WO2002066711A1 - Extraction of metals - Google Patents
Extraction of metals Download PDFInfo
- Publication number
- WO2002066711A1 WO2002066711A1 PCT/AU2002/000168 AU0200168W WO02066711A1 WO 2002066711 A1 WO2002066711 A1 WO 2002066711A1 AU 0200168 W AU0200168 W AU 0200168W WO 02066711 A1 WO02066711 A1 WO 02066711A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cathode
- electrolyte
- method defined
- electrolytic cell
- metalliferous material
- Prior art date
Links
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
-
- 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
-
- 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
- C22B34/1263—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, e.g. by reduction
-
- 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
- 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
- C25C3/26—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium
- C25C3/28—Electrolytic production, recovery or refining of metals by electrolysis of melts of titanium, zirconium, hafnium, tantalum or vanadium of titanium
Definitions
- the present invention relates to methods of producing metals from metalliferous materials such as metal oxides .
- the present invention is concerned with alternative methods of producing metals from metalliferous materials that are based on the use of electrochemical cells .
- the Okabe et al paper discloses an electrochemical method of removing oxygen dissolved in titanium.
- the paper reports experimental work on an electrolytic cell that included a cathode of titanium having up to 1400ppm dissolved oxygen and an anode of graphite.
- the cathode and the anode were immersed in a molten CaCl 2 electrolyte bath. Electrical potentials between 0 and 6V were applied between the anode and the cathode.
- CaCl 2 was employed to produce calcium and to facilitate the calcium reaction by decreasing the activity of the electrolytic by-product CaO.
- the calcium potential in CaCl 2 was increased at the titanium cathode surface as a result of the application of the electrical potential across the anode and the cathode.
- the Okabe et al paper discloses an electrochemical method of removing oxygen dissolved in yttrium.
- the paper describes experimental work on solid yttrium containing dissolved oxygen.
- the yttrium was placed in a titanium basket cathode and thereafter immersed in a bath of molten CaCl 2 electrolyte.
- the CaCl 2 electrolyte bath was contained in a titanium crucible and a constant voltage of between 3.2 to 3.8V was applied between the cathode and a graphite anode submerged in the electrolyte.
- Electrolysis was carried out at 1223K (950°C) for a specified time.
- One application is the direct production of metal from a metal oxide.
- the “discovery” is the realisation that an electrochemical method can be used to ionise oxygen contained in a solid metal so that the oxygen dissolves in an electrolyte", compare page 5, lines 14-16.
- the International application discloses that when a suitably negative potential is applied in an electrochemical cell with an oxygen-containing metal as a cathode, a reaction occurs whereby oxygen is ionised and is subsequently able to dissolve in the electrolyte of the cell.
- the International application discloses an electrolytic cell that includes a body of a metalliferous material (such as a metal oxide in which impurities are dissolved) as a cathode of the cell.
- the cathode is immersed in a molten bath of a suitable electrolyte.
- a predetermined electrical potential that is lower than the decomposition potential of the electrolyte is applied between the cathode and a suitable anode (either a separate graphite anode or the electrolyte crucible) .
- the potential is chosen such that it has a value that allows a selected impurity (i.e. 0, S, C or N) to be ionised and thus diffuse through the body of metalliferous material into the electrolyte where it dissolves.
- the International application lists a substantial number of metals that are said to be susceptible for use in the above-described method. These metals are titanium (Ti) , silicon (Si) , germanium (Ge) , zirconium (Zr) , hafnium (Hf) , samarium (Sm) , uranium (U) , aluminium (Al) , magnesium (Mg) , neodymium (Nd) , molybdenum (Mo) , chromium (Cr) , niobium (Nb) or any alloys thereof.
- Example 12 relates to the creation of a Ti-Al alloy starting from a mixture of Ti0 2 and Al 2 0 3 .
- the ranges of applied voltage in the different examples varied from as low as 1.75V (see example 2) to 3.3V (compare example 3).
- Most experiments were conducted at a controlled voltage of 3.0V.
- Process times varied.
