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WO2009026683A1 - Procédé hydrométallurgique utilisant de la résine en solution neutralisée d'un effluent de lixiviation en tas - Google Patents

Procédé hydrométallurgique utilisant de la résine en solution neutralisée d'un effluent de lixiviation en tas Download PDF

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Publication number
WO2009026683A1
WO2009026683A1 PCT/CA2008/001489 CA2008001489W WO2009026683A1 WO 2009026683 A1 WO2009026683 A1 WO 2009026683A1 CA 2008001489 W CA2008001489 W CA 2008001489W WO 2009026683 A1 WO2009026683 A1 WO 2009026683A1
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Prior art keywords
resin
process according
solution
nickel
neutralized
Prior art date
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Ceased
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PCT/CA2008/001489
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English (en)
Inventor
Flavia Dutra Mendes
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Vale Canada Ltd
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Vale Canada Ltd
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Publication of WO2009026683A1 publication Critical patent/WO2009026683A1/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
    • C22B23/04—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
    • C22B23/0407—Leaching processes
    • C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts 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
    • 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
    • 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
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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 is related to the field of the use of resin-in- neutralized-solution in the process of heap leaching effluent.
  • a major challenge faced by some plants is that the solid-liquid separation stage creates major problems for conventional circuits. Due to poor pulp settlement in a counter-current decantation (“CCD'") stage, roughly 10% of soluble nickel and cobalt are lost in rejects and in waste. In order to minimize such significant loss, a series of at least six large thickeners (over 50m diameter in each stage) are used in solid-liquid separation so as to ensure correct solid settlement and to produce clean overflow.
  • CCD' counter-current decantation
  • HPAL high pressure acid leaching process
  • PLS pressure leach solution
  • Performance of an ore about to undergo stockpile leaching can be evaluated through column and small heap tests. These tests provide maximum metal extraction in leach consumption and their concentration in the leaching slurry and also ensure its time evolution and leaching slurry concentration.
  • scaling is difficult because it is hard to reproduce geometric proportions of industrial stockpiles and their hydrodynamic conditions. Associated with costs and the time of assays, they call for use of phenomenological models aimed at circuit analysis and the project.
  • heap leaching As the ore-extraction technique is influenced by factors such as terrain topography (avoiding mountainous areas) and local hydrology. Maintaining a certain acid concentration is necessary to render the process effective and economic. However, this concentration can be affected by regional hydrological conditions. Where the climate is arid and evaporation rates high much additional water may be required to maintain the necessary water volume in the leaching circuit. Under humid weather conditions, on the other hand, infiltrated rainfall water can add water to the circuit decreasing solution concentration and jeopardizing the whole industrial process.
  • Material to be processed can come from various sources, such as newly mined ore, previously piled ore, waste residues from conventional processing, etc. Most applications involving heap leaching use newly mined ore which is more economically feasible for processing large volumes of low-metal-grade ores.
  • the paramount objective in ore preparation is to produce fragments sufficiently small to allow solution-metal contact while ensuring adequate permeability for flow through the entire heap.
  • ore pre-treatment such as direct leaching of run-of-mine ore extracted from mine in blocks up to 120 cm diameter
  • crushing and/or agglomeration may be required.
  • the permeability coefficient in ores with high percentage of fines can be very low, resulting in long time intervals for treatment and in low amounts of metal produced.
  • agglomeration with added ligants seeks to form a dense and porous material, stable when handled, which is stacked and percolates in the leaching solution.
  • the leaching solution based on sulfuric acid in nickel mining, is hauled from the barren pond to the heap through a piping system. ⁇ set of pumps is also necessary to supply sufficient pressure to the sprinklers.
  • a basic operational requirement is that the solution be uniformly distributed on the heap top and that typical discharges ensure non- saturated flow along the heap top.
  • the chemical reaction in which metals are dissolved demand the presence of oxygen. Therefore, non-saturated flow is essential for the leaching process.
  • a layer of permeable material is generally placed directly on the waterproof coating prior to heap construction. The purpose of this layer is to make possible solution drainage and to protect the coating during stockpile formation.
  • the pregnant solution is collected from the heap through a drainage system comprising perforated pipes placed inside the permeable layer on the heap pad. These pipes help decrease the pressure load on the heap pad and are connected to a collect system, which deposits the fluid in a pregnant solution pond.
