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WO2006074523A1 - Recovery of metals - Google Patents

Recovery of metals Download PDF

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Publication number
WO2006074523A1
WO2006074523A1 PCT/AU2006/000043 AU2006000043W WO2006074523A1 WO 2006074523 A1 WO2006074523 A1 WO 2006074523A1 AU 2006000043 W AU2006000043 W AU 2006000043W WO 2006074523 A1 WO2006074523 A1 WO 2006074523A1
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WO
WIPO (PCT)
Prior art keywords
ionic liquid
platinum
process according
group metal
electro
Prior art date
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Application number
PCT/AU2006/000043
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English (en)
Inventor
Martin Richard Houchin
Theo Rodopoulos
David Hughes Jenkins
Ewen James Silvester
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Commonwealth Scientific and Industrial Research Organization CSIRO
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Commonwealth Scientific and Industrial Research Organization CSIRO
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AU2005900150A external-priority patent/AU2005900150A0/en
Application filed by Commonwealth Scientific and Industrial Research Organization CSIRO filed Critical Commonwealth Scientific and Industrial Research Organization CSIRO
Publication of WO2006074523A1 publication Critical patent/WO2006074523A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C3/00—Electrolytic production, recovery or refining of metals by electrolysis of melts
    • C25C3/34—Electrolytic production, recovery or refining of metals by electrolysis of melts of metals not provided for in groups C25C3/02 - C25C3/32