- Crucibles used were made from alumina, graphite, or titanium whereby the anode was either the crucible or a separate graphite rod.
- the only electrolyte used in all of the examples was CaCl 2 .
- Titanium of very low oxygen concentration could be produced directly from titania by electrolysis in molten CaCl 2 .
- cell modification was required to reduce titania in an electrolytic cell, as the Fray et al International application in particular is silent on how to set up an electrolytic cell in order to achieve reduction of a good electrical insulator such as titania. Reduction of titania could not be achieved within required parameters by following the experimental set-up disclosed in the Fray et al International application.
- a first aspect of the invention is based on the realisation that the type of cathode leads in electrical contact with Ti0 2 and CaCl 2 electrolyte severely influence the titania reduction process. While there is only a preliminary understanding of the mechanism, it is likely that proper selection of the material and the type of electrical contact will be an important part of the electrolytic cell design specific to metal oxide to be reduced and the electrolyte employed therefor.
- the first aspect of the invention is a method of producing a metal or an alloy from metalliferous material by removing an impurity (I) selected from the group including O, S, or N from a solid body of metalliferous material by electrolysis in an electrolytic cell that includes molten halide salt or mixture of halide salts as an electrolyte, wherein the cation of said salt is selected from the group that includes Ca, Ba, Li, Na, K, Mg, Sr, Cs and Y, which method includes conducting the electrolysis under conditions wherein:
- the potential applied between an anode and a cathode of the electrolytic cell is chosen such that permanent decomposition of the electrolyte is avoided to an extent that substantial deposition of the electrolyte cation at the cathode is avoided;
- the body is made part of the cathode of the electrolytic cell, the cathode includes a conductor for electrically connecting the cathode with an electrical potential, the conductor has high resistance to chemical attack by the electrolyte at high temperatures, and the conductor is at least partly immersed in the electrolyte;
- the metalliferous material may contain an oxide, sulfide, carbide or nitride of said metal.
- the metalliferous material is a titanium-containing material.
- the impurity is oxygen.
- the titanium-containing material is titania.
- the anode is formed from graphite.
- the electrolyte is CaCl 2 .
- a method of producing a metal or an alloy from metalliferous material by removing an impurity (I) selected from the group including O, S, or N from a solid body of metalliferous material by electrolysis in an electrolytic cell that includes molten halide salt or mixture of halide salts as an electrolyte, wherein the cation of said salt is selected from the group that includes Ca, Ba, Li, Na, K, Mg, Sr, Cs and Y, which method includes conducting the electrolysis under conditions wherein:
- the potential applied between an anode and a cathode of the electrolytic cell is chosen such that permanent decomposition of the electrolyte is avoided to an extent that substantial deposition of the electrolyte cation at the cathode is avoided and anode material transport towards and into the cathode is substantially prevented;
- the body is made part of the cathode of the electrolytic cell
- the cathode includes a conductor having high resistance to chemical attack by the electrolyte at high temperatures for connecting the cathode with an electrical potential and the conductor is at least partly immersed in the electrolyte.
- the metalliferous material may contain an oxide, sulfide, carbide or nitride of said metal.
- the metalliferous material is a titanium-containing material.
- the impurity is oxygen.
- the titanium-containing material is titania.
- the anode is formed from graphite.
- the electrolyte is CaCl 2 .
- a cathode for use in the above described methods, wherein the cathode includes the body of metalliferous material distributed around one or more electrical conductors that are substantially inert in the electrolyte at high temperatures and which provide a plurality of reduction zones at the cathode.
- the purpose of the first experiment was to confirm (or otherwise) the feasibility of producing metallic titanium from titania by direct electrochemical reduction in molten CaCl 2 .
- the purpose of the first experiment was to confirm (or otherwise) the set-up described in the Fray et al International application. Accordingly, the conditions of the experiment were kept as close as possible to the conditions in the examples of the International application.
- the underlying principle of the process is based on ionisation of oxygen in an oxide as a result of applying suitable negative potential to it in electrochemical cell and subsequent dissolution in the electrolyte.
