WO2006092615A1 - Procédé et dispositif électrochimiques pour l’élimination de l’oxygène d’un composé ou d’un métal - Google Patents

Procédé et dispositif électrochimiques pour l’élimination de l’oxygène d’un composé ou d’un métal Download PDF

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Publication number
WO2006092615A1
WO2006092615A1 PCT/GB2006/000765 GB2006000765W WO2006092615A1 WO 2006092615 A1 WO2006092615 A1 WO 2006092615A1 GB 2006000765 W GB2006000765 W GB 2006000765W WO 2006092615 A1 WO2006092615 A1 WO 2006092615A1
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WO
WIPO (PCT)
Prior art keywords
metal
melt
anode
compound
cathode
Prior art date
Application number
PCT/GB2006/000765
Other languages
English (en)
Inventor
Derek John Fray
Carsten Schwandt
Original Assignee
Cambridge Enterprise Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cambridge Enterprise Limited filed Critical Cambridge Enterprise Limited
Priority to EP06709988A priority Critical patent/EP1866448A1/fr
Priority to JP2007557592A priority patent/JP2008531854A/ja
Priority to AU2006219725A priority patent/AU2006219725A1/en
Priority to EA200701896A priority patent/EA200701896A1/ru
Priority to US11/817,458 priority patent/US20080302655A1/en
Publication of WO2006092615A1 publication Critical patent/WO2006092615A1/fr

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/129—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds by dissociation, e.g. thermic dissociation of titanium tetraiodide, or by electrolysis or with the use of an electric arc
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B15/00—Other processes for the manufacture of iron from iron compounds
    • 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
    • C22B5/00—General methods of reducing to metals
    • 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
    • Y02P10/10—Reduction of greenhouse gas [GHG] emissions
    • Y02P10/134—Reduction of greenhouse gas [GHG] emissions by avoiding CO2, e.g. using hydrogen

