US20060169104A1 - Recovering nickel - Google Patents

Recovering nickel Download PDF

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Publication number
US20060169104A1
US20060169104A1 US10/524,574 US52457405A US2006169104A1 US 20060169104 A1 US20060169104 A1 US 20060169104A1 US 52457405 A US52457405 A US 52457405A US 2006169104 A1 US2006169104 A1 US 2006169104A1
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United States
Prior art keywords
process defined
precipitation
nickel
iron
seed
Prior art date
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Abandoned
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US10/524,574
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English (en)
Inventor
Anthony Chamberlain
Geoffrey Tindall
Bruce Wedderburn
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WMC Resources Ltd
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WMC Resources Ltd
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Assigned to WMC RESOURCES LTD. reassignment WMC RESOURCES LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHAMBERLAIN, ANTHONY, WEDDERBURN, BRUCE, TINDALL, GEOFFREY
Publication of US20060169104A1 publication Critical patent/US20060169104A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0453—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
    • 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
    • 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
    • C22B15/0084—Treating solutions
    • C22B15/0089—Treating solutions by chemical methods
    • C22B15/0093—Treating solutions by chemical methods by gases, e.g. hydrogen or hydrogen sulfide
    • 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 process for recovering valuable metals, such as nickel, from liquors obtained by processing laterite ores and concentrates of the ores that are contaminated with high levels of iron.
  • processing laterite ores and concentrates is understood herein to include processing by any one or more of heap leaching, pressure leaching, bacterial oxidation leaching, and atmospheric tank leaching.
  • the present invention relates particularly, although by no means exclusively, to a process for recovering nickel and cobalt from liquors obtained by acid leaching ores and concentrates of the ores that are contaminated with high levels of iron.
  • high levels of iron is understood to mean levels of iron whereby the mole ratio of Fe:Ni is greater than 2:1.
  • nickel can be recovered from such liquors containing nickel by contacting the liquors with H 2 S to precipitate nickel sulphides (and mixed sulphides in situations where nickel and other valuable metals such as cobalt are in the liquors).
  • iron can be removed from liquors prior to nickel (and cobalt) precipitation by using (a) high temperatures (180-220° C.) to selectively precipitate iron as hematite (b) low temperatures (90-120° C.) to precipitate iron as goethite, and low temperatures (70-150° C.) to precipitate iron as jarosite.
  • high temperature precipitation is capital intensive, requiring autoclaves and flash vessels, and low temperature precipitation results in high nickel losses as a result of nickel adsorption onto iron species.
  • the applicant has developed a process that is capable of recovering very high levels (greater than 99%) of nickel from nickel liquors with very low levels of co-precipitation of iron.
  • the reduction step (a) includes reducing ferric ions to ferrous ions using the reductant in the presence of 40-90 g/l free acid.
  • the reductant may be any suitable reductant.
  • One suitable reductant is NaHS.
  • the reductant is a gaseous reductant.
  • the gaseous reductant is H 2 S.
  • the neutralisation step (b) increases the pH of the solution to 2.
  • the neutralisation step (b) maintains iron in the ferrous state.
  • the valuable metal is nickel.
  • the valuable metals are nickel and cobalt.
  • the laterite ores are ores that contain nickel in a chlorite mineral phase.
  • the process conditions for the precipitation step (c) include operating at a partial pressure of the gaseous reductant of less than 60 psi.
  • gas partial pressure is less than 40 psi.
  • gas partial pressure is less than 30 psi.
  • the gas partial pressure be less than 25 psi.
  • the process conditions for the precipitation step (c) include operating at a liquor temperature of at least 50° C.
  • the liquor temperature is at least 60° C.
  • the seed particles for the precipitation step (c) have a particle size of P 50 less than 100 micron.
  • the particle size of the seed particles is P 50 less than 80 micron.
  • the particle size of the seed particles be P 50 less than 60 micron.
  • the seed particle concentration for the precipitation step (c) is greater than 30 g/l.
  • the seed particle concentration is greater than 40 g/l.
  • the ratio of iron and the valuable metal in the leach liquor supplied to step (a) is greater than 2:1.
  • the ratio is greater than 3:1.
  • the ratio is greater than 5:1.
  • the present invention is based on extensive experimental work carried out by the applicant to recover nickel and cobalt from laterite ores.
  • the experimental work included the following work.
  • the initial test work included test work for optimal precipitation conditions using the synthetic liquor.
