EP0719346A1 - Traitement de l'ilmenite par broyage a froid - Google Patents

Traitement de l'ilmenite par broyage a froid

Info

Publication number
EP0719346A1
EP0719346A1 EP94927454A EP94927454A EP0719346A1 EP 0719346 A1 EP0719346 A1 EP 0719346A1 EP 94927454 A EP94927454 A EP 94927454A EP 94927454 A EP94927454 A EP 94927454A EP 0719346 A1 EP0719346 A1 EP 0719346A1
Authority
EP
European Patent Office
Prior art keywords
dimethyl ammonium
ilmenite
milling
additive
titaniferous
Prior art date
Legal status (The legal status 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 status listed.)
Withdrawn
Application number
EP94927454A
Other languages
German (de)
English (en)
Other versions
EP0719346A4 (fr
Inventor
Andrzej Calka
Patrice Millet
Barry William Ninham
James Stanislaus Williams
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
WESTRALIAN SANDS Ltd
Australian National University
Original Assignee
WESTRALIAN SANDS Ltd
Australian National University
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 WESTRALIAN SANDS Ltd, Australian National University filed Critical WESTRALIAN SANDS Ltd
Publication of EP0719346A1 publication Critical patent/EP0719346A1/fr
Publication of EP0719346A4 publication Critical patent/EP0719346A4/fr
Withdrawn legal-status Critical Current

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
    • C22B34/1236—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 titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
    • C22B34/124—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 titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors
    • C22B34/1245—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 titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using acidic solutions or liquors containing a halogen ion as active agent
    • 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
    • C22B34/1204—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent
    • C22B34/1209—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 preliminary treatment of ores or scrap to eliminate non- titanium constituents, e.g. iron, without attacking the titanium constituent by dry processes, e.g. with selective chlorination of iron or with formation of a titanium bearing slag
    • 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
    • C22B34/1236—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 titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching

Definitions

  • the "Becher” process is also used to upgrade ilmenite - to remove iron and provide a feedstock for the "chloride route".
  • ilmenite is reacted with coal and sulphur in an iron reduction kiln at 1100°C. This reaction reduces the iron in the ilmenite to the metallic form.
  • the iron is rusted out in slurry form with ammonium chloride acting as a catalyst for the rusting.
  • the remaining iron compounds are removed by leaching with sulphuric acid.
  • the Murso process uses an oxidation of the ilmenite to convert substantially all the iron to the ferric state, then reduction of the oxidised material to convert substantially all the ferric iron to the ferrous state. These steps, of oxidation of the ilmenite followed by its reduction, produce a material which has an enhanced reactivity, from which the iron can be leached with dilute hydrochloric acid.
  • the prime object of the present invention is to provide a method of treating ilmenite and other titaniferous minerals to convert such minerals into a form from which the iron content can be removed by a simple leaching process.
  • That new ball mill which is described in the specification of International patent application No PCT/AU90/00471 (WIPO Publication No WO 91/04810), enables controlled-energy milling of a charge to be effected.
  • the present inventors have now discovered that under certain milling conditions, ilmenite can be reduced while being converted into a nanostructural form, and that iron can be removed from this product (for example, using hydrochloric acid at a temperature of about 100 C C).
  • the basic requirements of the cold milling process are: (i) that high energy milling is carried out at room temperature for a sufficient time period (up to 300 hours) to produce a powder having a nanostructural form, and (ii) that the milling is effected in the presence of suitable additives to the ball mill charge.
  • the milling is carried out in a ball mill of the type described and claimed in the specification of International patent application No PCT/AU90/00471.
  • simple milling of ilmenite did not produce a reactive nanostructural form of the mineral.
  • milling ilmenite with an additive to the ball mill charge did yield a reactive nanostructural product.
  • the milled samples were then leached with no further treatment.
  • the composition of each sample was assessed using one or more of the following techniques: x-ray diffraction; Mossbauer spectroscopy; transmission and scanning electron microscopy; atomic absorption spectrometry; Rutherford backscattering spectrometry.
  • structural development of the as-milled samples was monitored by x-ray diffraction of cobalt K ⁇ radiation using a Phillips diffractometer, and Rutherford backscattering spectrometry was used to analyse the presence of iron in chemically leached samples.
  • the pH was adjusted to a value of 5, which corresponds to positively charged ilmenite particles, in order to get adsorption of the anionic surfactant SDDS.
  • Potassium hydroxide and potassium chloride were used for pH adjustment.
  • No adjustment of the pH of the aqueous solution was necessary for experiments with the additive DDAOH.
  • the nanostructural ilmenite products obtained by milling the ilmenite with the additives (i) DDAOH, (ii) SDDS and (iii) amorphous boron, were leached with 4M hydrochloric acid at temperatures ranging from 80°C to 100°C.
  • the Rutherford backscattering spectroscopy spectra of the leached materials showed

