WO2005123986A1 - Reduction electrochimique d'oxydes metalliques - Google Patents

Reduction electrochimique d'oxydes metalliques Download PDF

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Publication number
WO2005123986A1
WO2005123986A1 PCT/AU2005/000899 AU2005000899W WO2005123986A1 WO 2005123986 A1 WO2005123986 A1 WO 2005123986A1 AU 2005000899 W AU2005000899 W AU 2005000899W WO 2005123986 A1 WO2005123986 A1 WO 2005123986A1
Authority
WO
WIPO (PCT)
Prior art keywords
powders
pellets
metal oxide
feed material
size
Prior art date
Application number
PCT/AU2005/000899
Other languages
English (en)
Inventor
René Ignacio OLIVARES
Ivan Ratchev
Gregory David Rigby
Andrew Arthur Shook
Original Assignee
Bhp Billiton Innovation Pty Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from AU2004903409A external-priority patent/AU2004903409A0/en
Application filed by Bhp Billiton Innovation Pty Ltd filed Critical Bhp Billiton Innovation Pty Ltd
Priority to AU2005254589A priority Critical patent/AU2005254589A1/en
Publication of WO2005123986A1 publication Critical patent/WO2005123986A1/fr
Priority to US11/615,263 priority patent/US20070181438A1/en

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
    • C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
    • C25C5/04—Electrolytic production, recovery or refining of metal powders or porous metal masses from melts
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • 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
    • 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
    • C22B5/02—Dry methods smelting of sulfides or formation of mattes