- the electrochemical cell included a graphite crucible equipped with a graphite lid.
- the crucible was used as the cell anode.
- a stainless steel rod was used to secure electrical contact between a d/c power supply and the crucible.
- the cell cathode consisted of Kanthal or platinum wire connected at one end to the power supply and Ti0 2 pellets suspended from the other end of the wire.
- An alumina tube was used as an insulator around the cathode.
- thermocouple contained in an alumina sheath, was immersed in the electrolyte in close proximity to the pellets.
- pellets Two types were used. One type was slip-cast and the other type was pressed. Both types of pellets were made from analytical grade Ti0 2 powder. Both types of pellets were sintered in air at 850°C. One pressed and one slip-cast pellet were used in the experiment .
- the experiment was conducted at 950°C. Voltages up to 3V were applied between the crucible wall and the Kanthal or platinum wire.
- the power-supply maintained a constant voltage throughout the experiment.
- the voltage and resulting cell current were logged using LabVIEW (TM) data acquisition software.
- the constant voltage (3V) used in the experiment produced an initial current of approximately 1.2A. A continuous drop in the current was observed during the initial 2 hours . After that a gradual increase in the current up to 1A was observed.
- the experimental set-up was essentially the same as in the case of titanium.
- the cathode consisted of platinum-rhodium wire and Si0 2 pellets suspended from the end of the wire.
- the voltage used in the experiment was 3V, which produced initial current of approximately 1.5A as shown in Figure 8. After that a gradual decrease in the current to 0.65A was observed.
- the working potential was selected as 3V in order to overcome resistance and overvoltage. However, chlorine liberation was observed at 3V although it is below the theoretical decomposition potential of CaCl 2 , which is 3.25V at 950°C.
- the experiment was terminated after 4 hours .
- the partially reduced pellets were isolated by dissolution of the CaCl 2 in water.
- the surface and interior of the samples were analysed by SEM.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
Claims
Priority Applications (12)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2002231464A AU2002231464B2 (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
KR10-2003-7010796A KR20030083716A (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
MXPA03007326A MXPA03007326A (en) | 2001-02-16 | 2002-02-18 | Extraction of metals. |
US10/468,215 US20040084323A1 (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
BR0207313-7A BR0207313A (en) | 2001-02-16 | 2002-02-18 | Process for producing a metal or an alloy from metal material and cathode for process use |
CA002438523A CA2438523A1 (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
EP02711649A EP1368513A4 (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
APAP/P/2003/002845A AP1528A (en) | 2001-02-16 | 2002-02-18 | Extraction of minerals |
EA200300899A EA200300899A1 (en) | 2001-02-16 | 2002-02-18 | EXTRACTION OF METALS |
JP2002566009A JP2004529266A (en) | 2001-02-16 | 2002-02-18 | Metal extraction |
NO20033627A NO20033627L (en) | 2001-02-16 | 2003-08-15 | Extraction of metals |
HK04109235A HK1066248A1 (en) | 2001-02-16 | 2004-11-23 | Extraction of metals |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AUPR3172 | 2001-02-16 | ||
AUPR3172A AUPR317201A0 (en) | 2001-02-16 | 2001-02-16 | Extraction of Metals |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2002066711A1 true WO2002066711A1 (en) | 2002-08-29 |
Family
ID=3827191