  • the stockpile must be designed as permeable as possible, with homogeneous-flow characteristics, in order to allow swift flow through the ore and its collection at the pad drainage system. It should also allow solution contact with as much ore as possible and oxygen maximization in the stockpile's empty spaces.
  • One or more layers are used in heap construction. Total heap height depends on its foundation, on its pad resistance, on its coating, on terrain topography, on ore mechanical properties, and on the type of equipment used in heap construction. Alternatives to heap construction include hauling material in conveyor belts, unloading it by truck and spreading it out by motor scraper, etc. Equipment traffic can fragment and compact ore, thus creating low surface permeability. ⁇ t the end of heap construction, this zone must be scrapped (scarified) and, whenever possible, equipment traffic must be minimized.
  • the pregnant solution contains dissolved ores; therefore, is economically imperative that no leaking whatsoever occurs through the pond.
  • a waterproof coating is used to contain the pregnant solution and to avoid possible environmental impacts caused by its seepage (liberation).
  • the barren solution contains a leaching solution.
  • the barren solution pond must likewise be contained via the waterproof coating.
  • concentration is corrected in the pond. It is common to construct both ponds adjacent to each other, confining large solution volumes in one specific area, thus minimizing construction and operation costs.
  • Every acid leaching effluent solution of nickel ores has several dissolved metals regarded as impurities, in addition to nickel and cobalt. As with every resin selective to nickel, iron, copper and aluminum, a previous stage is necessary for treatment of the solution, eliminating such impurities.
  • MSP mixed sulfide products
  • MHP mixed hydroxide products
  • Ionic exchange resin is regarded as an incipient technique, with no large- scale use, when compared to other options for solution treatment in nickel processing systems. Studies are being intensified and several approaches and results are so far promising. Recently, there has been considerable incentive to developing a nickel-centered technique, able to compete with conventional technologies (such as extraction by solvents and precipitation) given its operational simplicity, fewer equipment items and less cost involved. Its main upsides are an efficient recovery and removal of minor concentrations of some metallic ions with respect to: an excess of other metals, high metallic loading (charging), high mechanical resistance which reduces losses due to friction, swift elution and low losses due to contamination by organic matter.
  • Plants that make industrial use of acid leaching for lateritic ores include a multi-stage settling circuit in countercurrent flow for solid-liquid separation. This involves high capital and operating costs, occupies large areas and demands a significant amount of washing water. Taking advantage of ionic exchange technology, one alternative to recover nickel and cobalt from leaching pulp, without using thickeners, is to use a RIP system.
  • RIP operation has three distinct stages. Nickel and cobalt are selectively recovered in the adsorption stage. This stage can be by air agitation or by mechanical stirring in vats.
  • the resins suggested for this type of use are those with the iminodiacetic acid or picolylamine functional group. Resin-pulp contact is in countercurrent flow, with intermediate inter-vat screening sieves, for phase separation.
  • the loaded (charged) resin in the first vat is withdrawn from the circuit, washed for solid aggregate removal, and transferred to the elution circuit. Elution must be carried out with chloride acid (50-150 g/L concentration) obtained in the regeneration process during pyrohydrolysis.
  • the eluted resin then contacts a reagent—such as soda or limestone— in order to be regenerated and reverted to a calcium or sodium form.
  • Ionic exchange technology is being intensively developed with various promising approaches and results.
  • the ionic exchange technique with polymeric resins should offer advantages such as: (1) no reagent loss by dragging, as occurs in extraction by solvent: (2) efficient recovery and removal of minor concentrations o[ some metallic ions in relation to an excess of other metals; (3) high selectivity for metals of interest; (4) high separation capacity; (5) flexible process regimen; (6) simple process configuration; (7) high metal of interest concentration vis-a-vis other impurities; and (8) high automation level.
  • These features translate into lower capital and operating costs and less environmental impact (reduced water consumption and opportunities to recycle used water).
  • the ionic exchange technique with resins can be used in the effluent as pulp or solution, in order to recover nickel and cobalt.
