EP4587601A1 - Procédé de lixiviation oxydative de nitrate en tas - Google Patents

Procédé de lixiviation oxydative de nitrate en tas

Info

Publication number
EP4587601A1
EP4587601A1 EP23783026.0A EP23783026A EP4587601A1 EP 4587601 A1 EP4587601 A1 EP 4587601A1 EP 23783026 A EP23783026 A EP 23783026A EP 4587601 A1 EP4587601 A1 EP 4587601A1
Authority
EP
European Patent Office
Prior art keywords
heap
nitrate
acid
ore
solution
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.)
Pending
Application number
EP23783026.0A
Other languages
German (de)
English (en)
Inventor
Clement Chilowa CHIBWANA
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.)
BHP Chile Inc
Original Assignee
BHP Chile Inc
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
Application filed by BHP Chile Inc filed Critical BHP Chile Inc
Publication of EP4587601A1 publication Critical patent/EP4587601A1/fr
Pending legal-status Critical Current

Links

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
    • 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
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0065—Leaching or slurrying
    • C22B15/0067—Leaching or slurrying with acids or salts thereof
    • C22B15/0073—Leaching or slurrying with acids or salts thereof containing nitrogen
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0063—Hydrometallurgy
    • C22B15/0084—Treating solutions
    • C22B15/0089—Treating solutions by chemical methods
    • 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