Definitions

  • the invention relates to a method and an apparatus for removing oxygen from a compound, comprising a metal and oxygen, or from a metal or alloy, by an electrolytic process.
  • a cathode comprising or contacting the solid compound is immersed in or contacted with a fused salt and a voltage is applied between the cathode and an anode, which also contacts the salt, such that the substance dissolves in the salt.
  • This process may be used, for example, to extract the metal from the solid metal compound.
  • a cathode comprising or contacting a mixture of solid metal compounds, or of one or more compounds and one or more metals, may also be processed to form an alloy or an intermetallic compound.
  • electro-decomposition This process is termed electro-decomposition in this document but is also known by other terms including electro-deoxidation or electro-reduction.
  • the fused salt acts as an electrolyte in the electro-decomposition process.
  • the term fused salt may be used interchangeably with other terms commonly used in the art, such as electrolyte, molten salt and melt.
  • the invention provides a method and an apparatus for removing oxygen from a compound comprising a metal and oxygen, or from a metal or alloy, and an anode for an electro-decomposition process, as defined in the appended independent claims to which reference should now be made. Preferred or advantageous features of the invention are defined in dependent sub-claims.
  • the invention may advantageously provide a method of removing oxygen from a compound comprising a metal and oxygen which comprises the steps of arranging a cathode comprising or contacting the compound in contact with a melt comprising a hydroxide of an alkali metal.
  • An anode is also arranged in contact with the melt and a potential is applied between the anode and the cathode sufficient to remove oxygen from the solid compound.
  • the compound may be an intermetallic compound.
  • the cathode comprises or contacts a metal or alloy containing dissolved oxygen, and the applied potential is sufficient to remove oxygen from the metal or alloy.
  • the compound, metal or alloy is preferably solid.
  • the melt further comprises an oxide of the alkali metal and this oxide is particularly preferably soluble in the hydroxide.
  • a melt comprising an alkali metal oxide, which is dissolved in an alkali metal hydroxide, is a melt system that may advantageously support oxygen ion conductivity. Good oxygen ion conductivity may be advantageous in efficiently transferring oxygen from the solid compound at the cathode through the melt to be discharged at the anode.
  • the potential at the cathode during electro-decomposition is lower (in magnitude) than a potential for continuous evolution of hydrogen or continuous deposition of the alkali metal from the melt.
  • the potential (applied voltage) between the cathode and the anode is lower than a potential for continuous decomposition of the melt.
  • the alkali metal hydroxide may be any alkali metal hydroxide, s preferably it is sodium hydroxide and the alkali metal is sodium, or the hydroxide is potassium hydroxide and the alkali metal is potassium.
  • the oxide is then preferably sodium oxide or potassium oxide respectively. Mixtures of hydroxides and/or oxides comprising different cations may be used.
  • the solid compound may be any solid compound comprising a metal and oxygen that is less stable than an oxide of the alkali metal
  • the invention may be particularly advantageous when used to reduce oxides of low stability such as an iron oxide or an oxide of cobalt, nickel, copper, zinc or lead, or when used to remove oxygen from metals or alloys comprising such metals.
  • a precursor material at the cathode comprises a mixture of metal compounds, or a mixture of one or more metal compounds and one or more metals, then an alloy or an intermetallic compound comprising metal species in the precursor material may be produced.
  • the melt may comprise a mixture of hydroxides or oxides of more than one alkali metal, but may additionally contain other anion or cation species. Such species should preferably not, however, be such as to cause corrosion of an inert anode. 5
  • the melting point of sodium hydroxide is about 32O 0 C. This may advantageously allow the electro-decomposition process to be carried out at low temperatures compared to electro-decomposition in a calcium chloride melt. For example the reaction may proceed at temperatures below 65O 0 C or 0 below 500 0 C. The electro-decomposition may particularly advantageously proceed at any temperature at which the electrolyte is molten.
  • the melting point of sodium hydroxide may be decreased with the addition of a small amount of sodium iodide or sodium bromide. This may s allow electro-decomposition to proceed at even lower temperatures and so may reduce the energy needed to maintain the melt at an operating temperature and may reduce problems of corrosion in the electro- decomposition apparatus.
  • the removal of oxygen from the compound(s), metal(s) or alloy(s) at the cathode may involve diffusion. This process is accelerated by increasing temperature and so the rate of reaction may disadvantageously be reduced by operating at low temperature, depending on the materials involved and the geometry of the materials used (such as the particle size of the material at the cathode). Thus, a temperature greater than 500 0 C OR 550°c may advantageously be used.
  • the boiling point of NaOH, for example, is 1390 0 C and so higher temperatures than 500 0 C may in principle be used as long as any resulting reaction rate increase is appropriately balanced against any increase in corrosion of the apparatus at higher temperatures.
  • the anode is substantially inert with respect to the melt under operating conditions.
  • the electro-decomposition is carried out at 65O 0 C using a sodium hydroxide melt in which a small proportion of sodium oxide is dissolved, the anode should be substantially inert to this melt at this temperature.
  • Anodes containing nickel or nickel oxide are believed to be substantially inert in caustic melts such as molten sodium hydroxide.
  • the anode is made from a material that comprises nickel, for example nickel oxide or a nickel alloy or a nickel-rich alloy.
  • An InconelTM may be suitable.
  • a metal which forms an inert oxide layer may be suitable as an inert anode in a hydroxide melt.
  • inert anodes should be construed, as the skilled person would do, to encompass substantially inert anodes.
  • an inert anode should be sufficiently inert in practice to be usable for a suitably extended length of time.
  • a further aspect of the invention may advantageously provide a method of removing oxygen from a solid compound comprising a metal and oxygen which comprises the steps of arranging a cathode comprising or contacting the solid compound in contact with a melt comprising a hydroxide of an alkali metal.