Landscapes

  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

Le broyage à billes très énergique de particules d'ilménite (ou d'autres minerais titanifères) à température ambiante, pendant des périodes allant jusqu'à 300 heures et en présence d'un additif approprié, donne une poudre nanostructuelle dont peut être lessivée au moins une proportion majeure du fer contenu dans le minerai titanifère. L'additif peut être un agent réducteur (du bore amorphe par exemple), un hydrocarbure à chaîne longue (du dodécane par exemple) ou un agent tensio-actif (de préférence acétate de dihexadecy 1 diméthyle ammonium, ou bromure de didodécyle diméthyle ammonium, ou acétate de didodécyle diméthyle ammonium, ou hydroxyde de didodécyle diméthyle ammonium, ou sulfate de sodium didodécyle). Le lessivage s'effectue de préférence en utilisant un acide chlorhydrique de 4M porté à une température allant de 80 à 100 °C.
EP94927454A 1993-09-13 1994-09-13 Traitement de l'ilmenite par broyage a froid Withdrawn EP0719346A4 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
AUPM117793 1993-09-13
AUPM1177/93 1993-09-13
PCT/AU1994/000550 WO1995008004A1 (fr) 1993-09-13 1994-09-13 Traitement de l'ilmenite par broyage a froid

Publications (2)

Publication Number Publication Date
EP0719346A1 true EP0719346A1 (fr) 1996-07-03
EP0719346A4 EP0719346A4 (fr) 1997-05-07

Family

ID=3777190

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94927454A Withdrawn EP0719346A4 (fr) 1993-09-13 1994-09-13 Traitement de l'ilmenite par broyage a froid

Country Status (6)

Country Link
EP (1) EP0719346A4 (fr)
JP (1) JPH09504829A (fr)
CA (1) CA2169947A1 (fr)
NZ (1) NZ273552A (fr)
WO (1) WO1995008004A1 (fr)
ZA (1) ZA947050B (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10124523A1 (de) * 2001-05-19 2002-11-21 Deutsche Telekom Ag Verfahren zur Darstellung mehrerer elektronisch gespeicherter Seiten

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1996010653A1 (fr) * 1994-10-04 1996-04-11 The Australian National University Traitement des mineraux pour l'extraction du zirconium
ATE200236T1 (de) 1995-08-28 2001-04-15 Advanced Nano Technologies Pty Verfahren zur herstellung ultrafeiner teilchen
US6375923B1 (en) 1999-06-24 2002-04-23 Altair Nanomaterials Inc. Processing titaniferous ore to titanium dioxide pigment
US6440383B1 (en) 1999-06-24 2002-08-27 Altair Nanomaterials Inc. Processing aqueous titanium chloride solutions to ultrafine titanium dioxide
US6548039B1 (en) 1999-06-24 2003-04-15 Altair Nanomaterials Inc. Processing aqueous titanium solutions to titanium dioxide pigment
DE10249163A1 (de) * 2002-10-22 2004-05-06 Plath, Peter Jörg, Prof.Dr. Verfahren und Vorrichtung zur Nutzung von Faraday-Instabilitäten zur Durchführung von tribochemischen Reaktionen

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB714857A (en) * 1951-08-30 1954-09-01 British Titan Products Improvements in or relating to the manufacture of titanium dioxide pigments from mineral rutile ores
DE3721509A1 (de) * 1987-06-30 1989-01-12 Kloeckner Humboldt Deutz Ag Verfahren und vorrichtung zur laugung von metallhaltigen, nicht vorgetrockneten rohstoffen
WO1991004810A1 (fr) * 1989-10-03 1991-04-18 The Australian National University Appareil et procede de broyage a billes et production de materiaux metalliques amorphes

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1103379A (fr) * 1976-05-19 1981-06-16 Willy Manfroy Methode de broyage en milieu humide de mineraux non organiques ou organiques fossilises
BR7800585A (pt) * 1978-01-31 1979-08-21 Vale Do Rio Doce Co Processo de obtencao de concentrados mecanicos de anatasio
US4175952A (en) * 1978-07-19 1979-11-27 Uop Inc. Recovery of iron and titanium metal values
US4197276A (en) * 1978-07-31 1980-04-08 Uop Inc. Recovery of titanium metal values
US4175110A (en) * 1978-08-22 1979-11-20 Uop Inc. Recovery of titanium metal values

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB714857A (en) * 1951-08-30 1954-09-01 British Titan Products Improvements in or relating to the manufacture of titanium dioxide pigments from mineral rutile ores
DE3721509A1 (de) * 1987-06-30 1989-01-12 Kloeckner Humboldt Deutz Ag Verfahren und vorrichtung zur laugung von metallhaltigen, nicht vorgetrockneten rohstoffen
WO1991004810A1 (fr) * 1989-10-03 1991-04-18 The Australian National University Appareil et procede de broyage a billes et production de materiaux metalliques amorphes

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See also references of WO9508004A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10124523A1 (de) * 2001-05-19 2002-11-21 Deutsche Telekom Ag Verfahren zur Darstellung mehrerer elektronisch gespeicherter Seiten

Also Published As

Publication number Publication date
EP0719346A4 (fr) 1997-05-07
WO1995008004A1 (fr) 1995-03-23
JPH09504829A (ja) 1997-05-13
ZA947050B (en) 1995-08-07
CA2169947A1 (fr) 1995-03-23
NZ273552A (en) 1996-12-20

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