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WO2001042518A1 - Procede de digestion de metal contenant de la matiere a temperature elevee en presence d'une source d'oxyde de soufre tel le h2so¿4? - Google Patents

Procede de digestion de metal contenant de la matiere a temperature elevee en presence d'une source d'oxyde de soufre tel le h2so¿4? Download PDF

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Publication number
WO2001042518A1
WO2001042518A1 PCT/ZA2000/000245 ZA0000245W WO0142518A1 WO 2001042518 A1 WO2001042518 A1 WO 2001042518A1 ZA 0000245 W ZA0000245 W ZA 0000245W WO 0142518 A1 WO0142518 A1 WO 0142518A1
Authority
WO
WIPO (PCT)
Prior art keywords
metal containing
containing material
source
sulphate
oxide compound
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.)
Ceased
Application number
PCT/ZA2000/000245
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English (en)
Inventor
Gerard Pretorius
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.)
PACMIN INVESTMENTS Ltd
Original Assignee
PACMIN INVESTMENTS 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
Application filed by PACMIN INVESTMENTS Ltd filed Critical PACMIN INVESTMENTS Ltd
Priority to AU29791/01A priority Critical patent/AU2979101A/en
Publication of WO2001042518A1 publication Critical patent/WO2001042518A1/fr
Anticipated expiration legal-status Critical
Ceased 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • 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
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • 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
    • C22B34/1213—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 wet processes, e.g. using leaching methods or flotation techniques
    • 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
    • C22B34/125—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 sulfur ion as active agent
    • 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
    • Y02P10/20—Recycling

