WO2016018433A1 - Cellule électrochimique de récupération de métaux à partir d'oxydes métalliques solides - Google Patents

Cellule électrochimique de récupération de métaux à partir d'oxydes métalliques solides Download PDF

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Publication number
WO2016018433A1
WO2016018433A1 PCT/US2014/049455 US2014049455W WO2016018433A1 WO 2016018433 A1 WO2016018433 A1 WO 2016018433A1 US 2014049455 W US2014049455 W US 2014049455W WO 2016018433 A1 WO2016018433 A1 WO 2016018433A1
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Prior art keywords
electrode
metal oxide
electrochemical cell
oxygen ion
electrolyte
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PCT/US2014/049455
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English (en)
Inventor
Kyle BRINKMAN
Brenda L. Garcia-Diaz
Joshua R. Gray
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Savannah River Nuclear Solutions, Llc
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Publication of WO2016018433A1 publication Critical patent/WO2016018433A1/fr

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    • 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
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/02—Electrodes; Connections thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/04—Diaphragms; Spacing elements

Definitions

  • Electrolytic processes have been used to recover high purity metals (e.g., uranium) from the mixture of elements in used nuclear fuel, also known as spent nuclear fuel, as well as from mined ores containing desirable metals.
  • these processes are carried out in electrochemical cells in which an oxide of the metal to be recovered (e.g., uranium oxide) is dissolved in a molten salt electrolyte.
  • the cells also include two electrodes that can be submerged in the molten salt electrolyte.
  • the first electrode can include an inert electron-conducting material such as steel or other suitable metal and the second electrode can encourage oxidation of oxygen ions.
  • the molten salt electrolyte is an ionic conductor that allows the ionic species to separate, with the metal ions driven to and being deposited at the first electrode and the oxygen ions driven to the second electrode where oxidation occurs and molecular oxygen, carbon monoxide, carbon dioxide, or the like is generated.
  • Oxygen ion conducting membranes such as yttria-stabilized zirconia membranes, have also been incorporated in these types of electrochemical cells. Such membranes can improve separation of the ionic species within the cells and help to prevent corrosion of the electrodes.
  • an electrochemical cell that includes a first electrode and a second electrode. More specifically, the first electrode includes a solid metal oxide and a first current collector and the second electrode includes a material that encourages the oxidation of oxygen ion and a second current collector.
  • the electrochemical cell also includes an electrolyte that in turn includes an alkali metal or alkaline earth metal salt or a eutectic or mixture thereof that is molten at the operating temperature of the cell.
  • An oxygen ion conducting compound is mixed with the electrolyte.
  • the electrochemical cell includes an oxygen ion conducting membrane that separates the electrolyte from the second electrode.
  • the method can include locating the first electrode in the electrochemical cell and applying a voltage potential across the first and second electrodes.
  • the voltage potential is greater than the dissociation potential of the metal oxide and thus drives reaction of the metal oxide to form oxygen ions and a solid metal in the place of the solid metal oxide of the first electrode.
  • the oxygen ions are conducted across the electrolyte via the oxygen ion conductor and across the oxygen ion conducting membrane to the second electrode.
  • the oxygen ions are oxidized at the second electrode to form a molecular oxygen species (e.g., molecular oxygen, carbon dioxide, etc.).
  • the first electrode includes a solid uranium oxide and a current collector and the method can be used to purify uranium from spent nuclear fuel.
  • FIG. 1 schematically illustrates one embodiment of an electrochemical cell as described herein.
  • FIG. 2 schematically illustrates another embodiment of an electrochemical cell as described herein.
  • FIG. 3 illustrates an electrochemical cell utilized in the Example section described herein.
  • FIG. 4 graphically illustrates the equilibrium potential of the cell with cell temperature for several different molten salt electrolytes and for lithium oxide.
  • FIG. 5 illustrates the change in cell current and charge with time during cell operation.
  • FIG. 6 illustrates the oxygen generated at the second electrode with time during cell operation.
  • the present disclosure is generally directed to an electrochemical cell and methods of using the electrochemical cell. More specifically, the electrochemical cell can be utilized for the recovery of metals from metal oxides.
  • the electrochemical cell can be utilized for the recovery of metals from metal oxides.
  • the reduction reactions begin at the metal oxide-containing electrode, conductive reaction products are formed and the effective contact area between the conductive elements of the electrode and the oxides of the electrode will increase. This can increase the reaction rate (which can be demonstrated by an increase in current in the cell) and drive the complete reduction of the solid metal oxide.
  • metallic (and conductive) cerium will be formed. As the metallic cerium is formed where the cerium oxide contacts the current collector, the conductive phase of the electrode will grow, which can increase the current across the cell and increase the reaction rate for the metal formation.
  • the reaction rates of the cell can increase quickly leading to reduction of the metal oxide in relatively short order when processing metal oxides that form Magneli phases, which are electrically conductive sub-stoichiometric phases that can form prior to complete reduction to the metal and dissociation of the oxygen ion. Such phases are known for certain metal oxides including titanium dioxide and uranium dioxide, and may exist for others.