  • the initial test work investigated the following precipitation parameters to determine their effect on nickel and cobalt recovery and nickel/iron separation:
  • the heap leach liquors were spiked with nickel and cobalt sulphate salts to increase the nickel and cobalt concentration in solution to ⁇ 4 and 0.2 g/l respectively to simulate recycling of liquor to the heap.
  • the kinetics of precipitation are also influenced by temperature.
  • Tests 1 to 4 from these tests are summarised in FIG. 1 .
  • the surface area of seed particles can be increased by increasing the mass of seed in the reactor or by seeding with solids with a smaller average particle size. The influence of both factors was investigated. Detailed results are summarised in FIGS. 2 and 3 .
  • a second batch of liquors was generated and treated in the following sequence of process stages, as discussed below:
  • the Fe(III) was effectively reduced to Fe(II) under the conditions employed.
  • Nickel and cobalt precipitation were minimal. Nickel precipitation ranged from 0.083 to 0.67% while cobalt precipitation was less than 0.01%.
  • the concentrations of the other elements assayed were not significantly altered by the pre-reduction stage with precipitation consistently being less than 0.5% and typically less than 0.1%.
  • Residue assays showed sulphur as the main constituent (>80%).
  • the liquors generated from the pre-reduction stage were treated with limestone to increase the solution pH to ⁇ 2 in the neutralisation stage.
  • Nickel and cobalt losses by precipitation were low—ranging from 0.2 to 0.4% and 0.05% to 0.16%, respectively.
  • the copper concentration in solution was reduced to below the copper detection limit of 0.1 mg/l.
  • Precipitation of the remaining impurities was low, generally less than 1%.
  • the iron essentially remained in the Fe(II) state enabling sulphide precipitation from the liquor to be undertaken.
  • the residues were mainly composed of gypsum (indicated by high calcium and sulphur assays).
  • Limestone consumption was very high, ranging from 13 to 24 kg/kg (Ni+Co)—due to the high free acid concentration in the solution.
  • H 2 S H 2 S Pressure 20 psi Seed charge 30 g/l Temperature 80° C. Seed P 50 45 microns.
  • composition of the liquors used in the sulphide precipitation stage are summarised in Table 5.
  • Table 5 Liquor Compositions to Sulphide Precipitation Stage
  • Liquor Assay (mg/L) Sample Ni Co Fe Cu Cr Al Mn Zn Mg GL-Ev 4250 210 27940 0.2 621 5080 497 5 4780 GL-Tr 4050 197 22510 0.2 750 4260 519 3 3810 GL-Ka 4420 197 17280 0.2 114 347 330 77 14220 GL-Ak 4130 196 28340 0.4 554 5410 470 3 4930
  • the solids contained between 4.0 and 5.0% Fe with the Ni:Fe mole ratio ranging between 9.0 and 11.2.
  • Ni:Fe mole ratio could be upgraded from a range of 0.14-0.24 in solution to 9.0-11.2 in the sulphide product representing approximately a 50 fold upgrade of the nickel values with respect to iron.
  • Aluminium and chromium showed increased precipitation as the concentration of these metals in solution increased. However the concentrations of aluminium and chromium in the product remained low.
  • aluminium concentration in the product generally increased with aluminium concentration in solution. Aluminium does not form stable sulphides in solution and the increase in aluminium concentration in the product appears to be through adsorption/entrainment with the sulphide.
  • the chromium concentration in the product also increased with chromium concentration in solution. This effect is much stronger with the increase in chromium in the product increasing more steeply with chromium in the PLS compared to aluminium and could indicate that chromium precipitated as opposed to being adsorbed/entrained.
  • Zinc concentration in solution was reduced to between 2 and 3 mg/l.
  • the sulphide products were generally low in zinc (less than 0.03%) due to the relatively low zinc concentration in solution (3-5 mg/l). Only the sulphide generated from the GL-Ka ore contained significant zinc at 0.73% due to the feed solution having a higher zinc tenor (77 mg/l).
  • Copper concentration in the products was low due to copper removal in previous unit operations with copper in the product ranging between 0.01 and 0.03%.
  • Manganese and magnesium concentrations in the products were consistently low at less than 50 ppm and less than 500 ppm, respectively, reflecting the high selectivity of sulphide precipitation against these elements.
  • Nickel and cobalt precipitation increased as liquor temperature increased from 40° C. to 95° C.
  • the Ni/Fe separation appeared to reach a maximum at 86° C.
  • Aluminium, chromium, manganese and magnesium precipitation were not affected over the temperature range investigated.
  • Liquors can be treated with H 2 S gas in a pre-reduction stage to reduce Fe(III) to Fe(II) with low nickel and cobalt losses (ranging from 0.08%-0.67% and ⁇ 0.1%, respectively). Copper was the only impurity significantly removed during pre-reduction with copper concentration in solution being reduced below 1 mg/l.
  • the neutralisation stage effectively increased the pH of the liquor from the pre-reduction stage to ⁇ 2 while maintaining iron in the Fe(II) state.
  • Nickel and cobalt losses during the neutralisation stage were 0.2%-0.4% and 0.05%-0.16%, respectively.
  • the residues were mainly gypsum. Impurity removal during neutralisation was generally less than 1%.

