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WO2016025793A1 - Production de poudre de fer par électrolyse en écoulement - Google Patents

Production de poudre de fer par électrolyse en écoulement Download PDF

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Publication number
WO2016025793A1
WO2016025793A1 PCT/US2015/045204 US2015045204W WO2016025793A1 WO 2016025793 A1 WO2016025793 A1 WO 2016025793A1 US 2015045204 W US2015045204 W US 2015045204W WO 2016025793 A1 WO2016025793 A1 WO 2016025793A1
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WIPO (PCT)
Prior art keywords
substance
reactant
fluidic substance
fluidic
medium
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PCT/US2015/045204
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English (en)
Inventor
Yan Wang
Qiang Wang
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Worcester Polytechnic Institute
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Worcester Polytechnic Institute
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Publication of WO2016025793A1 publication Critical patent/WO2016025793A1/fr
Anticipated expiration legal-status Critical
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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
    • C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
    • C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
    • C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts 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
    • 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

Definitions

  • Iron is the most widely used metal, and currently nearly all crude Fe is produced by reducing Fe ores with coke in a blast furnace at a temperature of 2000 degrees Celsius. This carbothermic reduction process directly produces liquid metal, however it generates two metric tons of CO 2 per metric ton of crude Fe produced.
  • GFG greenhouse gas
  • conventional approaches suffer from the shortcoming that the carbothermic approach generates large quantities of carbon dioxide and other so-called "greenhouse gases” that are environmentally detrimental.
  • configurations herein substantially overcome the above described shortcomings by providing a low temperature electrolysis (LTE) approach that generates iron powder from an electrochemical reaction in a fluidic substance, and avoids the high temperature reaction and resulting volume of carbon dioxide.
  • LTE low temperature electrolysis
  • the solubility of reactant and liquid-to-surface mass-transfer control can be the main limitation for productivity.
  • one way is Fe203 particles suspend in alkaline solution and Fe203 particles also need to diffuse to the electrode surface for the electrochemical reaction to occur, which lowers the reaction rate.
  • the diffusion of solid Fe203 particles to the electrode surface can be the limiting step, and the point, or single, electrode area limits the reaction rate.
  • Fe is deposited on the electrode surface, and therefore the electrode must be removed in order to collect Fe, which could interrupt the production process.
  • the other way is Fe203 particles are pressed to a pellet under very high pressure. The pellet is treated as cathode in alkaline electrolyte. Due to the very poor electronic conductivity of Fe203, the reaction rate is also very slow.
  • configurations herein introduce a process where the electrons and ions can percolate into the liquid mixture, referred to as a colloid, and this mixture contains the iron oxide or other target substance that can be extracted easily from the electrolysis, which significantly increases the reaction rate and allow the production
  • the fluidic substance defining a conductive Fe203 colloidal electrode flows into an electrochemical cell, for continuous electrolysis, from an input reservoir. Fe is collected in an extraction reservoir, which facilitates the collection of the reduced Fe.
  • An electronic-ionic conductive colloidal electrode which contains the electrochemically active species (Fe203 particles), the liquid electrolyte (NaOH solution), SDBS and a percolating electronic conductor (carbon network) is utilized to overcome the diffusion limitation of Fe203 electrolysis associated with 2- dimensional reaction area and the poor electronic conductivity of Fe203.
  • a formed 3-dimensional network with mixed conductivity significantly increases the reaction area and electrolysis current. Fe203 particles then do not need to diffuse to the electrode surface for the effective electrochemical reaction to occur and percolated carbon network increases electronic conductivity effectively.
  • the method for low temperature electrolysis includes circulating a fluidic substance between opposed electrodes, in which the fluidic substance is defined by a colloid including a reactant, an electrolyte, and a disbursement medium, the colloid responsive to an electric charge for producing a target reaction.
  • a flow pump or other flow process agitates the fluidic substance for disposing the fluidic substance between the opposed electrodes, and an electrical source applies an electric charge to the opposed electrodes for electrolytically causing the target reaction.
  • Outflow from the pumped fluidic substance is directed to a reservoir for receiving the circulated fluidic substance, which now includes a precipitate or result of the target reaction for separating a desired substance from the fluidic substance.
  • Fig. la shows the dispersement medium in the fluidic substance including the reactant