  • the formation of the conductive sub-stoichiometric phases e.g., Ti 4 O 7 , Ti 3 O 5 , ⁇ 2 ⁇ 3, etc.
  • the conductive sub-stoichiometric phases will encourage increase in conduction and increase in conductive surface area throughout the electrode and thus further reduction to the pure metal.
  • the electrochemical cell can include a first electrode 2, an electrolyte 4 that has an oxygen ion conducting compound mixed with the electrolyte, an oxygen ion conducting membrane 8, and a second electrode 6.
  • the first and second electrodes 2, 6 are in electrical communication with one another via a first current collector 10 of the first electrode 2 and a second current collector 12 of the second electrode 6 that are electrically connected to one another in conjunction with a device or system that can establish a voltage potential across the first electrode 2 and the second electrode 6.
  • the first electrode also includes a solid oxide of the metal to be recovered.
  • the reduction products can initially include both the reduced metal and Magneli phases, depending upon the particular metal oxide of the first electrode.
  • the voltage potential can drive the oxygen ions across the electrolyte 4 via the oxygen ion carrying compound that is combined with the electrolyte 4 in a mixture.
  • the oxygen ions can then be conducted across the membrane 8 to the second electrode 6, where they are oxidized and can exit the cell, as at 14.
  • the electrode 2 can be simply removed from the electrochemical cell and replaced with a new electrode that includes metal oxide.
  • use of the cell can provide the purified metal in an easily retrievable form and allow for faster and more economical recovery of purified metals from metal oxides.
  • the electrochemical cells and methods utilizing the cells can be any electrochemical cells and methods utilizing the cells.
  • the electrochemical cell is not limited to this use, however, and may advantageously be utilized to recover purified metals of any type from the oxide form of the metal.
  • the electrochemical cell may be useful in recovery of metals from mining operations or in recycling
  • the electrode 2 can include the metal oxide in any suitable form.
  • the metal oxide can be pre-processed according to standard methodology to increase the surface area.
  • the metal oxide can be chopped or ground prior to location in the electrochemical cell to form metal oxide particles that can have a cross sectional dimension of about 2
  • a container which can be, for example, a basket or other suitable container.
  • the used metal oxide can be preprocessed according to other processing techniques as are known in the art. For instance used nuclear fuel including uranium dioxide can be subjected to high temperature treatments including voloxidation that can be utilized to capture tritium, iodine, technetium, etc.
  • the pre-processing steps may remove all or part of specific fission products. It should be understood, however, that this disclosure applies to any metal oxide composition that can result from any combination of pre-processing steps.
  • an electrode container (, FIG. 3) can be formed of any suitable material that is resistant to the components of the cell (e.g., the molten salts of the electrolyte) and that can provide contact between the electrolyte and the metal oxide of the first electrode held in the container.
  • the container can be a porous container formed of a corrosion resistant material including carbon
  • a container can be formed of a glassy carbon material.
  • any metal of the container can be insulated from the metal oxide held within the container, for instance by inclusion of an insulative covering on at least that portion of a metal or metal alloy of the container that would otherwise contact the metal oxide of the first electrode.
  • the metal oxide of the first electrode 2 can be provided in a high surface area form such as chopped or ground materials. This is not a requirement of the electrochemical cell, however, and the metal oxide may be in the form of a single or multiple solid pieces that can include porosity or not, as desired.
  • the metal oxide of the first electrode 2 can include a plurality of pores that extend across all or a portion of a single solid metal oxide piece.
  • a porous metal oxide component of the first electrode 2 can have a void fraction of from about 5% to about 90%, from about 10% to about 80%, or from about 20% to about 70%.
  • the oxygen ion formed upon dissociation of the metal oxide can diffuse out of the first electrode 2 to the electrolyte 4.
  • oxide ion can diffuse through metal that may have already formed in the first electrode 2. This allows for the metal oxide conversion to be carried out throughout the depth of the solid oxide material of the first electrode 2 and provides in one embodiment for complete conversion of the metal oxide to the desired metal.
  • the electrode 2 can include current collector 10 that can be capable of use at the expected operating temperatures of the electrochemical cell.
  • Examples of electrically conductive materials from which the current collector 10 can be formed include, without limitation, metallic materials based on nickel, tungsten, molybdenum, and cobalt as well as carbon based materials such as glassy carbon and graphite. Alloys including refractory metals such as niobium, molybdenum, tantalum, tungsten, and rhenium as well as conductive ceramics and composite materials can also be utilized in forming the current collector 10. For example, stainless steel may be utilized as a current collector in some embodiments.
  • the current collector 10 may be useful in some embodiments to provide the current collector 10 in an arrangement with the metal oxide so as to provide for a high contact area between the two, as this can increase the starting reaction rate of the dissociation and reduction reactions.
  • the current collector 10 can be in the form of a high surface area plate or leaf that is submerged within the metal oxide to allow for maximum possible contact area between the two.
  • the metal oxide can be in the form of particles and the container used to hold the particles can also function as a current collector, which can provide a high contact area between the current collector and the metal oxide of the first electrode 2.