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/AU2002/000168 WO2002066711A1 (en) | 2001-02-16 | 2002-02-18 | Extraction of metals |
Country Status (15)
Country | Link |
---|---|
US (1) | US20040084323A1 (en) |
EP (1) | EP1368513A4 (en) |
JP (1) | JP2004529266A (en) |
KR (1) | KR20030083716A (en) |
CN (1) | CN1285771C (en) |
AP (1) | AP1528A (en) |
AU (1) | AUPR317201A0 (en) |
BR (1) | BR0207313A (en) |
CA (1) | CA2438523A1 (en) |
EA (1) | EA200300899A1 (en) |
HK (1) | HK1066248A1 (en) |
MX (1) | MXPA03007326A (en) |
NO (1) | NO20033627L (en) |
WO (1) | WO2002066711A1 (en) |
ZA (1) | ZA200306394B (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004029309A1 (en) * | 2002-09-27 | 2004-04-08 | Qinetiq Limited | Improved process for removing oxygen from metal oxides by electrolysis in a fused salt |
WO2006010228A1 (en) * | 2004-07-30 | 2006-02-02 | Bhp Billiton Innovation Pty Ltd | Electrochemical reduction of metal oxides |
US7410562B2 (en) | 2003-08-20 | 2008-08-12 | Materials & Electrochemical Research Corp. | Thermal and electrochemical process for metal production |
AU2002349139B2 (en) * | 2001-12-01 | 2008-11-20 | Cambridge Enterprise Limited | Electrochemical processing of solid materials in fused salt |
US7794580B2 (en) | 2004-04-21 | 2010-09-14 | Materials & Electrochemical Research Corp. | Thermal and electrochemical process for metal production |
WO2012104640A2 (en) | 2011-02-04 | 2012-08-09 | Metalysis Limited | Electrolysis method, apparatus and product |
US9150943B2 (en) | 2007-01-22 | 2015-10-06 | Materials & Electrochemical Research Corp. | Metallothermic reduction of in-situ generated titanium chloride |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7086977B2 (en) * | 2001-05-03 | 2006-08-08 | Ford Global Technologies, Llc | Transmission arrangements for hybrid electric vehicles |
US7410610B2 (en) * | 2002-06-14 | 2008-08-12 | General Electric Company | Method for producing a titanium metallic composition having titanium boride particles dispersed therein |
US7416697B2 (en) | 2002-06-14 | 2008-08-26 | General Electric Company | Method for preparing a metallic article having an other additive constituent, without any melting |
US7531021B2 (en) | 2004-11-12 | 2009-05-12 | General Electric Company | Article having a dispersion of ultrafine titanium boride particles in a titanium-base matrix |
EP1982006A2 (en) * | 2006-02-06 | 2008-10-22 | E.I. Du Pont De Nemours And Company | Method for electrolytic production of titanium and other metal powders |
CN101597776B (en) * | 2009-07-07 | 2012-04-25 | 武汉大学 | Metallurgy method of metal sulfide M1S |
KR200457804Y1 (en) * | 2009-10-15 | 2012-01-03 | 이상수 | the hydraulic pressure type wood clamps structure |
GB201223375D0 (en) * | 2012-12-24 | 2013-02-06 | Metalysis Ltd | Method and apparatus for producing metal by electrolytic reduction |
JP6495142B2 (en) * | 2015-08-28 | 2019-04-03 | 株式会社神戸製鋼所 | Method for producing titanium metal |
CN109280941B (en) * | 2018-11-16 | 2020-02-28 | 北京科技大学 | Method for preparing metallic titanium by titanic iron composite ore, carbon sulfurization and electrolysis |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999064638A1 (en) * | 1998-06-05 | 1999-12-16 | Cambridge University Technical Services Limited | Removal of oxygen from metal oxides and solid solutions by electrolysis in a fused salt |
GB2359564A (en) * | 2000-02-22 | 2001-08-29 | Secr Defence | Electrolytic reduction of metal oxides |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5837122A (en) * | 1997-04-21 | 1998-11-17 | The Scientific Ecology Group, Inc. | Electrowinning electrode, cell and process |
GB0027929D0 (en) * | 2000-11-15 | 2001-01-03 | Univ Cambridge Tech | Metal and alloy powders |