Definitions

  • This invention relates to a method of digesting metal containing material to
  • the invention also relates to a method of
  • process is a batch process and the first step is to digest the Ti0 2 bearing ore in
  • each mole of Ti0 2 present in the titaniferous material at least two moles of
  • H 2 S0 4 is present. This excess ensures that during the H 2 S0 4 digestion process, Ti0 2 in the
  • titaniferous material reacts with the excess H 2 S0 4 to form H 2 TiO(S0 4 ) 2 also
  • acid titanium sulphate which is a water soluble compound.
  • H 2 TiO(S0 4 ) 2 can also be represented as TiOS0 4 .H 2 S0 4 .
  • the H 2 TiO(S0 4 ) 2 is extracted with water from the reaction product (in the
  • the H 2 S0 4 used to digest part of the titaniferous material may be concentrated
  • H 2 S0 4 has a high vapour pressure and a boiling point of 290°C and
  • H 2 S0 4 decomposes into S0 3 and H 2 0 at 340°C and 1 atmosphere
  • furnace temperature above 340°C (and typically at 600°C), that is where
  • the at least one metal containing sulphate which forms may be soluble in a
  • suitable solvent preferably water.
  • the metal containing material may contain a number of different metals.
  • metals may be in the form of metal oxides, and/or metal
  • the metal containing material may include
  • metal containing ore may comprise metal containing ore.
  • metal containing ore may comprise metal containing ore.
  • metal containing ore may comprise metal containing ore.
  • containing slag in one embodiment of the invention it may comprise
  • titaniferous material such as for example ilmenite ore, for example ilmenite
  • titaniferous material may comprise titaniferous slag which may include pseudo brookite and/or perovskiie. It may also comprise plasma dissociated zircon
  • Activation may be either by thermal dissociation e.g. plasma flame to produce
  • the aid of a flux like B 2 0 3 and/or CaF 2 can be used.
  • dissociated zircon or chemical activated zircon can react with H 2 S0 4 .
  • the material may comprise at least one selected from the group comprising
  • transition metal sulphide ores e.g. manganese iron
  • clays tungsten and molybdenum alloys and oxides
  • rare earth ores e.g.
  • One or more compounds selected from the following group may be digested
  • furnace temperature is at about 200°C.
  • the metal containing material may be sized to have a particle size of 850 ⁇ m
  • the metal containing material is sized to have a particle
  • the particle size of 75 ⁇ m and smaller. In some applications the particle size may be smaller
  • the metal containing material may be sized by means of grinding, milling or
  • the milling may comprise dry milling or
  • wet milling may take place in the presence of sulphuric acid
  • the source of a sulphur oxide compound may comprise H 2 S0 4 or a source of
  • H 2 S0 4 comprises any
  • the decomposition product including but
  • the source of H 2 S0 4 may comprise a sulphate salt
  • the source of sulphur oxide compound comprises H 2 S0 4
  • the H 2 S0 4 may be concentrated or diluted. Preferably it is provided in a
  • H 2 S0 4 decomposes to form S0 3 and H 2 0. It is believed that these decomposition products may react
  • a source of S0 3 may comprise H 2 S0 4 .
  • the source of sulphur oxide compound is preferably provided in a
  • the sulphatable species of the metal containing compound Preferably a 4/3
  • the molar ratio of H 2 S0 4 : Ti values may be
  • H 2 S0 4 Ti values is calculated as 1:1, that is to form TiOS0 4 . It will be
  • titanium containing material titanium containing material.
  • H 2 S0 4 will be the stoichiometric equivalent, namely (la + 3b + 3c + Id
  • FeO is present (such as in ilmenite) the H 2 S0 4 will oxidise the FeO to Fe 2 0 3
  • the digestion stage is above 400°C, preferably above 450°C, more
  • the reaction product of the digestion stage may be subjected to heat treatment
  • the dead burn stage (hereinafter referred to as the dead burn stage) to ensure that substantially all
  • containing material comprises titanium containing material and titanium
  • TiOS0 4 is present as the titanium containing sulphate forms
  • This step is considered to be most preferred, and is preferably carried
  • H 2 S0 4 is usually higher than 320°C to cause the sulphate in the form of H 2 S0 4 to dissociate into H 2 0 and S0 3 (S0 3 can also further dissociation into S0 2 and
  • the product temperature may be from 400 to 550°C.
  • the digestion stage and dead burn stage are preferably carried out as two
  • the product Prior to the digestion stage the product may go through a warming stage
  • the warming occurs as fast as possible.
  • the burn stage the product is allowed to cool (hereinafter referred to as the cooling stage).
  • the cooling may be natural, but it may also be forced to speed up this
  • the metal containing material is reacted with H 2 S0 4 by mixing
  • a first furnace such as
  • tunnel kiln may be used for the warming and digestion stages and a second
  • furnace such as a rotary kiln may be used for the other stages.
  • the reaction product of the digestion stage may also be milled prior to
  • the digestion process is preferably carried out at about atmospheric pressure
  • the reaction conditions are preferably such to prevent S0 3 from decomposing.
  • the additional source may comprise a source of sulphate.
  • additional source may comprise ammonium sulphate ((NH 4 ) 2 S0 4 ), or
  • ammonium bisulphate (NH 4 HS0 4 ).
  • it comprises ammonium
  • Ammonium sulphate converts to ammonium bisulphate in the
  • the additional source comprises ammonium sulphate, an amount thereof
  • ammonium bisulphate decomposes to produce off gases
  • the process may also include the step of removing sulphate (if present),
  • substantially only TiOS0 4 is present as the titanium containing sulphate.
  • sulphate especially H 2 S0 4 may be removed by means of heat treatment
  • treatment should preferably also remove the sulphate and S0 3 originating from
  • the reaction time is typically between half an hour and six hours depending
  • the digestion method may also include the step of separating the metal containing sulphate from other material. Where water soluble and water
  • the reaction product may
  • leachate may then be separated from undissolved solids.
  • titanium containing sulphate forms, it may be in the form water
  • H 2 TiO(S0 4 ) 2 which may soluble in water. Alternatively it may be
  • the leachate may be
  • containing sulphate is contained in the leachate.
  • Standard processes may be used for this purpose and may include pH control,
  • the invention also relates to a product formed by the digestion process
  • the water-soluble metal containing sulphate including water-soluble metal containing sulphate.
  • the sulphates are hydrated or dissolved in water. According to another aspect of the present invention a method of separating
  • reaction product including at least one metal containing sulphate
  • containing material comprises the steps of
  • reaction product including at least one metal containing sulphate
  • the method may also include the step of treating the leachate to separate
  • the invention also relates to a product formed by the process.
  • Zr0 can be retrieved, the lattice must be dissociated to form Zr0 2 .Si0 2 .
  • Plasma dissociated zircon Plasma dissociated zircon
  • dissociation of zircon is about 85% efficient, that is 15% (mass/mass) remains
  • 100kg of PDZ was provided and it contained 85kg Zr0 2 .Si0 4
  • the PDZ was dry milled to have a particle size smaller then
  • Zr(S0 4 ) 2 is stable at 600°C with the result that little
  • the crushed cake was
  • sulphate leach can be used as a feedstock to manufacture zirconium
  • the insoluble products of the cake comprised 15kg ZrSi0 4 ,
  • the furnace included a ceramic lined gas outlet which lead into a scrubber for
  • the scrubber comprised a stirred vessel containing water and slaked lime.
  • the scrubber was
  • the pressure in the furnace was slightly below atmospheric pressure. This was
  • One current process for treating ilmenite involves smelting iron ore in high
  • Such slags can be used in either the
  • the present invention allows ilmenite or similar materials i.e. titaniferous
  • feedstocks can be combined with fluxes like Si0 2 , CaO, dolomite (CaO: MgO)
  • Witbank was used. This slag has similarities to ilmenite slags that were
  • phases of this slag are as
  • the slag in an amount of 100kg was dry milled to a particle size of smaller than
  • H 2 S0 4 to be added was calculated on the basis as set out in Table 1.
  • the H 2 S0 4 provided a 41,7% excess H 2 S0 4 calculated on the basis of a Ti0 2 : S0 4 2"
  • This period is known as the digestion stage during which
  • the said gasses may be fed through a ceramic lined tube from
  • crushed cake was then leached with 375£ water at 60°C, thereby leaching the
  • leachate leachate are also indicated in Table 2.
  • the insolubles are safe to be dumped.
  • the leachate was then treated to reduce Fe 3+ to Fe 2+ . This was done by adding
  • the hydrolysed product, TiO(OH) 2 is also known as crude anatase pulp
  • CAP had a high purity and also has the advantage that it is in activated form.
  • the slag in an amount of 100kg was milled with 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to give 200kg H 2 S0 4 (98% purity) to
  • 6mm alumina beads was used for this purpose at 500rpm for 1 hour.
  • the H 2 S0 4 provided a 59.6% excess H 2 S0 4 calculated on the basis of a Ti0 2
  • the containers were introduced into a top hat furnace, and
  • the furnace was ramped up to 600°C to provide a product temperature
  • Insolubles and solubles may be separated by leaching the reaction product with
  • Insoluble TiOS0 4 is a lucrative feedstock to produce synthetic rutile
  • containing ore feedstock can be treated with H 2 S0 4 to produce soluble
  • Another variation involves the digestion of rare earth containing ores e.g.
  • precious metal mixtures and ores may be used to digest precious metal mixtures and ores. e.g. Pt, Au, Pd and Ag.

