WO2004038048A1 - Procede et dispositif pour effectuer une reaction tribochimique - Google Patents

Procede et dispositif pour effectuer une reaction tribochimique Download PDF

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Publication number
WO2004038048A1
WO2004038048A1 PCT/DE2003/003525 DE0303525W WO2004038048A1 WO 2004038048 A1 WO2004038048 A1 WO 2004038048A1 DE 0303525 W DE0303525 W DE 0303525W WO 2004038048 A1 WO2004038048 A1 WO 2004038048A1
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WO
WIPO (PCT)
Prior art keywords
reaction
titanium
granular
medium
metal
Prior art date
Application number
PCT/DE2003/003525
Other languages
German (de)
English (en)
Inventor
Peter Jörg PLATH
Original Assignee
Plath Peter Joerg
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 Plath Peter Joerg filed Critical Plath Peter Joerg
Priority to AU2003281966A priority Critical patent/AU2003281966A1/en
Priority to EP03773570A priority patent/EP1558774B1/fr
Priority to DE50309132T priority patent/DE50309132D1/de
Publication of WO2004038048A1 publication Critical patent/WO2004038048A1/fr

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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
    • 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
    • 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
    • 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
    • C22B34/1218—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 dry processes
    • C22B34/1222—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 dry processes using a halogen containing 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
    • C22B34/1263—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
    • C22B34/1281—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 using carbon containing agents, e.g. C, CO, carbides