  • An anode is also arranged in contact with the melt and a potential is applied between the anode and the cathode sufficient to remove oxygen from the solid compound, the anode comprising a metal or alloy which forms an inert oxide layer, or comprising nickel, nickel oxide or a nickel alloy.
  • An inert or substantially inert anode may provide a number of advantageous features when compared with carbon anodes as conventionally used in electro- decomposition processes.
  • Gas evolved at the inert anode during electro- decomposition may be substantially pure oxygen.
  • Carbon anodes generally evolve carbon dioxide or carbon monoxide, and these gases may have a deleterious effect on the environment if vented to the atmosphere in the volumes likely to be produced by a commercial industrial plant. Any oxygen produced may be vented to the atmosphere or may be collected as a product of the electro-decomposition process.
  • inert anodes do not react during electro-decomposition, they are not consumed by the process or are consumed at an advantageously slow rate. This may allow for longer running times for a cell implementing the process, simpler cell design and lower overall anode costs.
  • the melt and the product metal may not be contaminated by material from the anode, which may increase the working life of the melt and may reduce the number of postprocessing steps required for the product.
  • the method when operated for a sufficient time, has as its end product the metal; for example if Fe 2 O 3 is the solid compound the product would then be Fe.
  • the electro-decomposition of the solid compound from oxide to pure metal may take place via a number of intermediate compounds. Any of these intermediate compounds may be removed as the product of the process if the process is not run for a sufficient time to allow for complete reduction to the metal.
  • the process is advantageously run under conditions such that alkali metal from the hydroxide does not continuously deposit as a metal at the cathode.
  • the melt may contain more than one species of alkali metal in which case the potential applied between the anode and the cathode is preferably not sufficient for any alkali metal that is present in the melt to deposit continuously as a metal at the cathode. An absence of dissolved alkali metal in the melt is likely to advantageously reduce or substantially eliminate electronic conductivity of the melt.
  • the reaction at the cathode may be monitored by measuring the cathode potential against a reference electrode.
  • a reference electrode such as a Ag/AgCI electrode, or a psuedo-reference electrode calibrated by a method such as cyclic voltammetry, or a dynamic reference electrode such as an electrode comprising a metal that is the same as an alkali metal species in the melt.
  • a cell for operating a process according to a particularly-preferred embodiment of the invention would have a melt of sodium hydroxide, containing some sodium oxide, and an anode comprising nickel.
  • iron oxide may be electro-decomposed in a melt comprising sodium oxide dissolved in sodium hydroxide.
  • reaction equations and standard electrochemical potentials demonstrate the suitability of the approach disclosed.
  • the stability of the electrolyte is believed to be determined by the following 0 reaction equations and standard electrochemical potentials. The numbers refer to 600 0 C and unit activities.
  • the sodium oxide is diluted by the sodium hydroxide and so its actual decomposition potential is lower (more negative) than the one 0 calculated for standard conditions.
  • the decomposition potential of sodium oxide becomes more negative by 173 mV at 600°C for each order of magnitude the concentration falls below saturation concentration.
  • Concerning the sodium hydroxide the most favourable decomposition reaction leads to the generation of hydrogen gas (reaction 9), while decomposition reactions involving the deposition of sodium metal (reactions 10 and 11 ) 5 require significantly more negative potentials.
  • electro-decomposition of iron oxides in a sodium hydroxide melt should result in the formation of iron, preferably by applying a cell voltage which is sufficient to cause removal of oxygen from iron o oxides (reactions 1 to 6) but which is not sufficient to cause continuous evolution or deposition of hydrogen or sodium at the cathode (reactions 8 and 9). It should be noted that in order to cause such continuous evolution or deposition of hydrogen or sodium, the cell voltage would have to exceed-the voltages corresponding to reactions 8 or 9 by a sufficient margin in order to s overcome voltage losses in the cell.
  • the iron product should not react with the sodium hydroxide as the standard free energies for the following reactions are positive.
  • a method embodying the invention may advantageously be used to 5 remove oxygen from a compound, metal or alloy as long as a compound formed between oxygen and a cation in the melt is more stable than the oxygen or oxide in the compound, metal or alloy.
  • Figure 1 shows a cell for an electro-decomposition process according to an embodiment of the invention.
  • 5 Figure 1 shows a cell 10 for electro-decomposition containing a melt 20 of composition 98% sodium hydroxide and 2% sodium oxide.
  • a cathode 30 in the form of an iron basket 40 containing Fe 2 O 3 particles 50 is immersed in the melt.
  • An anode 60 of commercially pure nickel is also immersed in the melt, the anode and the cathode both being connected to a power supply 70.
  • the melt In operation the melt is heated up to its operating temperature, for example 400 0 C.
  • An operating potential of, for example, 2.5 to 3.0 V is applied between the anode and the cathode.
  • oxygen in the Fe 2 O 3 transfers to the melt and is transported to the anode, where it is evolved as oxygen gas.
  • the melt is heated to an operating temperature of 55O 0 C. All the other reaction conditions are described above.
  • This embodiment reduces the Fe 2 O 3 to Fe at a higher rate than in the first embodiment. It is believed that this is due to increased diffusion rate in the material at the cathode.
  • the cathode comprising a solid metal compound or solid metal
  • it may be advantageous to prepare the compound or metal into a porous form for example by slip-casting (and optionally sintering) the compound or metal in powdered form.
  • the material at the cathode should contain interconnected porosity to allow penetration of the melt, and the particle size should be small enough to allow oxygen diffusion.
  • the material at the cathode may be prepared in any manner and in any geometry, but the reaction rate may be limited by the rate of diffusion of oxygen in the material if disadvantageously thick sections of the material are used.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