Definitions

  • the present invention relates to the recovery of metals and, in particular, to the recovery of so-called platinum group metals (PGMs). More specifically, the present invention relates to the use of ionic liquids in metals recovery. The present invention also relates to certain ionic liquids that are useful in the recovery of PGMs.
  • PGMs platinum group metals
  • PGMs that is platinum (Pt), palladium (Pd), ruthenium (Ru), rhodium (Rh), iridium (Ir) and osmium (Os), occur in basic igneous rocks, often in association with nickel, copper and iron sulfides.
  • PGM minerals include native platinoids and their alloys, intermetallic compounds between PGMs and other (semi)metals, and sulfides and arsenides of the platinoids.
  • FIG. 1 A typical process for recovery of PGMs is shown in Figure 1. This process is practised, for example, in the Merensky horizon in South Africa. Initially, ore is treated to reduce it to a suitable particle size, followed by froth flotation and a gravity method to separate PGM particles. Part of the material obtained may be sent directly to the refinery with the remainder being concentrated further by techniques such as smelting, oxygen blowing, magnetic separation and pressure leaching. The final concentrate generally includes 50- 60% PGMs. Processes for refining the PGM concentrate vary but generally involve a complex series of steps including dissolution (often with Cl 2 -HCl), solvent extraction, distillation, ion exchange and precipitation. Overall the process tends to be complex and laborious. It would therefore be desirable to provide a simpler, more efficient refining process for recovery of PGMs.
  • the present invention seeks to address this need by providing an alternative pathway to recovery of PGMs. Disclosure of the Invention
  • the present invention provides a process for the recovery of a platinum group metal, which comprises the electro-deposition of the platinum group metal from an ionic liquid.
  • the invention may be applied for the electro-deposition of one or more PGMs.
  • PGMs for ease of reference, and unless otherwise stated, the present invention will be described with reference to electro-deposition of a single PGM.
  • the electro-deposition comprises electro- winning of the PGM from an ionic liquid in which a PGM precursor (a compound including the platinum group metal) has been dissolved.
  • the electro-deposition comprises electro- refining in which the PGM is transferred from one electrode to another electrode via the ionic liquid. In this case electro-deposition of the PGM still occurs from the ionic liquid.
  • ionic liquids may be used as a suitable solvent for PGMs and PGM precursors in order to facilitate electro- deposition of the PGM.
  • electro-deposition is used herein to embrace electro-winning and electro-refining processes.
  • the recovery of platinum and palladium is of particular interest, especially recovery of platinum.
  • Ionic liquids are a relatively new class of solvent. ILs are salts that are molten at, or near, ambient temperature, and have a number of properties that make them potentially attractive for a variety of industrial applications. These properties include:
  • Typical cations that may be used in ILs include the following:
  • the substituent groups R may be the same or different aliphatic or aromatic groups, or combinations of these groups.
  • the R group include alkyl, alkenyl, alkynyl and aryl groups and heteroaryl groups in which the hetero atom is selected from N, S, O, P, Si and Se.
  • the substituent groups may themselves be substituted by such groups as halogens and/or other functional groups.
  • Preferred functional groups include F and CN. Suitable substituents will be chosen on the basis that they enhance the desired properties/functionality of the ionic liquid and are stable under the process conditions.
  • the alkyl, alkenyl and alkynyl groups and moieties typically include up to about 10 carbon atoms. - A -
  • Anion components of ILs are typically smaller species, and include by way of example Cl “ , AlCl 4 ' , BF 4 " , PF 6 “ , NO 3 " and alkylsulfonate (RSO 3 -) anions.
  • Thiols (RS “ ), dithiocarbamates (RNCS 2 “ ) and xanthates (ROCS 2 “ ), in which the groups R are as defined above for the cationic component, are also believed to be useful in the formation of suitable ILs.
  • the anion may be selected from acetate, trifluoroacetate, substituted sulfonate (e.g. trifluoromethanesulfonate), bromide, tetracyanoborate, alkylsulfate, bis(trifiuoromethylsulfonyl)imide, bis(trifluoromethyl)imide and dicyanamide.
  • substituted sulfonate e.g. trifluoromethanesulfonate
  • bromide etracyanoborate
  • alkylsulfate bis(trifiuoromethylsulfonyl)imide, bis(trifluoromethyl)imide and dicyanamide.
  • the role of the anion component in an IL is often to control the miscibility properties of the ionic liquid, and the stability towards oxidation.
  • the anion may also have the role of stabilising (complexing) the PGM ion in solution, and an important aspect of the present invention is the selection of ILs having anion species that has/have a specific affinity for the PGM ion of interest.
  • the basis of this approach is that the anion species forms a complex with the target PGM ion, giving higher concentrations of the PGM ion in solution, thereby allowing higher current densities to be achieved. This advantageous property must however be balanced against the higher electro-deposition voltage required due to the higher stability of the complexed metal ion.
  • the ionic liquid is generally selected on the basis that:
  • the PGM precursor or at least the PGM component(s) of interest of the precursor, is substantially soluble in the IL. This criterion includes considerations such as the rate of solubilisation, variation of solubility with temperature, and the maximum solubility attainable.
  • the dissolution of the PGM precursor or PGM component must be sufficient to make the process economically viable.
  • the concentration of PGM, measured as the metal will be greater than 2Og per litre of ionic liquid.
  • the anion component of the ionic liquid must have sufficient affinity towards the PGM cation to displace at least some of this water into the bulk IL, from where the water can be removed by physical means (e.g. heating and/or vacuum).