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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)
US10/524,574 2002-08-15 2003-08-15 Recovering nickel Abandoned US20060169104A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AU2002950815 2002-08-15
AU2002950815A AU2002950815A0 (en) 2002-08-15 2002-08-15 Recovery nickel
PCT/AU2003/001037 WO2004016816A1 (en) 2002-08-15 2003-08-15 Recovering nickel

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US20060169104A1 true US20060169104A1 (en) 2006-08-03

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Country Status (6)

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US (1) US20060169104A1 (pt)
EP (1) EP1546418A4 (pt)
AU (1) AU2002950815A0 (pt)
BR (1) BR0313497A (pt)
RS (1) RS20050145A (pt)
WO (1) WO2004016816A1 (pt)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009155652A1 (en) * 2008-06-27 2009-12-30 Bhp Billiton Ssm Development Pty Ltd Process for forming high density sulfides
EP3266885A4 (en) * 2015-03-05 2018-03-07 Sumitomo Metal Mining Co., Ltd. Method for producing nickel sulfide and hydrometallurgical method for nickel oxide ore

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2007100742B4 (en) * 2006-01-10 2008-04-03 Murrin Murrin Operations Pty Ltd Method for the Precipitation of Nickel
CA2636378A1 (en) * 2006-01-10 2007-07-19 Murrin Murrin Operations Pty Ltd. Method for the precipitation of nickel
WO2007095689A1 (en) * 2006-02-24 2007-08-30 Murrin Murrin Operations Pty Ltd Hematite precipitation at elevated temperature and pressure

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2722480A (en) * 1954-06-21 1955-11-01 Chemical Construction Corp Catalytic precipitation of nickel, cobalt and zinc sulfides from dilute acid solutions
US4110400A (en) * 1977-08-01 1978-08-29 Amax Inc. Selective precipitation of nickel and cobalt sulfides from acidic sulfate solution
US4410498A (en) * 1980-11-05 1983-10-18 Falconbridge Nickel Mines Limited Acid leaching of nickel from serpentinic laterite ores
US4547348A (en) * 1984-02-02 1985-10-15 Amax Inc. Conditioning of laterite pressure leach liquor
US5783057A (en) * 1996-09-19 1998-07-21 Nippon Mining & Metals Co., Ltd. Method of purifying copper electrolytic solution
US6391089B1 (en) * 2000-11-29 2002-05-21 Walter Curlook Acid leaching of nickel laterite ores for the extraction of their nickel and cobalt values