La présente invention concerne une cathode qui comprend un composé contenant de l'oxygène, ou un métal contenant de l'oxygène dissous, et qui est mise en contact avec une fonte qui comprend un hydroxyde d'un métal alcalin. Une anode inerte, qui comprend de façon avantageuse du nickel, est également mise en contact avec la fonte et un potentiel est appliqué entre l'anode et la cathode de sorte que l'oxygène est éliminé du composé ou du métal.
PCT/GB2006/000765 2005-03-03 2006-03-03 Procédé et dispositif électrochimiques pour l’élimination de l’oxygène d’un composé ou d’un métal WO2006092615A1 (fr)

Priority Applications (5)

Application Number Priority Date Filing Date Title
EP06709988A EP1866448A1 (fr) 2005-03-03 2006-03-03 Procédé et dispositif électrochimiques pour l élimination de l oxygene d un composé ou d un metal
JP2007557592A JP2008531854A (ja) 2005-03-03 2006-03-03 化合物又は金属から酸素を除去するための方法及び装置
AU2006219725A AU2006219725A1 (en) 2005-03-03 2006-03-03 Electrochemical method and apparatus for removing oxygen from a compound or metal
EA200701896A EA200701896A1 (ru) 2005-03-03 2006-03-03 Способ и аппарат для удаления кислорода из соединения или металла
US11/817,458 US20080302655A1 (en) 2005-03-03 2006-03-03 Electrochemical Method and Apparatus For Removing Oxygen From a Compound or Metal

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GB0504444.1 2005-03-03
GBGB0504444.1A GB0504444D0 (en) 2005-03-03 2005-03-03 Method and apparatus for removing oxygen from a solid compound or metal

Publications (1)

Publication Number Publication Date
WO2006092615A1 true WO2006092615A1 (fr) 2006-09-08

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Country Status (9)

Country Link
US (1) US20080302655A1 (fr)
EP (1) EP1866448A1 (fr)
JP (1) JP2008531854A (fr)
CN (1) CN101163804A (fr)
AU (1) AU2006219725A1 (fr)
EA (1) EA200701896A1 (fr)
GB (2) GB0504444D0 (fr)
WO (1) WO2006092615A1 (fr)
ZA (1) ZA200707266B (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007094681A1 (fr) * 2006-02-17 2007-08-23 Norsk Titanium Metals As Procede et moyen de fabrication de metal dans des masses fondues a base de chlorure
WO2010069685A1 (fr) * 2008-12-18 2010-06-24 Silicon Fire Ag Silicium ou métaux élémentaires comme sources d'énergie
EP2461922A1 (fr) * 2009-08-09 2012-06-13 Rolls-Royce Corporation Résistance à la corrosion pour un procédé de lixivation
JP2013543059A (ja) * 2010-11-18 2013-11-28 メタリシス リミテッド 固体供給原料を電解により還元するための方法及びシステム
DE202009019105U1 (de) 2008-12-18 2016-07-14 Silicon Fire Ag Anlage zum Bereitstellen eines Energieträgers unter Einsatz von Kohlenstoffdioxid als Kohlenstofflieferant und von elektrischer Energie
WO2017081160A1 (fr) 2015-11-10 2017-05-18 Stichting Energieonderzoek Centrum Nederland Fabrication additive d'objets métalliques
US9725815B2 (en) 2010-11-18 2017-08-08 Metalysis Limited Electrolysis apparatus
WO2018208155A1 (fr) 2017-05-10 2018-11-15 Admatec Europe B.V. Fabrication additive d'objets métalliques
WO2020055252A2 (fr) 2018-09-12 2020-03-19 Admatec Europe B.V. Objet tridimensionnel et son procédé de fabrication