  • the IL must be stable enough (and non- volatile enough) to withstand the "water-removal" process.
  • the solvated PGM cation or cation comprising the PGM must have a half-cell potential (under the conditions being used) that is within the electrochemical stability window of the IL. In other words, the cation must be able to form a metallic deposit of the PGM at a potential at which the ionic liquid does not decompose.
  • a further desirable characteristic of the IL might be that it allows for selective electrodeposition of one or more PGMs from a PGM precursor dissolved in the IL. Separation of PGMs (via selective recovery of PGMs), as distinct from bulk recovery of mixed PGMs, is an important consideration. This would require the IL to provide half cell potentials for electrodeposition of various PGMs such that separation of PGMs via control of the electrodeposition potential (voltage) becomes possible.
  • Ionic liquids possess a range of physical properties depending on the anion/cation combination.
  • a low melting point ionic liquid means that minimal energy requirements are needed to maintain liquid form.
  • Ionic liquids useful in the invention may have a range of viscosities, again depending on the anion/cation combination.
  • a high viscosity ionic liquid means that ionic diffusion is low and this often limits the deposition currents.
  • a low viscosity means that ionic diffusion is high. ie. the diffusion is dependent on the viscosity of the solution.
  • the viscosity of ionic liquids useful in the present invention is usually from 1 to 50,00OcP at room temperature.
  • a suitable IL for any given PGM/PGM precursor may be determined based on these considerations. It should also be noted that preferably the IL is one that may be recycled for repeated use in the process of the present invention. Recycling may involve doing very little if the IL only (selectively) dissolves the PGM component to be recovered (eg, similar to recycling the organic extractant solution in solvent extraction/electro-winning processes).
  • impurities are formed in the ionic liquid during the electrodeposition process, they may be removed using appropriate existing technologies, depending on the nature of the impurities, for instance solid/liquid separation (filtration, settling/decanting), with or without a preceding precipitation step, further electrodeposition of other dissolved species, decomposition of dissolved impurities (eg organics), extraction of dissolved species into a non-miscible phase, removal of volatile impurities by heat/vacuum treatment etc.
  • solid/liquid separation filtration, settling/decanting
  • further electrodeposition of other dissolved species decomposition of dissolved impurities (eg organics)
  • extraction of dissolved species into a non-miscible phase removal of volatile impurities by heat/vacuum treatment etc.
  • the PGM precursor may be a primary source, e.g. a mineral, ore, matte or concentrate, or a secondary source from which the PGM is to be recovered and recycled, e.g. a catalytic converter or any other PGM-containing material.
  • a primary source e.g. a mineral, ore, matte or concentrate
  • a secondary source from which the PGM is to be recovered and recycled e.g. a catalytic converter or any other PGM-containing material.
  • the PGM precursor may be directly dissolved in the ionic liquid (with or without addition of an oxidant or reductant to assist dissolution) and the desired PGM recovered by electrodeposition as in electro-winning.
  • material including the PGM may be oxidised or reduced by application of a voltage resulting in dissolution of the PGM from the material and electro-deposition, as in electro-refining.
  • these particular techniques rely on the use of an ionic liquid, as is described herein. Otherwise they are practised in a conventional manner using conventional equipment and methodology.
  • an IL comprising 1 -methyl- 1-butyl- pyrrolidinium methanesulfonate and aluminium nitrate facilitates deposition of platinum during an electro-deposition process.
  • This IL is described in more detail in the examples included herein.
  • This example demonstrates the dissolution of Pt from a Pt anode and its subsequent electro-deposition on a glassy-carbon working electrode. This is equivalent to the industrial process of electro-refining.
  • the example also demonstrates the important role the additive A1(NO 3 ) 3 plays.
  • the ionic liquid used was 1 -methyl- 1-butyl-pyrrolidinium methanesulfonate (PuCH 3 SO 3 ) with and without 0.1 molal A1(NO 3 ) 3 .
  • the electrochemical cell used was a three-electrode arrangement with a glassy carbon working electrode, a platinum counter electrode and a silver pseudo-reference electrode.
  • a schematic diagram of the electrochemical cell is shown in Figure 3.
  • the ionic liquid used was the P 14 CH 3 SO 3 , initially without added A1(NO 3 ) 3 . As the ionic liquid rapidly absorbs moisture from the air, the electrochemical cell was continually flushed by a bleed of dry nitrogen during the tests.
  • this ionic liquid has a melting point of approximately 63 °C, it was necessary to complete the electrochemical tests at a temperature above the melting point.
  • the cell was suspended in a 170 mm diameter crystallising dish containing silicon oil on a hotplate thermostatically controlled at 95°C.
  • the voltage and current were supplied to the electrochemical cell from a Pine Instrument Company Bipotentiostat model No AFCBPl.
  • a DT 500 Datataker was used to log the voltage and current during the experiment.
  • a platinum RTD which measured the temperature of the silicon oil, was connected to the Datataker. Data was logged every 15 seconds during the electro-deposition tests and every 1 second during the cyclic voltammetry tests.
  • the voltage of -250 mV was applied to the glassy carbon working electrode for approximately five hours. At the end of the test, the potentiostat was switched off.
  • the current/time plot for the P 14 CH 3 SO 3 deposition test shown in Figure 4 indicates that the current was initially negative (-4.45 ⁇ mA) but gradually increased to a positive value of approximately 0.35 ⁇ mA.
  • the conditions of this test are shown in the following table.
  • the current time curve for this test is shown in Figure 5 and indicates that the current initially increased but then decreased through the test. Unlike the test using the "as produced" P 14 CH 3 SO 3 , here the current was negative for the whole test.