Definitions

  • the present invention relates to electrochemical reduction of metal oxides .
  • the present invention relates particularly to electrochemical reduction of metal oxides in the form of powders and/or pellets to produce metal having a low oxygen concentration, typically no more than 0.5% by weight.
  • the present invention is a metal oxide feed material for a process and an apparatus for electrochemically reducing metal oxide feed material in powder and/or pellet form on a continuous basis, or a semi-continuous basis or a batch basis .
  • the present invention is also a process for preparing a suitable metal oxide feed material for the process described in the preceding paragraph.
  • the present invention was made during the course of an on-going research project on electrochemical reduction of metal oxides being carried out by the applicant.
  • the research project has focussed on the reduction of titania (Ti0 2 ) .
  • the CaCl 2 -based electrolyte used in the experiments was a commercially available source of CaCl 2 , namely calcium chloride dihydrate, which decomposed on heating and produced a very small amount of CaO.
  • the applicant operated the electrolytic cells at a potential above the decomposition potential of CaO and below the decomposition potential of CaCl 2 .
  • the applicant found that the cells electrochemically reduced titania to titanium with low concentrations of oxygen, ie concentrations less than 0.2 wt . % , at these potentials .
  • the applicant operated the cells under a wide range of different operating set-ups and conditions .
  • One of the inventions made by the applicant in the course of the research project is a process and an apparatus for electrochemically reducing metal oxides, such as titania, on a continuous or a semi-continuous basis .
  • powders and/or pellets is understood to mean particles having a particle size of 3.5 mm or less .
  • the upper end of this particle size range covers particles that are usually described as "pellets”.
  • the remainder of the particle size range covers particles that are usually described as "powders".
  • powders may be single particle powders .
  • Powders may also be made from a plurality of smaller particles . Powders tend to be generally uniform in size, with no immediately apparent length and width dimensions for individual particles. Pellets tend to be shaped, for example by being slip cast in moulds . The shapes can be any suitable shapes .
  • a shape is a disc with a cylindrical side wall and flat top and bottom walls, and with the diameter of the cylinder being considerably greater that the thickness of the disc between the top and bottom walls .
  • a disc that is 20 mm in diameter and 2 mm thick.
  • references to dimensions of powders and/or pellets is understood to mean the minimum dimensions of the powders and pellets .
  • the above-mentioned maximum size of 3.5 mm is the size of the minimum dimension of a powder and/or a pellet.
  • the term "semi-continuously" is understood in the International application and herein to mean that the process includes : (a) periods during which metal oxide powders and/or pellets are supplied to the cell and periods during which there is no such supply of metal oxide powders and/or pellets to the cell, and (b) periods during which reduced material is removed from the cell and periods during which there is no such removal of reduced material from the cell .
  • the term "batch” is understood to mean supplying a batch, ie a selected amount, of metal oxide powders and/or pellets to a cell, operating the process in the cell for a period of time and reducing the powders and/or pellets , and removing the reduced material f om the cell , and repeating the procedure for a next batch of metal oxide powders and/or pellets .
  • the applicant has realised that the physical properties of the metal oxide feed material are extremely important to successful operation of the process on a continuous basis, a semi-continuous basis, and a batch basis .
  • the present invention is a metal oxide feed material in a form of powders and/or pellets that have sufficient porosity, typically 35-60%, to enable penetration of molten electrolyte into the powders and/or pellets during the course of an electrochemical reduction process in which metal oxide is at least partially reduced to metal in an electrolytic cell and subsequent washing of electrolyte from the powders and/or pellets after the powders and/or pellets are discharged from the cell.
  • a metal oxide feed material for electrochemically reducing metal oxides such as titania
  • an apparatus that includes an electrolytic cell that includes a bath of molten electrolyte and an anode and a cathode, which metal oxide feed material is in a form of powders and/or pellets and includes a sufficient porosity to enable penetration of molten electrolyte into the powders and/or pellets during the course of an electrochemical reduction process that reduces metal oxide in the powders and/or pellets to metal and subsequent washing of electrolyte from powders and/or pellets after the powders and/or pellets are discharged from the cell .
  • the metal oxide feed material also includes any one or more than one of :
  • the metal oxide feed material includes powders and/or pellets of a titanium oxide, such as titania
  • the electrolyte is a CaCl 2 - based electrolyte that contains CaO when in a molten state
  • the powders and/or pellets have an open connected pore structure with a porosity in the range of 35-60% by volume.
  • open connected pore structure is understood herein to mean that the powders and/or pellets have a series of interconnected pores that are open to the outer surface of the powders and/or pellets that enable penetration of liquids , such as molten electrolyte and washing water into the powders and/or pellets . It is preferred particularly that the porosity be at least 40 vol . % . It is also preferred particularly that the porosity be less that 55 vol . % .
  • the porosity is in a range of 40-50 vol . % .
  • At least 25 vol . % of the pores have a size of 0.005-10 microns measured by Mercury Intrusion porosimetry.
  • the remainder of the pores have a size of less than 0.005 microns measured by gas absorption.