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE720881C (de) * 1939-02-05 1942-05-18 Ig Farbenindustrie Ag Verfahren zur Abtrennung von Schwermetallen, wie Zink, Cadmium und Nickel, aus eisen- und sulfatreichen, metallurgischen Laugen
CA1035152A (en) * 1974-09-19 1978-07-25 Inco Limited Recovery of nickel from nickel sulfate solutions
SU704231A1 (ru) * 1977-05-11 1981-07-30 Государственный Научно-Исследо-Вательский Институт Цветных Метал-Лов "Гинцветмет" Способ переработки железистыхНиКЕль-КОбАльТОВыХ лАТЕРиТОВыХРуд
CA1116412A (en) * 1979-05-10 1982-01-19 Kohur N. Subramanian Recovery of nickel and cobalt from leach slurries
JPS6032698B2 (ja) * 1980-03-28 1985-07-30 三菱マテリアル株式会社 マンガンノジユ−ルの硫酸浸出溶液中の銅，ニツケルおよびコバルトの回収方法
JPS6054378B2 (ja) * 1983-08-13 1985-11-29 三菱マテリアル株式会社 ニツケルイオンを含む酸性水溶液からのニツケルの回収方法
AUPN498595A0 (en) * 1995-08-23 1995-09-14 International Water Solutions Corporation Extraction of valuable metals
DE10022867A1 (de) * 2000-05-10 2001-11-22 Kronos Titan Gmbh & Co Ohg Verfahren zum Entfernen von Nickel- und Bleiionen aus Eisensalzlösungen
CN1166816C (zh) * 2000-11-28 2004-09-15 华东理工大学 含镍三氯化铁蚀刻废液再生和镍回收方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2722480A (en) * 1954-06-21 1955-11-01 Chemical Construction Corp Catalytic precipitation of nickel, cobalt and zinc sulfides from dilute acid solutions
US4110400A (en) * 1977-08-01 1978-08-29 Amax Inc. Selective precipitation of nickel and cobalt sulfides from acidic sulfate solution
US4410498A (en) * 1980-11-05 1983-10-18 Falconbridge Nickel Mines Limited Acid leaching of nickel from serpentinic laterite ores
US4547348A (en) * 1984-02-02 1985-10-15 Amax Inc. Conditioning of laterite pressure leach liquor
US5783057A (en) * 1996-09-19 1998-07-21 Nippon Mining & Metals Co., Ltd. Method of purifying copper electrolytic solution
US6391089B1 (en) * 2000-11-29 2002-05-21 Walter Curlook Acid leaching of nickel laterite ores for the extraction of their nickel and cobalt values

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009155652A1 (en) * 2008-06-27 2009-12-30 Bhp Billiton Ssm Development Pty Ltd Process for forming high density sulfides
US20110123418A1 (en) * 2008-06-27 2011-05-26 Bhp Billiton Ssm Development Pty Ltd Process for Forming High Density Sulfides
US8298501B2 (en) 2008-06-27 2012-10-30 Bhp Billiton Ssm Development Pty Ltd. Process for forming high density sulfides
EP3266885A4 (en) * 2015-03-05 2018-03-07 Sumitomo Metal Mining Co., Ltd. Method for producing nickel sulfide and hydrometallurgical method for nickel oxide ore
US10017835B2 (en) 2015-03-05 2018-07-10 Sumitomo Metal Mining Co., Ltd. Method for producing nickel sulfide and hydrometallurgical method for nickel oxide ore

Also Published As

Publication number Publication date
WO2004016816A1 (en) 2004-02-26
BR0313497A (pt) 2005-07-05
EP1546418A4 (en) 2005-11-23
EP1546418A1 (en) 2005-06-29
AU2002950815A0 (en) 2002-09-12
RS20050145A (en) 2007-06-04

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Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:CHAMBERLAIN, ANTHONY;TINDALL, GEOFFREY;WEDDERBURN, BRUCE;REEL/FRAME:016462/0035;SIGNING DATES FROM 20050408 TO 20050609

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