  • Fig. lb shows a graphing of an increase in electrical charge resulting from the dispersement medium of Fig. la;
  • Fig. 2 shows a flow electrolysis design for agitating the fluidic substance between the opposed electrodes for facilitating electrolysis using the dispersement medium of Fig. lb; and Figs. 3a-3c show promoting or shifting the electrochemical reaction rate away from undesired substances such as hydrogen gas.
  • the fluidic substance defining the colloid circulates through a flow vessel or other containment for agitating the fluidic substance in
  • the fluidic substance flows between a source and collection reservoir.
  • the source reservoir contains a mixture defining the colloid including the iron oxide or other reactant, the electrolyte, typically an alkaline substance, and the dispersement medium for facilitating charge conductivity through the fluidic substance, such as a carbon network resulting from carbon powder.
  • the colloid mixture including the disbursement medium (carbon) therefore defines a colloid electrode because the liquid substance itself conducts the electrical charge to the Fe203 particles.
  • the fluidic substance flows to the collection reservoir where iron particles (Fe) or other result of the electrolysis are gathered and extracted by a magnetic, filtration or other separation approach.
  • Fig. la shows the dispersement medium in the fluidic substance including the Fe203 reactant.
  • a dispersement medium 110 such as carbon powder percolates throughout the fluidic substance 100 to form a carbon network 112.
  • An electron flow 114 from an electrode 116 transports electrons to a reactant 120 such as iron oxide (Fe203).
  • a resulting electrolysis electrochemical reaction
  • iron particles (Fe) as the desired substance 130, which is then physically extracted or filtered out as the fluidic substance 100 is pumped into a containment reservoir.
  • the electrolysis reaction is given by:
  • Aiiode 60 H ⁇ ⁇ 0 2 (g) + 3H 2 0 + 6e ⁇
  • Fig. lb shows a graphing of an increase in electrical charge resulting from the dispersement medium of Fig. la.
  • the electrode 116 provides voltage resulting in a current to an opposed electrode through the fluidic substance 100.
  • electrical flow is limited as current encounters resistance, as shown by line 140.
  • current flow is facilitated as electrons may pass between particles of the particles (i.e. carbon atoms) of the dispersement medium 110, as shown by line 142.
  • the disclosed colloids may include gels, sols, and emulsions, such that the particles do not settle and are difficult to separate out by ordinary filtering or centrifuging as in a suspension.
  • the fluidic substance 100 is defined by a colloid mixture defining a colloidal electrode, which contains the electrochemically active species (Fe203 particles), the liquid electrolyte (NaOH solution), and a 3D percolating electrical conductor (C network).
  • the simultaneous percolation of electrons and ions effectively increases the area of the current collector, and enables the process to function at high currents rates such as those in Fig. lb.
  • the iron oxide defines a reactant responsive to electrolysis for generating iron particles and oxygen as a by-product, rather than CO 2 as in conventional approaches.
  • Alternate configurations may employ other reactants, in which the reactant is form of the desired substance in a molecular form responsive to the electric charge to result in a desired substance as a result of the target reaction.
  • a fluidic substance 100 including the reactant generates the desired substance from electrolysis of the reactant resulting in an alternate molecular form of the reactant, such as the disclosed Fe203 to Fe as in the reaction above.
  • the reactant may also benefit from the approach herein in addition to iron oxide.
  • the reactant may include forms of other metals such as Fe, Ag, Ni, Cu, and rare earth elements for extraction as the desired substance.
  • Fig. 2 shows a flow electrolysis design for agitating the fluidic substance 100 between the opposed electrodes for facilitating electrolysis using the dispersement medium of Fig. lb.
  • a flow vessel 150 may include an electrochemical cell fluidically coupled between a colloid reservoir 152, or source, and an output reservoir 154.
  • a pump 156 drives and agitates the fluidic substance 100 from the reservoir 152 through the flow vessel 150 where the fluidic substance 150 is in communication with opposed electrodes, including a titanium plate cathode 160 and a platinum foil anode 162 connected to a voltage source 164 such as a potentiostat.
  • the electrodes are not limited to titanium and platinum.
  • a series of parallel opposed plates 160-N and 162-N define the electrodes and enhance the surface area of the electrodes for transfer of electrons to the fluidic substance 100, and the resulting iron particles contained in an outflow liquid 100' in the output reservoir 154.
  • the pump 156 operation and a resulting flow rate of the fluidic substance 100 across the electrodes may be altered to conform to a desired reaction rate in the flow vessel.
  • the reaction rate may depend on such factors as the electrical plate size, the fluid vessel size, the capacity of the pump, and other factors which affect the speed with which electrolysis occurs in the flow vessel.