  • the metal oxide feed material includes powders and/or pellets of a titanium oxide, such as titania
  • the electrolyte is a CaCl 2 -based electrolyte that contains CaO when in a molten state
  • the powders and/or pellets also include any one or more than one of :
  • the powder/pellet size be 1-2.5 mm. It is noted that, in the context of the discussion on page 4, the size of 1-2.5 mm is the size measured in the minimum dimensions of the powders and/or pellets .
  • the powder/pellet size be 1.5-2 mm.
  • a process for preparing a metal oxide feed material for electrochemically reducing metal oxides, such as titania in an apparatus that includes an electrolytic cell that includes a bath of molten electrolyte and an anode and a cathode, which process includes the steps of:
  • step (b) sintering powders and/or pellets from step (a) to a required strength; and (c) washing the sintered powders and/or pellets to remove fines attached to the powders and/or pellets .
  • the process includes a further step of separating the powders and/or pellets formed in step (a) into at least two fractions on the basis of size.
  • the process includes supplying a larger size fraction to step (b) .
  • the process includes returning a smaller size fraction to step (a) .
  • the pore structure of the powders and/or pellets formed in step (a) is an open connected pore structure and the required porosity is 35-60 vol.%.
  • step (a) includes forming powders and/or pellets of metal oxide feed material having a required size and/or a required density.
  • step (a) includes forming powders and/or pellets of metal oxide feed material by agglomerating particles of metal oxide material.
  • the particles of metal oxide material for agglomeration are fully dense particles.
  • the minimum dimensions of the particles of metal oxide material for agglomeration are less than 50 microns .
  • the minimum dimensions of the particles of metal oxide material for agglomeration are less than 30 microns .
  • the minimum dimensions of the particles of metal oxide material for agglomeration range from nanometer size up to 15 microns .
  • step (a) includes forming powders and/or pellets of metal oxide feed material by agglomerating particles of metal oxide material with or without binders .
  • step (a) includes forming powders and/or pellets of metal oxide feed material by agglomerating (i) particles of metal oxide material, (ii) fines washed from the sintered powders and/or pellets in step (c) , and (iii) the smaller size fraction from the separation step, with or without binders.
  • step (a) includes agglomerating particles of metal oxide material in a mixer, such as a pin mixer, that is capable of high impact and high velocity mixing of metal oxide material .
  • a mixer such as a pin mixer
  • step (a) includes agglomerating particles of metal oxide material by supplying particles of metal oxide material and water to the mixer and operating the mixer and forming agglomerates of a required porosity.
  • the required strength for sintered powders and/or pellets in step (b) is a strength that is sufficient to withstand thermal shock associated with introducing powders and/or pellets into the cell .
  • the metal oxide feed material is a titanium oxide, such as titania
  • the required porosity of the powders and/or pellets formed in step (a) is an open pore structure with 35-60 vol.%, more preferably 40-50%, porosity.
  • step (a) preferably the powders and/or pellets formed in step (a) have a size of 1-4 mm and a density of 2.5-3.5 g/cc.
  • step (b) includes sintering the powders and/or pellets formed in step (a) at a temperature in the range of 850-1400°C.
  • step (b) includes sintering the powders and/or pellets formed in step (a) in air.
  • an apparatus that includes an electrolytic cell that includes a bath of molten electrolyte and an anode and a cathode using the above- described metal oxide feed material.
  • a process for electrochemically reducing metal oxides, such as titania in an apparatus that includes an electrolytic cell that includes a bath of molten electrolyte and an anode and a cathode, which process includes the above-described feed preparation process .
  • the present invention is described further by way of example only with reference to the accompanying drawing which is a flowsheet of one embodiment of a process for electrochemically reducing titania in accordance with the present invention that includes one embodiment of a process for preparing titania for use as a feed material in the process in accordance with the present invention.
  • the flowsheet includes the following steps .
  • preferred agglomerates have a density of 2.5-3.5 g/cc in air, a size of 1-4 mm, and an open pore structure with a porosity of 40-50%.
  • the agglomerates may be described as powders or pellets depending on the particle size.
  • agglomerates Drying and sintering the material retained on screen 2 , hereinafter referred to as "agglomerates" at a temperature of 850- 1400°C in air, for example in a multi-hearth furnace, and thereby increasing the mechanical strength of the agglomerates as required.
  • the mechanical strength be sufficient to withstand thermal shock when supplied to a molten electrolyte bath and be handled prior to being supplied to the bath and while in the bath without substantial break-down of the agglomerated powders/pellets .
  • the sintering step does not increase the overall size of the agglomerates .
  • the sintering step increases the size of crystals in the agglomerated powders/pellets , typically to 2-10 microns, subject to the sintering temperature and time, and decreases slightly the porosity of the agglomerates , without affecting the open pore structure.
  • the cell includes a bath of molten electrolyte and an anode and a cathode.
  • the process may be carried out on a continuous basis , a semi-continuous basis , and a batch basis .
  • step (a) of the above- described embodiment includes agglomerating pigment grade titania in a pin mixer
  • the present invention is not so limited and extends to any suitable means of forming powders and/or pellets of titania having a required porosity.
  • shaped pellets may be formed by slip casting.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Electrolytic Production Of Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