  • This invention relates generally to a process of leaching base metals from a heap of ore.
  • the invention is particularly suitable for the treatment of primary copper ores containing chalcopyrite and secondary sulfide minerals e.g. enargite, bornite, chalcocite and covellite in an oxidative environment.
  • Ricardo Andres Soto Mellado (Ibanez & Mellado, 2018) describes a process of copper sulfide mineral oxidation and leaching in acid chloride and sulfuric acid chloride/nitrate solutions.
  • the publication discloses the treatment of a low-grade copper sulfide ore in an acid chloride-nitrate medium.
  • the concept of pre-treating ore in an agglomeration step followed by a curing step is disclosed.
  • Mechanisms for chalcopyrite leaching in acid ferric sulfate and sulfuric acid and chloride solutions, and the action of adding nitrate (as sodium nitrate or ferric nitrate) to increase the solution oxidation potential are disclosed.
  • WO 2012/162851, WO 2017/063099, US 9683277, and CL 43295 each disclose a method of heap leaching in which either ferric nitrate, ammonium nitrate or sodium nitrate act as an oxidising agent, in a sulfuric acid or sulfuric acid/chloride aqueous solution.
  • US 4,647,307 discloses a process for the hydrometallurgical recovery of precious metal from an ore or concentrate containing at least some arsenopyrite or pyrite.
  • the process comprises forming in a common volume space a gas phase and a liquid slurry comprising the ore or concentrate as the solid phase and acid and water as the liquid phase of the slurry, effecting in the slurry an oxidation-reduction reaction between the arsenopyrite or pyrite and an oxidized nitrogen species in which the nitrogen has a valence of at least plus 3 thereby solubilizing in the liquid phase the arsenic, iron and sulphur in the arsenopyrite, or the iron and sulphur in the pyrite, and producing in the liquid phase nitric oxide in which the nitrogen has a valence of plus 2; releasing at least part of the nitric oxide from the liquid phase into the gas phase, oxidizing the nitric oxide in the gas phase,
  • WO 2021/186376 A1 describes an oxidative bioleaching process for leaching a base metal from an ore that includes an ore agglomeration step, an ore stacking step wherein agglomerated ore is stacked to form a heap, a curing step, a rinse step, an inoculation step and a leach step, and wherein, during the ore agglomeration step, the ore is contacted with an acid solution containing nitrate and nitrite thereby to accelerate the leaching rate in the leach step.
  • a further aim of the invention is to provide a bio-heap leaching process using a nitrogen compound as an oxidant wherein the inoculation and bioleaching steps are not adversely affected due to inhibiting effect of nitrate compounds on microbial growth.
  • the method is limited by the need to include an ore agglomeration and curing step.
  • bioleaching processes While effective to a limited extent, bioleaching processes often have slow reaction rates, and the initial heat generation is slow. Consequently, bioleaching methods are not effective for the treatment of ROM ore.
  • nitrate in an acid medium provides an option for leaching of sulfide minerals at an acceptable kinetic rate.
  • these applications involve high temperatures and high levels of pressure.
  • the prior art methods show that agglomeration and curing steps are necessary to create reactive conditions in a heap leach environment thereby achieving relatively high acid and nitrate conditions in an almost closed system resulting in active oxidation conditions.
  • NOx (NO and NO 2 ) gases leave the system in the leach cycle and ore agglomeration steps and result in high nitrate and acid consumption rates in the heap leach stage.
  • NOx gases leave the system in the leach cycle and ore agglomeration steps and result in high nitrate and acid consumption rates in the heap leach stage.
  • direct nitrate leaching with capture of NOx gases has only been achieved commercially in a closed system under conditions of elevated pressures, or by use of gas capture and scrubbing steps in the ore agglomeration stage prior to heap construction (as part of the ore agglomerator design).
  • NOx gases principally as NO (low solubility in aqueous solution)
  • leaving the surface of the heap during the leach cycle are difficult to capture and overall nitrate consumption remains high, in the range 10 -20 kg/T or above 20 kg/T.
  • Efficient recycle of NO and NO 2 gas has not been demonstrated in a heap leach process operating at ambient pressures.
  • the invention aims, at least partly, to address the aforementioned issues.
  • Heap as used in herein includes treating ore in an irrigated heap, in a column, in a large vat or in a large ore dump.
  • the invention provides a method of extracting copper from a sulfide mineral ore selected from ROM ore, crushed ore or crushed ore subject to acid agglomeration, including the steps of: a) stacking the ore to form a heap; b) in a leach step, irrigating the heap with a first irrigation solution containing an acid nitrate (NO 3 -) solution, and nitrite (NO 2 -) at a concentration of between 50 - 500 ppm thereby to cause the oxidation of sulfide minerals within the heap; c) adding air or oxygen, or oxygen enriched air into the heap; d) oxidising NO gas released during the oxidation of the sulfide minerals within the heap by oxygen to form nitrogen dioxide ( NO 2 ); and e) hydrolysing the nitrogen dioxide (NO 2 ) to form nitric acid and/or nitrous acid in the solution within the heap, to continue the leaching step.
  • a first irrigation solution containing an acid n
  • step (e) Recycling the nitric acid and/or nitrous acid produced within the heap in step (e) for use in the first irrigation solution reduces the loss of NO gas from the heap to between 5%- 30%.