  • the electrolyte 4 includes one or more salts that can be held in the form of a molten salt electrolyte bath during operation of the cell 10.
  • the salts can include any alkali metal or alkaline earth metal halide salt, or eutectics or mixtures thereof.
  • the electrolyte can include one or more chloride salts of sodium, potassium, lithium, magnesium, calcium, aluminum, one or more fluoride salts of sodium, potassium, lithium, magnesium, calcium, aluminum, cryolite (Na3AIF 6 ), mixtures thereof, and so forth.
  • the electrochemical cell can also include an oxygen ion conducting compound.
  • the ion conducting compound can be an oxygen ion conducting oxide that is an alkali metal or alkali earth metal oxide such as an oxide of lithium, calcium, aluminum, magnesium, zinc, silicon, titanium, lead, or mixtures thereof.
  • the ion conducting compound can include an oxide of the metal to be recovered.
  • the electrochemical cell also includes an oxygen ion conducting
  • the oxygen ion conducting membrane 8 can have a molecular framework structure that permits the oxide ions to move from the electrolyte 4 to the second cathode 6, without exposing the second cathode 6 to the molten salts of the electrolyte 4.
  • the oxygen ion conducting membrane 8 can include a solid electrolyte composition formed between oxides containing divalent and/or trivalent cations such as alkaline earth oxides, e.g., calcium oxide, or rare earth oxides, e.g., scandium oxide, yttrium oxide, lanthanum oxide, etc., and oxides containing tetravalent cations such as zirconia, hafnia, thoria and ceria.
  • the oxygen ion conducting phases of the membrane 8 can be a mixed metal oxide having a fluorite structure, for instance a doped fluorite compound.
  • the fluorite crystal structure can provide large amounts of oxygen vacancy when substituted with the aliovalent oxides.
  • one oxygen ion vacancy can occur for each divalent or each two trivalent cations that are substituted for a tetravalent ion in the lattice. Accordingly, the membrane can exhibit have high oxygen mobility and oxygen ion conduction.
  • the oxygen ion conducting membrane 8 can include zirconia (ZrO 2 ) or hafnia (HfO 2 ) stabilized in cubic form by a divalent or trivalent metal oxide dopant such as MgO, NiO, SrO, CaO, NiO, Y 2 O 3 , Sc 2 O 3 , La 2 O 3 , Gd 2 O 3 and Ce 2 O 3 .
  • the oxygen ion conducting membrane 8 can include zirconia stabilized by addition of yttria (Y 2 O 3 ).
  • the oxygen ion conducting membrane 8 may comprise predominately hafnia or ceria (CeO 2 ) doped with one or more divalent or trivalent metal oxides.
  • Additional examples of materials for the oxygen ion conducting membrane 8 include strontium- and magnesium-doped lanthanum gallate (LSGM). Many other oxides are known which have demonstrated oxygen ion-conducting ability, which could be used as the oxygen ion conducting membrane 8.
  • LSGM strontium- and magnesium-doped lanthanum gallate
  • additives that may be found in the oxygen ion conducting membrane 8 can include, without limitation, AI 2 O 3 and Fe 2 O 3 . These oxides may provide other benefits, such as mixed conduction and lower overvoltage.
  • the oxygen ion conducting membrane 8 may generally be provided as a layer or sheet electrically connected to the second electrode 6 and forming a barrier between the second electrode 6 and the electrolyte 4, as shown in FIG. 1 .
  • the oxygen ion conducting membrane 8 can have a thickness of about 0.5 millimeters or less, or about 0.2 millimeters or less in some embodiments.
  • the solid oxide electrolyte membrane can be in any shape, however, and is not limited to a layer or sheet.
  • the oxygen ion conducting membrane 8 is in a tubular shape, with one end of the tube being closed with a plug 16 formed of a suitable material that can withstand the operating temperatures of the cell, for instance a metallic or polymeric plug 16.
  • Another suitable shape illustrated in FIG. 2 and discussed further herein is in the form a container 208 that can hold the electrolyte 204.
  • the electrochemical cell also includes a second electrode that includes a material to encourage oxidation of the oxygen ion to produce molecular oxygen.
  • Suitable oxygen-producing materials possess high electronic conductivity (for example about 10 S/cm or greater) and charge
  • Exemplary oxygen-producing materials of the second electrode include, without limitation, a noble metal (e.g., platinum), silver alloys (Silver-Copper, Silver- Tin etc.), cermets, electronic oxides and composites thereof with stabilized zirconia.
  • a cermet can be for example a composite of an oxygen stable noble metal such as iridium or platinum and a stabilized zirconia. The noble metal can be capable of withstanding the operating temperatures of the cell without melting.
  • Stabilized zirconia may be a rare earth element- or alkaline earth-stabilized zirconia, such as zirconia stabilized with yttria, calcium oxide, scandium oxide and the like as discussed above.
  • Other cermets as are known in the art may be utilized. For instance, a cermet including a sintered combination of iron and nickel oxides with copper and/or silver may be utilized.
  • the second electrode can include an oxygen stable electronic oxide such as strontium-doped lanthanum manganite (Lai -X
  • Sr x MnO3 (LSM)
  • Other stable electronic oxides as may be utilized include A-site deficient acceptor-doped lanthanum ferrite and lanthanum cobaltite, e.g., Lai -X A x FeO3 and/or Lai -x A x CoO3.
  • the oxygen producing materials may include one or more dopants from the group consisting of Ca, Ce, Pr, Nd, and Gd in the La site and from the group consisting of Ni, Cr, Mg, Al, and Mn in the Fe or Co site; Fe may also be used as a dopant in the cobalt site.
  • Dopant materials and amounts for electronic oxides such as lanthanum ferrite and the lanthanum cobaltite may be selected to decrease the thermal expansion of the ceramic and to provide a closer thermal match to the oxygen ion conducting membrane.