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

Abstract

La présente invention concerne un procédé de digestion de métal contenant de la matière comportant des étapes de mise à disposition de métal contenant de la matière et de réaction du métal contenant de la matière avec une source d'au moins un composé d'oxydes de soufre à une température de fourneau supérieure à 340 °C afin de former au moins un métal contenant du sulfate. Le produit de réaction dudit procédé peut aussi être soumis à une lixiviation au moyen d'un solvant en vue de séparer certains métaux précieux d'une autre matière dans un composé contenant du métal.
PCT/ZA2000/000245 1999-12-13 2000-12-12 Procede de digestion de metal contenant de la matiere a temperature elevee en presence d'une source d'oxyde de soufre tel le h2so¿4? Ceased WO2001042518A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU29791/01A AU2979101A (en) 1999-12-13 2000-12-12 Method of digesting metal containing material at elevated temperature in the presence of sulphur oxide compound source such as h2s04

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ZA997628 1999-12-13
ZA99/7628 1999-12-13

Publications (1)

Publication Number Publication Date
WO2001042518A1 true WO2001042518A1 (fr) 2001-06-14

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Family Applications (2)

Application Number Title Priority Date Filing Date
PCT/ZA2000/000245 Ceased WO2001042518A1 (fr) 1999-12-13 2000-12-12 Procede de digestion de metal contenant de la matiere a temperature elevee en presence d'une source d'oxyde de soufre tel le h2so¿4?
PCT/ZA2000/000246 Ceased WO2001042520A1 (fr) 1999-12-13 2000-12-12 Procede de digestion du titane contenant de la matiere et produits obtenus par ce procede

Family Applications After (1)

Application Number Title Priority Date Filing Date
PCT/ZA2000/000246 Ceased WO2001042520A1 (fr) 1999-12-13 2000-12-12 Procede de digestion du titane contenant de la matiere et produits obtenus par ce procede

Country Status (2)