  • the glassy carbon working electrode was examined by SEM.
  • Figure 6 shows a view of the lower end of the glassy carbon working electrode with metallic deposits in place.
  • Shown in Figure 7 is a close-up view of the platinum deposit shown in Figure 6 while the EDAX scan for this particle is shown in Figure 8. This scan indicates that, while platinum is the major component, silver and aluminium were also detected. Silver was deposited from the ionic liquid as the ionic liquid was prepared from silver methane sulfonate and still contains some of the silver salt.
  • the previous example confirmed the deposition of platinum on the glassy carbon electrode during five hour electro-deposition tests from 1 -methyl- 1-butyl-pyrrolidinium methanesulfonate (P 14 CH 3 SO 3 ) containing 0.1 molal A1(NO 3 ) 3 . These tests used -250 mV (as was used in Example 1) as well as -400 mV.
  • the initial intention was to produce a solution containing 0.1 molal H 2 PtCl 6 .6H 2 O, i.e. similar to the amount of A1(NO 3 ) 3 dissolved in the P 14 CH 3 SO 3 solution in Example 1.
  • the platinum salt did not readily dissolve in the hot P 14 CH 3 SO 3 so the final solution concentration was only 0.0736 molal.
  • Additional water was added to the platinum containing P 14 CH 3 SO 3 and the solution evaporated using a Rotavopor. Initially, the solution became clear but as the water was evaporated, crystals appeared in the solution. Nevertheless, the solution was stored in a vacuum oven overnight prior to being dehydrated at 105 0 C using the high vacuum system.
  • the solution bubbled, indicating that moisture was being removed from the system and the solution gradually cleared over time, producing a dark brown liquid. After dehydration for 24 hours, the solution was stoppered and stored in an oven at 100° C prior to use.
  • a series of cyclic voltammetry tests were completed on a sample of the above solution. Tests were completed at approximately 100°C using voltage ranges of ⁇ 250 mV, ⁇ 500 mV, ⁇ 1000 mV, ⁇ 1500 mV, ⁇ 2000 mV and ⁇ 2500 mV. The previously used platinum- flag counter-electrode was replaced by a spiral of platinum wire.
  • Figure 9 Figure 10 and Figure 11 show cyclic voltammograms completed at approximately 100°C at a sweep rate of 10 mV/s using the P 14 CH 3 SO 3 ZH 2 PtCl 6 solution at voltage ranges of ⁇ 500 mV, ⁇ 1500 mV and ⁇ 2000 mV.
  • Figure 9 shows a peak in the voltammogram at approximately -250 mV, which was the voltage used in the test using platinum containing ionic liquids. This voltage may correspond to the silver deposition voltage.
  • Figure 10 shows the -250 mV peak as well as a further peak at approximately -750 mV while the voltammogram, shown in Figure 11, shows three peaks. It is believed that the two peaks at -750 mV and -1750 mV may correspond to the following cathode reactions
  • the platinum deposit was dissolved in a small volume of aqua regia.
  • the aqua regia bubbled when the electrode was placed in the liquid. Dissolution of the platinum deposit was deemed to be complete when the bubbling had almost finished.
  • the dissolved platinum was transferred to a 50 niL volumetric flask and made to volume for subsequent platinum analysis. The analysis of this solution indicated that it contained 0.108 mg of platinum.
  • the charge, in coulombs, required to deposit 0.108 mg of platinum was calculated based upon Avogadro's number and the elemental charge for platinum.
  • the charge added during the test was calculated by summing the average current during each 15 second logging interval multiplied by the deposition time. From these calculations the approximate efficiency of platinum deposition was determined for the test and is shown in the following table.
  • NH 4 NO 3 was selected as the ammonium salt to add to the ionic liquid.
  • the NH 4 NO 3 equivalent to 0.141 molal, dissolved relatively easily in the ionic liquid Pi 4 CH 3 SO 3 solution during dehydration at approximately 10O 0 C- 105 0 C using high vacuum.
  • the colour of the ionic liquid did not change during dehydration and remained a pale straw colour.
  • the concentration OfNH 4 NO 3 in the ionic liquid was slightly less than the theoretical molality as the salt was not dried prior to its addition to the ionic liquid. After dehydration for 24 hours, the solution was stoppered and stored in an oven at 11O 0 C prior to use.
  • the potential used for the electro-deposition test from the P 14 CH 3 SO 3 containing NH 4 NO 3 was -2100 mV based upon the deposition peak observed in this cyclic voltammogram. Like the previous tests, this test ran for over five hours at a temperature of 115°C.
  • a sample of the ionic liquid was withdrawn from the cell, weighed and made to volume for subsequent platinum analysis. Chemical analysis of this sample indicated that it contained 0.29% platinum.
  • the glassy-carbon electrode was initially washed with acetone and subsequently stored overnight in water to dissolve any adhering ionic liquid.
  • a counter electrode was constructed using some platinum/13% rhodium thermocouple (T/C) wire, which was tested using a P 14 CH 3 SO 3 ionic liquid solution.
  • the solution used was the P 14 CH 3 SO 3 ionic liquid containing 0.025 molal K 2 PtCl 6 .
  • thermocouple wire Pt/13% Rh
  • platinum to rhodium ratio is shown in the table below. Also shown in this Table are the weights of the platinum and rhodium dissolved from the glassy-carbon electrode by aqua-regia at the end of the electro-deposition test and the platinum rhodium ratio in the deposits. This Table indicates that more platinum was deposited in the test than rhodium, compared to the amounts of these metals in the counter-electrode.
  • Figure 23 shows an SEM photomicrograph of the base of the glassy-carbon electrode while Figure 24 shows a close-up view of the deposit.
  • the deposit formed in this test appears similar to the deposits produced during electro-deposition from other platinum salt containing ionic liquid tests.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A process for the recovery of a platinum group metal, which comprises the electro-deposition of the platinum group metal from an ionic liquid.
PCT/AU2006/000043 2005-01-13 2006-01-13 Recovery of metals Ceased WO2006074523A1 (fr)