  • Use of the ionic exchange technique with polymeric resins to selectively adsorb nickel can occur in two ways:
  • RIC Resin-in-Column
  • Resin-in-Pulp In this type of operation, ore pulp directly contacts the resin, through a stirring system, causing metal adsorption with no need of previous solid-liquid separation in the pulp, thus avoiding product loss. Following contact, resin and pulp are separated from each other via screening.
  • Cobalt From Oxidic Ore Leach Slurry to W.
  • Duyvesteyn, et al. refers to a process for the recovery of nickel and cobalt from nickcliferous oxide ore leach slurry by ion exchange. It also teaches that nickel and/or cobalt are recovered by known processes. Thus, the disclosed process teaches the recovery of nickel and cobalt avoiding the use of solid/liquid separation, but without describing specifically the ways the leaching can be accomplished.
  • Duyvesteyn, et al. describes a process for selectively recovering nickel by ion exchange absorption from a Ni/Co sulfuric acid feed solution obtained from limonite ore, which is pressure leached with sulfuric acid and then neutralized and solid/liquid separated, containing nickel in the range of about 0.5 to 40 gpl and cobalt in the range of about 0.01 to 2 gpl as sulfates.
  • the document describes that the absorbed nickel is stripped from the said resin with sulfuric acid to form a nickel sulfate solution characterized by a nickel to cobalt ratio of at least about 50: 1 suitable for the recovery of substantially pure nickel by electrolysis.
  • the document refers to the recovery of nickel merely by electrolysis, which is a well-known method for this specific technology and it also uses the solid/liquid separation.
  • US 4756887 "Process Of Heap Leaching" to S. Lesty, et al. describes a heap leaching process and comprises the following steps: (a) preparing the ground to receive the heap; (b) forming the heap; (c) sinking injection wells into the heap; (d) injecting the leaching solution by means of injection wells; and (e) recovering the leaching solution at the base of the heap, or by pumping from wells neighboring those used for injection.
  • This patent is merely focused on the functional characteristics of a heap leaching method. Heap leaching is broadly known. It does not mention the use of such a method for the recovery of nickel and cobalt.
  • Duyvesteyn, et al. describes a method of heap leaching ore to recover nickel by forming at least one heap from a mixture of the ore and concentrated sulfuric acid; applying a leaching solution to the top of the heap at a first predetermined average flux rate wherein a leach liquor is formed at a bottom of the heap; and directing the leach liquor into a product liquor sump for direct delivery to a processing plant for substantially extracting nickel values.
  • This document refers to the heap leaching methodology in a general sense without mentioning any kind of use of resin-in-pulp or ion exchange technology.
  • Leaching to M. Rodriguez, et al. discloses a process for the recovery of base metals from an oxide ore, comprising the steps of: forming at least one heap of the oxide ore containing the base metals to be recovered; irrigating at least one heap of oxide ore with a leach solution comprising sulphuric acid; collecting resulting pregnant leach solution from the irrigated heap; and treating the pregnant leach solution with a reducing gas stream to create a treated pregnant leach solution for recovery of required base metals.
  • the process disclosed by the document is applicable to the conversion of ferric ions to ferrous ions, with regeneration of sulphuric acid in the process.
  • the present invention refers to a hydro-metallurgical process using resin- in-neutralized-solution in heap leaching effluent.
  • the process is applicable to lateritic ore, nickel oxidate, cobalt oxidate or a mixture containing value metals of interest—nickel, cobalt and other secondary metals— wherein ore is leached by adding an acid or a base with possible pH adjustment, aided by acid or base with neutralization of heap leaching effluent, by adding lime, limestone, soda or ammonia in the temperature of 70° to 95°C range, at pll in the pII4 to pH5 range; wherein soluble impurity species can be reduced or cementing/complexation techniques, comprising a neutralized leaching effluent, as a slurry, made up of solid particles (precipitated compounds) and solution, but ore and ore residue-free, which is fed into the resin-in-neutralized-solution ("RINS " ') circuit, with no need for solid-liquid separation; wherein the resin-in-neutralized-solution circuit comprises vats stirred in countercurrent flow and wherein the loaded resin is
  • RINS is used in recovering nickel from acid leaching, the following benefits are to be expected: a) Acid leaching, followed by neutralization, can produce a hard-to-settle slurry or solids which, when separated, arc difficult to wash. The RINS process can get around these operating difficulties by eliminating the solid-liquid separation stage. b) Neutralizing solution acidity is conveniently carried out in the same adsorption stage, during contact. Inexpensive reagents, such as lime or limestone, can be used, and gypsum formed during neutralization would become part of the pulp. c) Use of the resin, which is also iron selective, requires neutralization prior to nickel recovery. If lime or limestone is added, ferric hydroxide precipitates easily and becomes part of the neutralized solution [0040] In any resin operation, a previous stage is needed to neutralize acidity, elevate pH, and eliminate impurities through precipitation (Figure T).