  • Flow may be altered according to static and continuous modes, and circulating the fluidic substance based on intervals of static containment of the fluidic substance and resuming a fluidic flow of the fluidic substance across the opposed electrodes following the interval.
  • a continuous mode may also be employed for circulating the fluidic substance in a continuous flow across the electrodes and collecting the continuous flow in a reservoir for extracting the desired substance.
  • the dispersement medium 110 percolates throughout the fluidic substance
  • the dispersement medium 110 defines a percolating electrical conductor dispersed in the fluidic substance 100 and conducive to conducting electrical charges throughout the fluidic substance 100 for providing electrons to the target reaction.
  • the pump 156 draws the fluidic substance from the colloid reservoir 152 to propel the fluidic substance 110 through the flow vessel 150 for agitating the fluidic substance 100 to disposing the fluidic substance between the opposed electrodes. Movement of the fluidic substance, in combination with the dispersement medium, allows electrical communication between the reactant particles as electrons flow to the reactant for generating the desired substance through electrolysis. In this manner, the flow vessel 150 circulates the fluidic substance between the opposed electrodes 160, 162, such that the fluidic substance 100 is defined by a colloid including a reactant, an electrolyte, and a disbursement medium, in which the colloid includes the reactant responsive to an electric charge for producing a target reaction.
  • the reactant flowing through the flow vessel 150 generates an electrolytic reaction from a colloidal electrode, in which the colloidal electrode is defined by the combination of the dispersement medium 110 and the reactant for transporting electrons to reactant molecules distant from a charge surface, and the electrolytic reaction results in the desired substance through electrolysis of the reactant, Fe203 in the example shown. While the disclosed examples exhibit an example reactant as iron oxide (Fe203) and the dispersement medium as carbon for resulting in iron particles (Fe) as the desired substance, other reactants responsive to electrolysis may also be employed in the colloidal electrode.
  • the opposed electrodes include a colloid electrode 160 defined by a titanium plate, and a counter electrode 162 defined by a platinum foil
  • the flow vessel 150 employs a plurality of titanium plates 160-N and opposed planar platinum foil 162-N electrodes arranged in a series of parallel planes, typically opposed pairs, in the flow vessel 150 for transporting the fluidic substance 100 between the opposed electrodes for collection in the reservoir 154.
  • the disclosed fluid substance 100 depicts a colloidal electrode that possesses both electrically and ionically conductive properties, hematite particles don't need to diffuse from bulk solution to the surface of the electrode for electrolyzing, and the conversion rate from Fe203 to Fe is not limited by the residence time of the particle adsorbing on electrode surface.
  • the carbon network can conduct the electrons, which forms a 3D reaction network, significantly increasing reaction area and reaction rate.
  • the disclosed approach demonstrates the use of electrolysis in a colloidal electrode for LTE to avoid generation of greenhouse gases resulting from high temperature reactions.
  • a further consideration includes ensuring that the electrochemical reaction does not generate undesirable by-products, such as hydrogen gas.
  • Figs. 3a-3c show promoting or shifting the electrochemical reaction (rate) potential away from undesired substances such as hydrogen gas. Selection of a particular electrolyte provides an alkaline substance that shifts the reaction to avoid generation of undesirable or harmful precipitants.
  • the potential 170 at which iron electrolysis occurs is very close to the potential at which hydrogen is produced (2H + -> Fh), and the current peak of reducing Fe 2+ to Fe is merged with the current of H2 evolution.
  • the colloid therefore benefits by defining the fluid substance 100 based on selecting the electrolyte based on an electrochemical reaction rate for shifting electrolysis towards reactions resulting in the generation of the desired substance and away from reactions resulting in hydrogen gas (Fb).
  • the electrolyte may be an alkaline substance selected from the group consisting of sodium hydroxide (NaOH) and sodium sulfide (Na 2 S).
  • the dispersement medium demonstrates how carbon affects the electronic conductivity and viscosity of the colloidal electrodes under static condition. Alternate configurations systematically determine the electronic conductivity, viscosity and stability of the colloidal electrodes, by changing the content of the disbursement medium and electrolyte before and after flow. It is desirable to have a high concentration of carbon, to increase electronic conductivity, and a high concentration of Fe203 to get a high current density, although at a certain point the colloidal electrodes may become excessively viscous and unusable in flow electrolysis. The electronic conductivity and viscosity will be measured with different compositions of the colloidal electrodes.
  • Correlations may then link the viscosity with the electronic conductivity to determine the effects of the rheology on the conductivity. For example, it may be revealed that colloidal electrodes with the same amount of C and different viscosity possibly possess different electronic conductivity and electrolysis currents.