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AU (2) AU2979201A (fr)
WO (2) WO2001042518A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11083796B2 (en) 2005-07-26 2021-08-10 Durect Corporation Peroxide removal from drug delivery vehicle
US11400019B2 (en) 2020-01-13 2022-08-02 Durect Corporation Sustained release drug delivery systems with reduced impurities and related methods
US12433877B2 (en) 2021-01-12 2025-10-07 Durect Corporation Sustained release drug delivery systems and related methods

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA2989128A1 (fr) * 2014-07-08 2016-01-14 Avertana Limited Extraction de produits presents dans des mineraux contenant du titane
US12172905B2 (en) 2018-12-14 2024-12-24 Avertana Limited Methods of extraction of products from titanium-bearing materials
CN111422905A (zh) * 2020-04-02 2020-07-17 绵竹市金坤化工有限公司 一种硫酸锆的制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4120694A (en) * 1977-09-06 1978-10-17 The United States Of America As Represented By The Secretary Of The Interior Process for purifying a titanium-bearing material and upgrading ilmenite to synthetic rutile with sulfur trioxide
FR2463189A1 (fr) * 1979-08-13 1981-02-20 Metallurgie Hoboken Procede de recuperation de metaux non ferreux contenus dans un residu riche en goethite
GB2162831A (en) * 1984-07-27 1986-02-12 Cookson Group Plc Process for extracting zirconia from dissociated zircon
US4902485A (en) * 1986-08-14 1990-02-20 Bayer Aktiengesellschaft Process for the production of titanium dioxide pigments
EP0659688A1 (fr) * 1993-12-23 1995-06-28 Bayer Ag Procédé de préparation de dioxyde de titane selon le procédé sulfate
DE4421818C1 (de) * 1994-06-22 1996-02-29 Bayer Ag Verfahren zur Herstellung von Titandioxid nach dem Sulfatverfahren
US5618331A (en) * 1995-12-04 1997-04-08 Kemicraft Overseas Limited Vapor phase fluidized bed sulfation of titaniferous materials

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA942437A (en) * 1970-05-15 1974-02-19 David Weston Flotation of copper ores
DE3313072A1 (de) * 1982-07-17 1984-01-19 Bayer Ag, 5090 Leverkusen Verfahren zur herstellung einer hydrolysierbaren titanylsulfatloesung

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4120694A (en) * 1977-09-06 1978-10-17 The United States Of America As Represented By The Secretary Of The Interior Process for purifying a titanium-bearing material and upgrading ilmenite to synthetic rutile with sulfur trioxide
FR2463189A1 (fr) * 1979-08-13 1981-02-20 Metallurgie Hoboken Procede de recuperation de metaux non ferreux contenus dans un residu riche en goethite
GB2162831A (en) * 1984-07-27 1986-02-12 Cookson Group Plc Process for extracting zirconia from dissociated zircon
US4902485A (en) * 1986-08-14 1990-02-20 Bayer Aktiengesellschaft Process for the production of titanium dioxide pigments
EP0659688A1 (fr) * 1993-12-23 1995-06-28 Bayer Ag Procédé de préparation de dioxyde de titane selon le procédé sulfate
DE4421818C1 (de) * 1994-06-22 1996-02-29 Bayer Ag Verfahren zur Herstellung von Titandioxid nach dem Sulfatverfahren
US5618331A (en) * 1995-12-04 1997-04-08 Kemicraft Overseas Limited Vapor phase fluidized bed sulfation of titaniferous materials

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SAHOO P K ET AL: "SULPHATION-ROASTING OF LOW-GRADE MANGANESE ORES - OPTIMISATION BY FACTORIAL DESIGN", INTERNATIONAL JOURNAL OF MINERAL PROCESSING,NL,ELSEVIER SCIENCE PUBLISHERS, AMSTERDAM, vol. 25, no. 1/02, 1989, pages 147 - 152, XP000005998 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11083796B2 (en) 2005-07-26 2021-08-10 Durect Corporation Peroxide removal from drug delivery vehicle
US11400019B2 (en) 2020-01-13 2022-08-02 Durect Corporation Sustained release drug delivery systems with reduced impurities and related methods
US11771624B2 (en) 2020-01-13 2023-10-03 Durect Corporation Sustained release drug delivery systems with reduced impurities and related methods
US12433877B2 (en) 2021-01-12 2025-10-07 Durect Corporation Sustained release drug delivery systems and related methods

Also Published As

Publication number Publication date
AU2979101A (en) 2001-06-18
AU2979201A (en) 2001-06-18
WO2001042520A8 (fr) 2001-10-11
WO2001042520A1 (fr) 2001-06-14

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