  • the method may include the step of capturing NOx gas expelled from the heap surface and recycling the evolved gas to the first irrigation solution in a gas scrubbing process to further reduce loss of nitrate from the leach process.
  • the NOx gas expelled from the heap may be contained, for subsequent capture, by covering the heap with a sealed cover, for example an insulated thermofilm or any impermeable cover.
  • the nitric oxide gas generated may be drawn away from the heap using a suitable suction pump system.
  • the NOx leaving the heap may be readily oxidised by oxygen contained in the air being fed from a bottom of the heap and contained with the expelled NOx gases.
  • Additional air or oxygen, or oxygen enriched air may be injected during a scrubbing process to ensure the total oxidation of the NO to NO 2 .
  • the generated NO 2 may react with a scrubber solution to produce a scrubber effluent containing nitrous acid and nitric acid.
  • the scrubber solution can either be wash water, raffinate solution or any aqueous media in which NO 2 can easily dissolve.
  • Hydrogen peroxide or any other oxidant can also be added to the scrubber solution to help oxidise the unreacted NO absorbed into solution from the gas phase.
  • the nitrate concentration in the first irrigation solution may be controlled according to the rate of mineral oxidation and heap temperature such that it is within the range 10g/L to 80 g/L nitrate.
  • Air or oxygen, or oxygen enriched air may be passed into the heap at a base of the heap or at multiple points from the base of the heap to the top of the heap and/or at one or more levels above the base of the heap.
  • the aeration rate may be controlled to a specific rate within the range 0.01 - 0.05 Nm 3 /h.t to maximise heap temperatures (heat generation rate) and minimise NOx gas loss from the heap.
  • Irrigation rates and aeration rates may be controlled to maximise heat generation within the heap, to minimise NO loss and to maximise the recycle of nitrate to the first irrigation solution.
  • Example, but not limiting irrigation rates may be in the range of 2.5 - 6L/h.m 2 and the specific mass flowrate of air (Ga in kg/h.m 2 ) to irrigation rate (Gi in kg/h.m 2 ) may be in the range 0.10 - 0.3.
  • the method may include a rinse step, whereby the heap is rinsed with a low nitrate process water to recover excess nitrate in the heap.
  • the method may include the additional steps of: f) rinsing the heap with a low nitrate raffinate or process water to remove excess nitrate; g) in a separate leach step, irrigating the heap with a second irrigation solution containing an acid nitrate solution.
  • the concentration of nitrate in the second irrigation solution may be low and in the range 0.5g/L to 15 g/L nitrate.
  • the sulfide mineral ore may be selected from chalcopyrite, pyrite, covellite, chalcocite, bornite, enargite, copper oxide minerals or nickel sulfide minerals. This is not limiting.
  • the acid concentration in the first irrigation solution and the second irrigation solution may be within the range 5g/L to 40g/L and up to 50 g/L sulfuric acid.
  • the method may be carried out at atmospheric pressure and ambient temperatures in the environment outside of the heap.
  • the nitrate and nitrite salts may be added in a solution or may be added as a solid salt to the ore during heap construction.
  • the source of nitrate may be selected from nitric acid (HNOs), NaNOj, KNO3 or any other soluble inorganic nitrate salt.
  • the source of nitrite may be selected from nitrous acid (HNO 2 ), NaNCte, KNO 2 or any other soluble inorganic nitrite salt, or as a known impurity in the nitrate salt.
  • the addition of sulfuric acid may be of the order of 5kg/T - 20kg/T.
  • the acid addition is determined by:
  • the first and second irrigation solutions in contact with the ore in the leach stage are acidic with a pH lower than pH3 and preferably lower than pH2.
  • Each of the first and second irrigation solutions may contain iron, copper and other dissolved cations and anions as leach product species.
  • Recycled process solution containing nitrate and nitrite may be used in ore irrigation during the leach cycles.
  • Figure 11 is a comparison plot of solution potential over time with and without nitric acid regeneration
  • each of the methods 10A and 10B (see Figures 1a and 1b wherein corresponding features of method 10B have been included in parenthesis), ore in the form of run-of-mine (ROM) ore 12 (12A) is stacked 24A to form a heap 24.
  • the ore 12 (12A) may be crushed in a crusher 14 (14A) to ensure that the crushed ore 16 (16A) is suitably sized, according to requirement.
  • the ore has a crush size in the range of Pso (80% passing size) of 4mm to a Pso of 102mm.
  • the copper stripped PLS1 28 (28A) constitutes a high nitrate and nitrite raffinate solution 28B and is mixed with a saturated scrubber raffinate 36 (36A) to produce a high nitrate, and nitrite, raffinate 18A (18D) which is then collected in the high nitrate, and nitrite, raffinate pond 38.
  • Nitrate 62 (62A) is added to the raffinate 18A (18D), if necessary and a resulting solution 18B (18E) drains from the pond and is recycled to the leach step 24B as the high nitrate raffinate solution 18 (18C).
  • Nitrate, acid, and water may be added to raffinate 1 or raffinate 2 to maintain required concentrations.
  • forced aeration 40 (40A) is applied to the bottom of the heap 24 and/or to one or more levels above the bottom of the heap at the rate of 0.01 - 0.05Nm 3 /hr.t.
  • the process 10A may include an optional second leach step.
  • a leach step 24C is carried out following the leach step 24B.
  • forced aeration 40 is also applied from the bottom of the heap 24 and/or to one or more levels above the bottom of the heap at the rate of 0.01 - 0.05Nm 3 /hr.t.