  • a high purity product known as eluate is obtained in ion exchange. This is conducive not only to simplification of the next stages but also to simpler unit operations. The process flowchart is thus simplified; eliminating possible operational problems that are common to impure solutions. Once separated, nickel and cobalt are individually recovered. Nickel and cobalt can then be recovered as diverse products.
  • Figure 1 is to a schematic prior art representation of ore processing using heap leaching.
  • Figure 2 is a schematic representation of the invention.
  • the present invention refers to a hydro-metallurgical process using resin-in- neutralized-solution of a heap leaching effluent. It provides the following advantages:
  • Ore leaching is preferably acid, with an option to use sulfuric or hydrochloric acid.
  • the pregnant leaching solution (“'PLS”) coming from the pile should have free acidity preferably between 02 and 200 grams per litre.
  • One such technology is heap leaching. Downsides are less nickel recovery efficiency and higher operating cost (due to greater acid consumption). However, lower investment cost makes it a highly attractive technical alternative.
  • Leaching yields an impurity-bearing solution and highly concentrated with metals of interest. However, neutralization is necessary to adjust this solution's pH, complying with RINS operational standards. That demands neutralizing excessive leaching effluent acid, in addition to precipitating iron and some impurities. Temperature in this stage should be in the 70°C-95°C range.
  • Lime or limestone can be added and air injected in order to oxidize iron.
  • pH is in the 4 to 5 range. This can be done in a single step or in a two-step operation. In this case, the first stage would increase the pH to a 1.5 to 4.5 range, and the second stage to a 3.0 to 5 range.
  • RINS operation occurs in stirred vessels. Stirring can be mechanical or by air agitation.
  • a pachuca vessel is preferred. It's bottom is cone-shaped and from a center draft tube air is injected into the tank containing a solid-liquid mixture.
  • the pachuca air- stirring system has the advantages of reduced physical degradation of the resin and better RINS particle dispersion when compared to mechanical stirring.
  • the slurry cascades down by gravity, from vessel to vessel, displaying approximately 25% to 45% of solids, preferably 35%.
  • Resin-in-Neutralized-Solution operation must take place at an adequate temperature, coherent with the resin's thermal stability limit (about 80 0 C). Generally, the adsorption rate will increase as the temperature rises, due to better slurry viscosity.
  • Slurry residence time can be up to twelve hours (30 to 60 minutes per stage) and it is influenced by the size of the feeding material particles. Resin volume in each stage is roughly 10% to 30% of slurry volume in the vessel.
  • the resin advances in countercurrent flow, from one stage to another, through pumping or pneumatically hauling both slurry and resin to the next adsorption stage. I he loaded (charged) resin leaves the first adsorption stage and is pumped to a static or vibrating horizontal screen, to be washed and separated from the pulp.
  • the resin is composed of the bis-picolylamine or iminodiacetic acid functional group.
  • the resin Once the resin has been loaded (charged) with metals, it is physically separated from the slurry. Screening separates larger-diameter resins from the slurry's fine particulates. Exiting the first adsorption stage, the resin is sieved for separation and washing. Washed, humid and drained, the resin next goes to the elution circuit, for nickel and cobalt desorption. Elution can be initially with acidified water (preferably pH 2), to remove iron adsorbed in the resin. Next is the use of ammonium salt (ammonia sulfate or hydroxide) for copper removal. Finally, acid is used (0.50 to 4M, preferably 1 M) for nickel and cobalt elution.
  • acidified water preferably pH 2
  • ammonium salt ammonia sulfate or hydroxide
  • the resin After elution and, if necessary, the resin can be regenerated and ions (such as Na +, Ca 2+) can be included as mobile ions.
  • ions such as Na +, Ca 2+
  • the eluate obtained in this stage may contain nickel concentrations above 45g/L with low impurity concentrations.