L'invention porte sur un matériau de charge d'oxyde métallique destiné à être utilisé dans un processus de réduction électrochimique. Le matériau de charge se présente sous la forme de poudres et/ou de paillettes qui ont une porosité suffisante, généralement comprise entre 35 et 60 %, pour permettre la pénétration de l'électrolyte fondu dans les poudres et/ou les paillettes au cours du processus de réduction électrochimique dans une cellule électrolytique et ensuite l'élimination de l'électrolyte des poudres et/ou des paillettes après l'évacuation de ces dernières de la cellule. L'invention porte également sur un procédé de préparation du matériau de charge d'oxyde métallique.
PCT/AU2005/000899 2004-06-22 2005-06-22 Reduction electrochimique d'oxydes metalliques WO2005123986A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU2005254589A AU2005254589A1 (en) 2004-06-22 2005-06-22 Electrochemical reduction of metal oxides
US11/615,263 US20070181438A1 (en) 2004-06-22 2006-12-22 Electrochemical Reduction of Metal Oxides

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2004903409A AU2004903409A0 (en) 2004-06-22 Electrochemical reduction of metal oxides
AU2004903409 2004-06-22

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US11/615,263 Continuation-In-Part US20070181438A1 (en) 2004-06-22 2006-12-22 Electrochemical Reduction of Metal Oxides

Publications (1)

Publication Number Publication Date
WO2005123986A1 true WO2005123986A1 (fr) 2005-12-29

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/AU2005/000899 WO2005123986A1 (fr) 2004-06-22 2005-06-22 Reduction electrochimique d'oxydes metalliques

Country Status (3)

Country Link
US (1) US20070181438A1 (fr)
CN (1) CN101006204A (fr)
WO (1) WO2005123986A1 (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU2002951962A0 (en) * 2002-10-09 2002-10-24 Bhp Billiton Innovation Pty Ltd Electrolytic reduction of metal oxides
AU2002952083A0 (en) 2002-10-16 2002-10-31 Bhp Billiton Innovation Pty Ltd Minimising carbon transfer in an electrolytic cell
AU2003903150A0 (en) * 2003-06-20 2003-07-03 Bhp Billiton Innovation Pty Ltd Electrochemical reduction of metal oxides
RU2006114034A (ru) * 2003-09-26 2007-11-20 Би Эйч Пи БИЛЛИТОН ИННОВЕЙШН ПТИ ЛТД (AU) Электрохимическое восстановление оксидов металлов
WO2005038092A1 (fr) * 2003-10-14 2005-04-28 Bhp Billiton Innovation Pty Ltd Reduction electrochimique d'oxydes metalliques
JP2007529631A (ja) * 2004-03-22 2007-10-25 ビーエイチピー ビリトン イノベーション プロプライアタリー リミテッド 金属酸化物の電気化学的還元
WO2006010229A1 (fr) * 2004-07-30 2006-02-02 Bhp Billiton Innovation Pty Ltd Reduction electrochimique d'oxydes metalliques
EP1789609A4 (fr) * 2004-07-30 2008-11-12 Bhp Billiton Innovation Pty Reduction electrochimique d'oxydes metalliques

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AU2003257839A1 (en) * 2002-09-11 2004-04-30 Sumitomo Titanium Corporation Porous sintered compact of titanium oxide for production of metallic titanium through direct electrolytic process and process for producing the same

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AU2003257839A1 (en) * 2002-09-11 2004-04-30 Sumitomo Titanium Corporation Porous sintered compact of titanium oxide for production of metallic titanium through direct electrolytic process and process for producing the same

Also Published As

Publication number Publication date
CN101006204A (zh) 2007-07-25
US20070181438A1 (en) 2007-08-09

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