  • La(Ca,Ce,Sm,Pr,Gd,Nd) Fe(Mn,Ni,AI,Cr,Mg)O3 -x and La(Ca,Ce,Sm,Pr,Gd,Nd)Co(Mn,Ni,AI,Cr,Mg,Fe)O 3- x powders of varying compositions can synthesized by mixing high purity precursors of carbonates and oxides in appropriate stoichiometric ratios and calcining them at a temperature of about 1200°C to about 1300°C for about 4 hours in air, as known. The calcined powders can be lightly crushed and the calcination step can be repeated to complete the solid-state reaction.
  • the oxygen-producing material of the second electrode may be a composite material including an electronically conducting oxide and a stabilized zirconia.
  • the oxygen-producing material of the second electrode can alternatively include a carbonaceous substance that can form a carbon oxide upon oxidation of the oxygen ion, e.g., carbon dioxide and/or carbon monoxide.
  • the carbonaceous material may be produced by molding petroleum coke and coal tar pitch followed by heat treatment at about 1000°C to about 1200°C.
  • the second electrode 6 can be in the form of a porous layer on the oxygen ion conducting membrane 8.
  • the second electrode 6 can be applied as a layer, coating, or film on the oxygen ion conducting membrane 8 via a suitable technique such as flame spraying, plasma spraying, sputtering, evaporation, laser ablation, chemical vapor deposition, spray deposition, molecular beam epitaxy, or any other suitable application technique.
  • the second electrode 6 can be formed as a thin membrane or film and can be laminated to the oxygen ion conducting membrane 8.
  • the porosity of the second electrode 6 can be suitable to allow diffusion of the molecule oxygen species that is formed at the anode.
  • the second electrode can have a porosity of about 50% or less, or from about 20% to about 40% in one embodiment.
  • the current collector 12 of the second electrode 6 can include any suitable conductive material a is known in the art such as, and without limitation, iridium or other noble metals such as platinum or a solid (non-porous) sintered rod of the aforementioned anode material (electronic oxides, cermets and electronic oxide composites).
  • a voltage potential that is greater than the dissociation potential of the metal oxide can be placed across the first and second electrodes 2, 6, via the current collectors 10, 12.
  • Any method or device as is generally known in the art may be utilized to control the voltage potential across the first and second electrodes of the electrochemical cell. In general, the voltage potential for the reaction can be about 30 volts or less.
  • the preferred voltage potential can depend on a plurality of parameters including the electrode spacing as well as the thickness of the solid oxide membrane. For instance, if the electrodes are spaced far apart and/or if the solid oxide membrane is significantly thicker, the voltage potential may be greater than about 30V.
  • the electrochemical cell of FIG. 1 includes a surrounding tank 18 that can be formed of any suitable insulative or conductive material and in any suitable configuration.
  • the tank 18 can be formed of a coated steel or other metallic material or a polymeric material that can withstand the operating conditions and components of the system.
  • Temperature control elements such as coils, etc. (not shown in FIG. 1 ) can be associated with the tank 18 to control the temperature of the electrolyte 4, as is known.
  • the temperature of the galvanic cell during operation can be from about 300°C to about 1000°C, or from about 300°C to about 800°C, in one embodiment.
  • FIG. 2 A second embodiment of an electrochemical cell is illustrated in FIG. 2.
  • the oxygen ion conducting membrane 208 in the form a container 208 that can hold the electrolyte 204.
  • the second electrode 206 is in electrical communication with the oxygen ion conducting membrane 208 and the first electrode 202 is immersed in the electrolyte 204 that also carries an oxygen ion conducting compound as discussed above.
  • the first current collector 210 and the second current collector 212 are in electrical communication with one another such that a voltage potential can be placed across the cell that is greater than the dissociation potential of the metal oxide of the first electrode 202.
  • a molecular oxygen species can be released from the electrochemical cell as at 214, as discussed above for the electrochemical cell of FIG. 1 .
  • the first electrode can be removed from the cell for recovery of the metal.
  • Another electrode including a metal oxide can then be immersed in the electrolyte, and the process can be repeated.
  • the recovered metal can be processed for recovery as desired.
  • metallic uranium can be converted to metallic uranium in pellets, ingots, or other forms and in one particular embodiment, uranium as may be utilized as a fuel.
  • the recovered metal can also be mixed with other metallic species to form a mixture of metals or alloy.
  • recovered uranium can be mixed with other metallic fission products including but not limited to actinides such as plutonium, neptunium, americium, and curium.
  • the mixture of metals including the recovered uranium could be used as fuel.
  • An electrochemical cell as described herein and schematically illustrated in FIG. 3 was utilized to reduce CeO2 as a surrogate of used nuclear fuel to yield a metallic product.
  • the CeO2 was chopped and located in a basket formed of graphite that was immersed in one of a variety of electrolytes mixed with 3 wt.% Li 2 O based on the weight of the electrolyte.
  • the current collector formed of metallic tungsten was immersed in the CeO2.
  • a yttria stabilized zirconia (YSZ) membrane coated on a surface with platinum was formed into a tube with the platinum on the interior of the tube and isolated from the electrolyte was immersed in the electrolyte as shown as the second electrode.
  • a voltage potential was placed across the first and second electrode to initiate dissociation of the CeO2 and reduction of the cerium.
  • FIG. 4 illustrates the change in electric potential of the cell with
  • FIG. 5 illustrates the change in cell current and charge of the cell with time with a lithium chloride electrolyte
  • FIG. 6 illustrates the oxygen level determined at the oxygen meter (see FIG. 3) with time utilizing a lithium chloride electrolyte. As can be seen, there was a large increase in the current near 4.5 hours (FIG.