  • a second irrigation solution in the form of a low nitrate raffinate solution 20 is applied to the heap 24 and is collected in the drainage at the bottom of the heap 24 as a low nitrate pregnant leach solution 2 (PLS 2) 42 which contains a high copper concentration and other cationic and anionic species from the leached ore.
  • PLS 2 low nitrate pregnant leach solution 2
  • the PLS 2 42 is collected in a PLS 2 pond 44 which feeds the solvent extraction (SX) plant 30 where copper is concentrated to produce the advance electrolyte solution 32 which is treated to recover metallic copper by means of electro-winning in the electro-winning tank-house 34.
  • the resulting PLS 242, stripped of copper and enriched with acid, constitutes a low nitrate raffinate solution 20A which is collected in a low nitrate and nitrite raffinate pond 46.
  • Hydrogen peroxide (not shown) or any other oxidant can also be added to the scrubber solution to help oxidise the unreacted NO absorbed into the scrubber raffinate solution from the gas phase.
  • the concentration of NOx in the bulk gas stream is expected to be reduced from 50ppm to fess than 5ppm before its discharge to the atmosphere.
  • the scrubber raffinate solution 36 (36A) is combined with high nitrate raffinate 18A (18D) from the leach step 24B to produce the solution 18B (18E) which is then recycled to the leach step 24B as the high nitrate raffinate solution 18 (18C).
  • nitrate 62 (62A) may be added as make-up nitrate in order to compensate for nitrate loss in the heap leach circuit.
  • Sulfuric acid 64 (64A) may also be added in order to replace the acid that is consumed by the ore in the leach step 24B.
  • nitrate consumption for leaching of pyrite and typical copper sulfide minerals from a primary copper ore may be represented by the following equations, where y is the fraction of nitric oxide gas lost from the ore bed of the heap: FeS 2 + 5y N03’ + 15(l-y)/40 2 + (1-5y)/2 H 2 0 -> Fe 3+ + 2 SO 4 2- + 5y NO(g) + (l-5y) H +
  • a maximum nitrate consumption for economic recovery of metals from an ore is 10 kg/T ore treated and preferably 5 kg/T or less.
  • Dissolution of pyrite by oxidation with nitrate ions is very slow in the absence of nitrite ions.
  • addition of small amounts of nitrite (as low as 50ppm) can initiate oxidation of pyrite with the mixed potential increasing by some 50-70 mV while the solution potential increases to above 0.9 V.
  • Figure 7 shows the measured and calculated acid concentrations and the calculated nitrate concentration during the leach test.
  • the solid lines and dashed lines are the calculated concentrations with and without nitric acid regeneration, respectively.
  • Model parameters were derived from the test data and model outputs were tested and verified against results of the 10m simulation column tests. The model results were then used to describe the observed results. Examples of the column experiments completed as 10 separate case studies are summarized in Table 6 below and results of the case studies showing effects of operating conditions and reagent concentrations are shown in Figures 12 to 21.
  • the acid and nitrate concentrations refer to the concentrations in the irrigation solution of the 10m simulation column tests.
  • Gangue refers to the acid consuming non-sulfide minerals in the ore and are predominantly silicate minerals, for example chlorite and biotite.
  • Low refers to low GAC (gangue acid consumption) (relatively low content of chlorite and biotite) and “high” refers to high GAC (typically relatively high chlorite and biotite content.
  • Air is the aeration rate to the column, expressed as Nm 3 per hour per metric t ore loaded in the column (Nm 3 defined here as the air flow at OoC and 101.325kPa).
  • Case 4 and Case 8 show the effect of a reduced nitrate concentration in the irrigation solution for a low and high acid consuming gangue respectively.
  • the method of the invention provides an effective solution for the regeneration of nitrate, reducing the operating costs of the process. Additionally, the method ensures high oxidation potentials to allow efficient leaching of the sulfide mineral ores without the need for agglomerating and curing steps.
  • Sample M1 was irrigated with raffinate solution containing only high nitrate at 50g/L nitrate throughout the leach cycle while in sample M2 the raffinate was changed from high nitrate to low nitrate once the desired leach temperature was achieved. After 200 days of irrigation, the results show that there is no significant difference in final extractions for columns (83% vs 81 %) operated with or without change in raffinate solutions - Figure 22.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (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 un procédé d'extraction de cuivre d'un minerai de sulfure, qui comprend les étapes consistant à : empiler le minerai pour former un tas; dans une étape de lixiviation, irriguer le tas à l'aide d'une première solution d'irrigation contenant une solution de nitrate acide et du nitrite pour provoquer ainsi l'oxydation de minéraux sulfurés à l'intérieur du tas; oxyder le gaz d'oxyde nitrique libéré pendant l'oxydation des minéraux sulfurés à l'intérieur du tas par l'oxygène pour former du dioxyde d'azote; et hydrolyser le dioxyde d'azote pour former de l'acide nitrique et/ou de l'acide nitreux dans la première solution d'irrigation à l'intérieur du tas, pour poursuivre l'étape de lixiviation et pour réduire la perte d'oxyde nitrique du tas.
EP23783026.0A 2022-09-16 2023-09-13 Procédé de lixiviation oxydative de nitrate en tas Pending EP4587601A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ZA202210270 2022-09-16
PCT/IB2023/059066 WO2024057216A1 (fr) 2022-09-16 2023-09-13 Procédé de lixiviation oxydative de nitrate en tas