-
2001
- 2001-02-16 AU AUPR3172A patent/AUPR317201A0/en not_active Abandoned
-
2002
- 2002-02-18 CN CNB028073037A patent/CN1285771C/en not_active Expired - Fee Related
- 2002-02-18 EA EA200300899A patent/EA200300899A1/en unknown
- 2002-02-18 JP JP2002566009A patent/JP2004529266A/en active Pending
- 2002-02-18 BR BR0207313-7A patent/BR0207313A/en not_active IP Right Cessation
- 2002-02-18 AP APAP/P/2003/002845A patent/AP1528A/en active
- 2002-02-18 MX MXPA03007326A patent/MXPA03007326A/en not_active Application Discontinuation
- 2002-02-18 US US10/468,215 patent/US20040084323A1/en not_active Abandoned
- 2002-02-18 KR KR10-2003-7010796A patent/KR20030083716A/en not_active Application Discontinuation
- 2002-02-18 EP EP02711649A patent/EP1368513A4/en not_active Ceased
- 2002-02-18 WO PCT/AU2002/000168 patent/WO2002066711A1/en active Application Filing
- 2002-02-18 CA CA002438523A patent/CA2438523A1/en not_active Abandoned
-
2003
- 2003-08-15 NO NO20033627A patent/NO20033627L/en not_active Application Discontinuation
- 2003-08-18 ZA ZA200306394A patent/ZA200306394B/en unknown
-
2004
- 2004-11-23 HK HK04109235A patent/HK1066248A1/en not_active IP Right Cessation
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999064638A1 (en) * | 1998-06-05 | 1999-12-16 | Cambridge University Technical Services Limited | Removal of oxygen from metal oxides and solid solutions by electrolysis in a fused salt |
GB2359564A (en) * | 2000-02-22 | 2001-08-29 | Secr Defence | Electrolytic reduction of metal oxides |
Non-Patent Citations (1)
Title |
---|
See also references of EP1368513A4 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU2002349139B2 (en) * | 2001-12-01 | 2008-11-20 | Cambridge Enterprise Limited | Electrochemical processing of solid materials in fused salt |
WO2004029309A1 (en) * | 2002-09-27 | 2004-04-08 | Qinetiq Limited | Improved process for removing oxygen from metal oxides by electrolysis in a fused salt |
US7410562B2 (en) | 2003-08-20 | 2008-08-12 | Materials & Electrochemical Research Corp. | Thermal and electrochemical process for metal production |
EP2322693A1 (en) | 2003-08-20 | 2011-05-18 | Materials And Electrochemical Research Corporation | Electrochemical process for titanium production |
US7985326B2 (en) | 2003-08-20 | 2011-07-26 | Materials And Electrochemical Research Corp. | Thermal and electrochemical process for metal production |
US7794580B2 (en) | 2004-04-21 | 2010-09-14 | Materials & Electrochemical Research Corp. | Thermal and electrochemical process for metal production |
WO2006010228A1 (en) * | 2004-07-30 | 2006-02-02 | Bhp Billiton Innovation Pty Ltd | Electrochemical reduction of metal oxides |
US9150943B2 (en) | 2007-01-22 | 2015-10-06 | Materials & Electrochemical Research Corp. | Metallothermic reduction of in-situ generated titanium chloride |
WO2012104640A2 (en) | 2011-02-04 | 2012-08-09 | Metalysis Limited | Electrolysis method, apparatus and product |
Also Published As
Publication number | Publication date |
---|---|
AP1528A (en) | 2006-01-03 |
NO20033627L (en) | 2003-10-03 |
AUPR317201A0 (en) | 2001-03-15 |
HK1066248A1 (en) | 2005-03-18 |
NO20033627D0 (en) | 2003-08-15 |
CN1500156A (en) | 2004-05-26 |
US20040084323A1 (en) | 2004-05-06 |
BR0207313A (en) | 2004-02-10 |
EA200300899A1 (en) | 2004-02-26 |
CN1285771C (en) | 2006-11-22 |
JP2004529266A (en) | 2004-09-24 |
CA2438523A1 (en) | 2002-08-29 |
EP1368513A1 (en) | 2003-12-10 |
ZA200306394B (en) | 2004-09-13 |
AP2003002845A0 (en) | 2003-09-30 |
KR20030083716A (en) | 2003-10-30 |
EP1368513A4 (en) | 2006-06-28 |
MXPA03007326A (en) | 2005-02-14 |
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