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  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

L'invention concerne une cellule électrochimique et des procédés d'utilisation de la cellule électrochimique, qui peuvent être utilisés pour la récupération de métaux à partir d'oxydes métalliques. La cellule comprend une première électrode qui comprend un oxyde métallique solide, un électrolyte comprenant un conducteur d'ions oxygène et une seconde électrode séparée de l'électrolyte par une membrane conductrice d'ions oxygène. Lors de la réduction de l'oxyde métallique, il se forme du métal solide qui remplace l'oxyde métallique de l'électrode et permet la récupération simplifiée du métal à partir de l'oxyde métallique. La membrane protège la seconde électrode de la corrosion et de la dégradation due à l'électrolyte, ce qui augmente la durée de vie de la cellule.
PCT/US2014/049455 2014-08-01 2014-08-01 Cellule électrochimique de récupération de métaux à partir d'oxydes métalliques solides WO2016018433A1 (fr)

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US14/449,783 US20160032473A1 (en) 2014-08-01 2014-08-01 Electrochemical cell for recovery of metals from solid metal oxides

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RU2756775C2 (ru) * 2019-12-26 2021-10-05 Федеральное государственное автономное образовательное учреждение высшего образования "Уральский федеральный университет имени первого Президента России Б.Н. Ельцина" Способ и электрохимическая ячейка для синтеза электролита для получения рения

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