Publications (1)

Publication Number Publication Date
EP4587601A1 true EP4587601A1 (fr) 2025-07-23

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Application Number Title Priority Date Filing Date
EP23783026.0A Pending EP4587601A1 (fr) 2022-09-16 2023-09-13 Procédé de lixiviation oxydative de nitrate en tas

Country Status (10)

Country Link
EP (1) EP4587601A1 (fr)
CN (1) CN119948181A (fr)
AR (1) AR130496A1 (fr)
AU (1) AU2023343440A1 (fr)
CA (1) CA3266651A1 (fr)
CL (1) CL2025000472A1 (fr)
MX (1) MX2025002050A (fr)
PE (1) PE20251495A1 (fr)
WO (1) WO2024057216A1 (fr)
ZA (1) ZA202503034B (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110352256B (zh) 2016-10-19 2023-01-10 捷迪资源有限责任公司 用具有硫代羰基官能团的试剂浸出金属硫化物的工艺
WO2022056622A1 (fr) 2020-09-18 2022-03-24 The University Of British Columbia Extraction de métaux de base à l'aide d'un agent mouillant et d'un réactif à groupe fonctionnel thiocarbonyle
WO2024258938A2 (fr) * 2023-06-14 2024-12-19 Ceibo Inc. Procédé catalytique de transformation progressive de minerai dans la lixiviation du cuivre

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Publication number Priority date Publication date Assignee Title
US3888748A (en) 1972-06-28 1975-06-10 Du Pont Recovery of metal values from ore concentrates
US4647307A (en) 1983-01-18 1987-03-03 Rein Raudsepp Process for recovering gold and silver from refractory ores
US4834793A (en) * 1985-03-19 1989-05-30 Hydrochem Developments Ltd. Oxidation process for releasing metal values in which nitric acid is regenerated in situ
US5096486A (en) 1990-12-13 1992-03-17 Sunshine Precious Metals Incorporated Treatment of metal bearing mineral material
DE602004006510D1 (de) 2003-12-23 2007-06-28 Bhp Billiton Sa Ltd Verfahren und vorrichtung zur simulation eines biologischen haufenlaugungverfahrens
EP2716775A4 (fr) 2011-05-27 2015-03-11 Lixivia Ltda Obtention in situ de réactif de nitrate ferrique à partir d'une solution de raffinage de cuivre dans un traitement hydrométallurgique de cuivre
US9683277B2 (en) 2013-09-24 2017-06-20 Likivia Process Metalúrgicos SPA Process for preparing a ferric nitrate reagent from copper raffinate solution and use of such reagent in the leaching and/or curing of copper substances
JP2015078414A (ja) * 2013-10-17 2015-04-23 Jx日鉱日石金属株式会社 硫化銅鉱から銅を浸出する方法
CL2015003082A1 (es) 2015-10-16 2016-06-10 Lixivia Procesos Metalúrgicos S P A Proceso hidrometalúrgico para lixiviación de minerales de cobre y productos que los contienen, y mezcla reactiva utilizada en el mismo
CN115485401A (zh) * 2020-03-18 2022-12-16 Bhp智利股份有限公司 贱金属的氧化堆浸
AR121604A1 (es) 2020-03-18 2022-06-22 Bhp Chile Inc Biolixiviación oxidativa de metales básicos

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Publication number Publication date
CL2025000472A1 (es) 2025-05-30
WO2024057216A1 (fr) 2024-03-21
ZA202503034B (en) 2025-11-26
AR130496A1 (es) 2024-12-11
PE20251495A1 (es) 2025-06-02
AU2023343440A1 (en) 2025-04-03
CN119948181A (zh) 2025-05-06
CA3266651A1 (en) 2024-03-21
MX2025002050A (es) 2025-04-02

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