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AU2005900150 2005-01-13
AU2005900150A AU2005900150A0 (en) 2005-01-13 Recovery of Metals

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2368706C2 (ru) * 2007-09-25 2009-09-27 Институт высокотемпературной электрохимии Уральского отделения Российской академии наук Способ очистки расплавленного хлоридного электролита для получения платиновых металлов
US8361300B2 (en) 2006-02-15 2013-01-29 Akzo Nobel N.V. Method to electrodeposit metals using ionic liquids
EP3263744A1 (fr) * 2016-07-01 2018-01-03 Commissariat à l'énergie atomique et aux énergies alternatives Procédé de récupération de platine, par voie électrochimique, à partir d'un matériau dans lequel il est contenu
FR3099492A1 (fr) 2019-08-02 2021-02-05 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de recuperation de rhodium par voie electrochimique
US11434576B2 (en) * 2016-12-08 2022-09-06 Clean Resources Pte. Ltd Recovery of gold and silver from precious metals-containing solids

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001013379A1 (fr) * 1999-08-18 2001-02-22 British Nuclear Fuels Plc Procede de separation de metaux
US20020070122A1 (en) * 2000-10-20 2002-06-13 The University Of Alabama Production, refining and recycling of lightweight and reactive metals in ionic liquids
US6552843B1 (en) * 2002-01-31 2003-04-22 Innovative Technology Licensing Llc Reversible electrodeposition device with ionic liquid electrolyte
US20040262166A1 (en) * 2003-06-24 2004-12-30 O'gardy William E. Low temperature refining and formation of refractory metals
US20050106440A1 (en) * 2003-11-19 2005-05-19 Honda Motor Co., Ltd. Proton conductor and method for producing the same
WO2005103338A1 (fr) * 2004-04-27 2005-11-03 Technological Resources Pty. Limited Production d'alliages de fer/titane

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001013379A1 (fr) * 1999-08-18 2001-02-22 British Nuclear Fuels Plc Procede de separation de metaux
US20020070122A1 (en) * 2000-10-20 2002-06-13 The University Of Alabama Production, refining and recycling of lightweight and reactive metals in ionic liquids
US20040238352A1 (en) * 2000-10-20 2004-12-02 The University Of Alabama Production, refining and recycling of lightweight and reactive metals in ionic liquids
US6552843B1 (en) * 2002-01-31 2003-04-22 Innovative Technology Licensing Llc Reversible electrodeposition device with ionic liquid electrolyte
US20040262166A1 (en) * 2003-06-24 2004-12-30 O'gardy William E. Low temperature refining and formation of refractory metals
US20050106440A1 (en) * 2003-11-19 2005-05-19 Honda Motor Co., Ltd. Proton conductor and method for producing the same
WO2005103338A1 (fr) * 2004-04-27 2005-11-03 Technological Resources Pty. Limited Production d'alliages de fer/titane

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
GOLDING J. ET AL.: "Methanesulfonate and P-Toluenesulfonate Salts of the N-Methyl-N-Alkylpyrrolidinium and Quaternary Ammonium Cations: Novel Low Cost Ionic Liquids", GREEN CHEMISTRY, vol. 4, no. 3, 2002, pages 223 - 229 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8361300B2 (en) 2006-02-15 2013-01-29 Akzo Nobel N.V. Method to electrodeposit metals using ionic liquids
RU2368706C2 (ru) * 2007-09-25 2009-09-27 Институт высокотемпературной электрохимии Уральского отделения Российской академии наук Способ очистки расплавленного хлоридного электролита для получения платиновых металлов
EP3263744A1 (fr) * 2016-07-01 2018-01-03 Commissariat à l'énergie atomique et aux énergies alternatives Procédé de récupération de platine, par voie électrochimique, à partir d'un matériau dans lequel il est contenu
FR3053364A1 (fr) * 2016-07-01 2018-01-05 Commissariat Energie Atomique Procede de recuperation de platine, par voie electrochimique, a partir d'un materiau dans lequel il est contenu
US11434576B2 (en) * 2016-12-08 2022-09-06 Clean Resources Pte. Ltd Recovery of gold and silver from precious metals-containing solids
FR3099492A1 (fr) 2019-08-02 2021-02-05 Commissariat A L'energie Atomique Et Aux Energies Alternatives Procede de recuperation de rhodium par voie electrochimique

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