the specific consumption of acid during leaching due to transition of magnesium to solution.
  • specific consumption of sulfuric acid at pH 3 does not exceed 100 kg per ton of ore, in the case of magnesium-silicate ore, the acid consumption reaches 250 kg/ton.
  • Table 2 shows examples of the implementation of the method with various process parameters. Examples with optimal recovery rates of nickel and cobalt are shown in bold in the table.
  • the use of the inventive method for recovery of nickel and cobalt from ferruginous laterite ores offers a means to: - ensure a high degree of recovery of nickel (up to 99%) and cobalt (up to 83%) from laterite ores;
  • the leaching period is usually 2-2.5 hours
  • the invention can be applied to the processing of ferruginous laterite ores and their mixture with magnesium silicate laterite (saprolite) ores of various deposits for the rational use of natural resources.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention concerne le domaine de la métallurgie non ferreuse, en particulier un procédé pour le traitement de minerais de nickel latéritiques avec récupération de nickel et de cobalt. Selon un procédé impliquant le broyage du minerai, le grillage du minerai dans une atmosphère réductrice pour la réduction sélective du nickel et du cobalt, le refroidissement du minerai réduit dans une atmosphère non oxydante à une température de 150 à 300 °C et la lixiviation des scories refroidies avec un transfert du nickel et du cobalt vers la solution, le grillage du minerai dans une atmosphère réductrice est effectué dans la plage de température de 700 à 800 °C, de préférence à 725 à 775 °C, et les scories refroidies sont lixiviées avec de l'acide sulfurique dans un milieu faiblement acide à un pH de 1,4 à 3,5, de préférence à un pH de 2,5 à 3,0, à une température de 30 à 100 °C, de préférence à 85 à 95 °C pendant 45 à 120 minutes, de préférence pendant 60 à 90 minutes. Avant le grillage, le minerai est de préférence mélangé avec un agent réducteur : du charbon brun (subbitumineux) dans une quantité de 3 à 3,5 % du poids du minerai. En outre, un carburant pétrolier, tel que du mazout, peut être utilisé en tant qu'agent réducteur. Le traitement de grillage est effectué dans le four rotatif ou dans un four à foyer multiple vertical. Pour une réduction sélective du nickel et du cobalt pendant le grillage, une atmosphère réductrice peut être créée par régulation de la teneur en ¾ et en CO dans l'atmosphère gazeuse du four. Dans ces conditions, le degré de récupération du nickel à partir du minerai est de 88 à 99 %, et le degré de récupération du cobalt est de 73 à 84 %. Lorsque le traitement est effectué dans les paramètres établis, avec la réalisation d'un degré élevé de récupération de métal, le matériau s'écoule dans la conversion hydrométallurgique en diminuant de 2 à 2,5 fois, et les paramètres techniques et économiques du traitement dans son ensemble sont améliorés.
PCT/RU2018/000254 2018-04-20 2018-04-20 Procédé de récupération de nickel et de cobalt à partir de minerais latéritiques ferrugineux Ceased WO2019203680A1 (fr)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115747517A (zh) * 2022-11-29 2023-03-07 昆明理工大学 从低品位红土镍矿中超声强化提取镍钴的方法
WO2024207242A1 (fr) * 2023-04-04 2024-10-10 广东邦普循环科技有限公司 Procédé de traitement intégré à chaîne complète de minerai de latérite de nickel

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB658199A (en) * 1948-10-06 1951-10-03 Erie Mining Co Process for reducing the ferric oxide content of ferruginous ore materials
US20060263282A1 (en) * 2003-01-30 2006-11-23 Francis Boyd R Process for nickel and cobalt extraction from laterite ores
WO2015071547A1 (fr) * 2013-11-15 2015-05-21 Outotec (Finland) Oy Procédé et système permettant de séparer du nickel et du cobalt de latérites de nickel et de solutions de lixiviation de latérite de nickel
CN107893141A (zh) * 2017-11-15 2018-04-10 东北大学 一种复杂难选铁矿石预还原‑冶炼‑铸轧全流程工艺

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB658199A (en) * 1948-10-06 1951-10-03 Erie Mining Co Process for reducing the ferric oxide content of ferruginous ore materials
US20060263282A1 (en) * 2003-01-30 2006-11-23 Francis Boyd R Process for nickel and cobalt extraction from laterite ores
WO2015071547A1 (fr) * 2013-11-15 2015-05-21 Outotec (Finland) Oy Procédé et système permettant de séparer du nickel et du cobalt de latérites de nickel et de solutions de lixiviation de latérite de nickel
CN107893141A (zh) * 2017-11-15 2018-04-10 东北大学 一种复杂难选铁矿石预还原‑冶炼‑铸轧全流程工艺

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115747517A (zh) * 2022-11-29 2023-03-07 昆明理工大学 从低品位红土镍矿中超声强化提取镍钴的方法
WO2024207242A1 (fr) * 2023-04-04 2024-10-10 广东邦普循环科技有限公司 Procédé de traitement intégré à chaîne complète de minerai de latérite de nickel

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