  • This high-purity product must be sent to a unit operation, for the sole purpose of Ni and Co separation (through extraction by solvents or continuous ion exchange). Following their separation, nickel and cobalt may be separately recovered in various ways.
  • the ore and ore residue-free slurry obtained in neutralization is fed to the RINS unit.
  • the leaching effluent is ore and ore residue-free and preferably contains solid compounds of precipitated aluminum and iron.
  • the present invention provides the use of a RINS (resin-in-neutralized- solution) system as an alternative to recover nickel and cobalt from heap leaching effluents, with no solid-liquid separators, such as thickeners.
  • This type of ionic exchange process directly applied to the slurry eliminates costly solid-liquid separation and offers greater efficiency in recovering nickel contained in the leaching effluent, in view of the desorption-leaching phenomenon, which recovers nickel in both the solid and liquid phases.

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Abstract

L'invention concerne un procédé hydrométallurgique utilisant de la résine en solution neutralisée d'un effluent de lixiviation en tas. Plus spécifiquement, le procédé est applicable au minerai latéritique, à l'oxyde de nickel, à l'oxyde de cobalt ou à un mélange contenant des métaux d'intérêt tels le nickel, le cobalt et autres métaux secondaires. Dans ledit procédé, le minerai est lixivié par ajout d'un acide ou d'une base, avec une éventuelle régulation du pH, à l'aide d'un acide ou d'une base avec neutralisation d'un effluent de lixiviation en tas, par ajout de chaux, de castine, de sodium ou d'ammoniac, à une température allant de 70° à 95°C, à un pH allant de 4pH à 5pH. Dans ledit procédé, les espèces d'impuretés solubles peuvent être réduites par des techniques de cémentation/complexation, comprenant un effluent de lixiviation neutralisé, tel qu'une boue faite de particules solides (composés précipités) et d'une solution, mais exempte de minerai. Ladite boue est acheminée dans le circuit de RINS (résine en solution neutralisée) sans qu'une séparation des solides et des liquides soit nécessaire. Ledit circuit de résine en solution neutralisée comprend de multiples bassins séquentiels mélangés à contre-courant. La résine chargée est séparée de la boue par tamisage.
PCT/CA2008/001489 2007-08-29 2008-08-22 Procédé hydrométallurgique utilisant de la résine en solution neutralisée d'un effluent de lixiviation en tas Ceased WO2009026683A1 (fr)

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FR2925349A1 (fr) * 2007-12-20 2009-06-26 Applexion Procede de separation sequence multicolonnes d'un derive metallique ionique
WO2010126593A1 (fr) * 2009-04-30 2010-11-04 World Resources Company Procédé de récupération de métaux et de composés métalliques à partir de minerai extrait et d'autres matières premières sources contenant des métaux
CN102443700B (zh) * 2011-12-12 2013-10-30 四川金岳新型材料有限公司 从镍红土浸出液回收镍的方法和装置
WO2013165735A1 (fr) 2012-05-01 2013-11-07 Dow Global Technologies Llc Récupération de nickel de cobalt en utilisant l'échange d'ions continu
CN109652646B (zh) * 2018-12-20 2020-09-01 昆明理工大学 一种综合回收高镁硅红土镍矿中镍、钴、镁、硅的方法
CN110453070A (zh) * 2019-03-11 2019-11-15 西安蓝晓科技新材料股份有限公司 一种直接从红土镍矿浸提液中提取回收镍的方法
CN111100985B (zh) * 2019-12-30 2021-05-18 荆门市格林美新材料有限公司 一种含钠铵废液应用于红土镍矿的综合处理方法
EP4174195A1 (fr) * 2021-10-29 2023-05-03 Eramet Récupération de nickel et/ou de cobalt contenus dans des résidus solides de fer et/ou d'aluminium
US12353196B2 (en) * 2022-06-27 2025-07-08 Freeport Minerals Corporation System and method for determining changes to a heat profile of a stockpile
CN115505733B (zh) * 2022-09-05 2024-11-19 中铁资源集团有限公司 一种适用于雨季的矿石堆浸堆体结构
JP7758078B2 (ja) * 2024-03-08 2025-10-22 三菱マテリアル株式会社 有価金属の回収方法

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