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AR076567A1 (es) * 2009-05-12 2011-06-22 Metalysis Ltd Metodo y aparato para reduccion de materia prima solida
US8764962B2 (en) * 2010-08-23 2014-07-01 Massachusetts Institute Of Technology Extraction of liquid elements by electrolysis of oxides
US8900439B2 (en) 2010-12-23 2014-12-02 Ge-Hitachi Nuclear Energy Americas Llc Modular cathode assemblies and methods of using the same for electrochemical reduction
GB201223375D0 (en) * 2012-12-24 2013-02-06 Metalysis Ltd Method and apparatus for producing metal by electrolytic reduction
CN110184626B (zh) * 2018-07-10 2021-06-22 东北大学 潮湿气氛的高温熔盐电解的电化学方法
CN113802149B (zh) * 2021-08-11 2023-06-27 华北理工大学 一种从锌窑渣中提取金属铁的方法

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007094681A1 (fr) * 2006-02-17 2007-08-23 Norsk Titanium Metals As Procede et moyen de fabrication de metal dans des masses fondues a base de chlorure
WO2010069685A1 (fr) * 2008-12-18 2010-06-24 Silicon Fire Ag Silicium ou métaux élémentaires comme sources d'énergie
DE202009019105U1 (de) 2008-12-18 2016-07-14 Silicon Fire Ag Anlage zum Bereitstellen eines Energieträgers unter Einsatz von Kohlenstoffdioxid als Kohlenstofflieferant und von elektrischer Energie
US9631287B2 (en) 2008-12-18 2017-04-25 Silicon Fire Ag Method and facility system for providing an energy carrier by application of carbon dioxide as a carbon supplier of electric energy
EP2461922A1 (fr) * 2009-08-09 2012-06-13 Rolls-Royce Corporation Résistance à la corrosion pour un procédé de lixivation
EP2461922A4 (fr) * 2009-08-09 2014-04-16 Rolls Royce Corp Résistance à la corrosion pour un procédé de lixivation
JP2013543059A (ja) * 2010-11-18 2013-11-28 メタリシス リミテッド 固体供給原料を電解により還元するための方法及びシステム
US9725815B2 (en) 2010-11-18 2017-08-08 Metalysis Limited Electrolysis apparatus
WO2017081160A1 (fr) 2015-11-10 2017-05-18 Stichting Energieonderzoek Centrum Nederland Fabrication additive d'objets métalliques
WO2018208155A1 (fr) 2017-05-10 2018-11-15 Admatec Europe B.V. Fabrication additive d'objets métalliques
US11772157B2 (en) 2017-05-10 2023-10-03 Admatec Europe B.V. Additive manufacturing of metal objects
WO2020055252A2 (fr) 2018-09-12 2020-03-19 Admatec Europe B.V. Objet tridimensionnel et son procédé de fabrication

Also Published As

Publication number Publication date
EA200701896A1 (ru) 2008-02-28
US20080302655A1 (en) 2008-12-11
CN101163804A (zh) 2008-04-16
GB0504444D0 (en) 2005-04-06
JP2008531854A (ja) 2008-08-14
ZA200707266B (en) 2008-09-25
GB0604348D0 (en) 2006-04-12
AU2006219725A1 (en) 2006-09-08
EP1866448A1 (fr) 2007-12-19

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