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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)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

Selon la présente invention, le secteur de la sidérurgie se soucie depuis longtemps de l'environnement et des efforts sont continuellement réalisées pour réduire la consommation d'énergie et les émissions de CO2. Cependant le procédé carbothermique a approché ses limites en termes de réduction des émissions de gaz à effet de serre, et on peut s'attendre uniquement à des améliorations marginales. L'électrolyse à basse température utilisant un milieu de dispersion pour distribuer efficacement la charge au sein d'un mélange colloïdal comprenant de l'oxyde de fer constitue un procédé respectueux de l'environnement pour réaliser une réduction électrochimique de Fe2O3 et produire du Fe granulaire. Une électrode colloïdale conductrice de l'électricité ionique contenant l'espèce électrochimiquement active (particules de Fe2O3), l'électrolyte liquide (solution de NaOH), et un conducteur électrique de percolation (réseau de carbone) sont utilisés pour produire Fe. La percolation simultanée d'électrons et des ions qui en résulte accroît efficacement la surface du collecteur de courant, et permet au processus de fonctionner à des intensités et à une vitesse de transfert de charge plus élevées qu'une électrolyse statique.
PCT/US2015/045204 2014-08-15 2015-08-14 Production de poudre de fer par électrolyse en écoulement Ceased WO2016025793A1 (fr)

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US62/037,723 2014-08-15

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Cited By (1)

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CN110565120A (zh) * 2019-10-18 2019-12-13 东北大学 一种在含铜铁液中脱除并回收铜的方法

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* Cited by examiner, † Cited by third party
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WO2023111640A1 (fr) * 2021-12-15 2023-06-22 Arcelormittal Appareil d'électrolyse pour la production de fer avec un dispositif d'alimentation en oxyde de fer amélioré
US20240426015A1 (en) 2023-06-21 2024-12-26 SiTration, Inc. Methods and apparatus for extracting metals from materials
WO2025096918A1 (fr) * 2023-11-01 2025-05-08 Worcester Polytechnic Institute Production de fer à basse température et à faible émission

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Publication number Priority date Publication date Assignee Title
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CN110565120B (zh) * 2019-10-18 2021-09-07 东北大学 一种在含铜铁液中脱除并回收铜的方法

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