Definitions

  • the invention is in the field of tribochemical reactions and relates in particular to the use of Faraday instabilities when carrying out a tribochemical reaction.
  • titanium tetrachloride can be obtained from the known titanium-containing minerals such as e.g. Ilmenite or rutile is produced in a rotary kiln or in a fluidized bed furnace at temperatures of approx. 800 - 1000 ° C. After appropriate cleaning (crystallization and subsequent distillation at 136 ° C), the liquid titanium tetrachloride is then reduced to titanium sponge with liquid magnesium at approx. 800 - 1000 ° C. The resulting magnesium chloride is washed out and electrolytically reduced again to magnesium, which is returned to the process.
  • the known titanium-containing minerals such as e.g. Ilmenite or rutile is produced in a rotary kiln or in a fluidized bed furnace at temperatures of approx. 800 - 1000 ° C. After appropriate cleaning (crystallization and subsequent distillation at 136 ° C), the liquid titanium tetrachloride is then reduced to titanium sponge with liquid magnesium at approx. 800 - 1000 ° C. The resulting magnesium chloride is
  • the titanium sponge Due to its large surface area, the titanium sponge contains even larger amounts of oxygen bound, which are not required as an alloy component in the metal to be produced.
  • the titanium sponge has to be broken, crushed, pressed into electrodes and then remelted in an arc using the zone melting process to form compact metallic titanium. All titanium-related steps are carried out under protective gas (inert gas) to avoid oxidation.
  • titanium tetraiodide which is obtained from titanium tetrachloride, is decomposed on thin, 1300 ° C hot tungsten wires using the van Arkel and de Boer process.
  • the object of the invention is to provide an improved method and an improved device for carrying out a tribochemical reaction in which the disadvantages of the prior art are avoided, in particular in the production of titanium.
  • the granular medium can either participate in the reaction or be inert to reaction products and starting materials.
  • the object of the invention is also to generate a special tribochemical reaction situation with the aid of the generation of Faraday instabilities in a granular (granules preferably with grains of preferably 0.1 to 20 mm diameter) of the ores / minerals, which the direct conversion of the Ore / mineral granules permitted by means of reducing agents and halogen gas by heterogeneous catalytic reaction and oxidation of the reducing agent.
  • the object of the invention in connection with the production of titanium is, in particular, with the aid of the generation of Faraday instabilities in a granular (preferably granules with a grain size of 0.1 to 20 mm diameter) medium of the ores / minerals (eg ilmenite or rutile) to produce a special tribochemical reaction situation, which the direct conversion of the ore / mineral granulate to metallic titanium, which preferably only has customary accompanying elements, using a reducing agent, preferably carbon monoxide and halogen gas (preferably iodine or chlorine) by heterogeneous catalytic reaction and oxidation of the reducing agent , for example, the oxidation of carbon monoxide to carbon dioxide.
  • a reducing agent preferably carbon monoxide and halogen gas (preferably iodine or chlorine)
  • the object of the invention in connection with the production of titanium dioxide is, with the aid of the production of Faraday instabilities in a granular (preferably granules with a grain size of 0.1 to 20 mm diameter) medium of the ores / minerals (eg ilmenite or rutile ) to produce a special tribochemical reaction situation which allows the direct conversion of the ore / mineral granules to titanium dioxide by means of a reducing agent, preferably carbon monoxide and halogen gas (preferably chlorine) by heterogeneous catalytic reaction and oxidation of the reducing agent, for example the oxidation of carbon monoxide to carbon dioxide.
  • a reducing agent preferably carbon monoxide and halogen gas (preferably chlorine)
  • the invention encompasses the idea in granular or spherical media
  • the granular medium is moved up and down in the gravitational field in order to to be brought into a state in which the granular bed behaves similar to a liquid phase consisting of solid components. In this state, Faraday instabilities occur on the particles of the granular medium.
  • the Farady instabilities are generated by moving a granular, granular or spherical medium up and down, with the help of the Farady instabilities at contact points / points of the components of the medium forming tribochemical reaction conditions under which the tribochemical Reactions expires.
  • the Faraday instabilities lead to a spatial or spatio-temporal pattern formation with zones of high mechanical energy in the granular medium. In these zones, even at comparatively low temperatures, the tribochemical reactions in the area between or on the colliding particles of the granulate or. of the balls take place.
  • the advantage of using the Faraday instabilities to carry out tribochemical reactions over the known fluidized bed process is, in particular, that in the granular fluidized bed using Faraday instabilities, excitation areas arise in which the tribochemical reactions can take place at much lower temperatures than in a conventional one Fluidized bed.
  • An advantage of the method when used for metal extraction is that the reduction of the metal oxide (ore) by means of coal and halogen gas is replaced by the much more effective heterogeneous catalytic gas-solid reaction between ore, reducing agent (e.g. carbon monoxide) and halogen gas to metal halide and carbon dioxide ,
  • reducing agent e.g. carbon monoxide
  • One advantage of the process with regard to the production of titanium by the titanium tetrajodide process is that the very energy-intensive, multi-stage process of producing titanium from titanium ore (eg ilmenite or rutile) via the titanium sponge, which is technically very complex to handle, by means of a single-stage, energy-saving process is replaced without an intermediate step over titanium sponge.
  • An advantage of the process with regard to the production of titanium white (titanium dioxide) by the titanium tetrachloride method is that the multi-stage process can be replaced by a one-stage process (addition of oxygen in the titanium tetrachloride stream).
  • Figure 1 is a schematic representation of a device for performing a tribochemical reaction in which Faraday instabilities are used.
  • Figure 2 is a schematic representation of another device for performing a tribochemical reaction in which Faraday instabilities are used.
  • FIG. 1 shows a device 1 for using Faraday instabilities to carry out a tribochemical reaction.
  • the device 1 is particularly suitable for the extraction of raw titanium (titanium tetrahalide) for further processing to titanium or titanium white (titanium dioxide) from titanium-containing ore / minerals.
  • the ore or minerals are applied to a horizontal plate or plate 9.
  • the plate / plate 9 is moved in the vertical direction by means of a movement device 5.
  • Pneumatic, hydraulic cylinders or linear drives can be used in particular as movement devices 5.
  • the vertical movement is such that Faraday instability occurs in the granular ore or mineral.
  • the movement can take place in a periodic or chaotic manner in particular.
  • educt fluids can be introduced into the reaction mixture through bores.
  • these are gaseous halides and carbon monoxide as reducing agents.
  • the reaction space of the device 1 is delimited from the environment. This is done in particular by a side wall of the lower reactor part 8, which is advantageously cylindrical, and by a cover 3, which is sealed in the parting plane 4 against the side wall of the lower reactor part 8.
  • the cover 3 can be flanged while a seal (not shown) is introduced in the parting plane 4.
  • at least one inlet 6 may be provided. This can advantageously be attached to the lower part 8 of the reactor.
  • this is provided with at least one opening 2, which is advantageously made on the cover 3 of the reactor.
  • heatable metal wires can be attached, in particular on the cover of the reactor, on which titanium tetrahalide can precipitate and decompose.
  • titanium iodide these are, for example, tungsten wires.
  • a further opening can be provided in order to introduce oxygen into the reaction space for the production of titanium dioxide from titanium tetrachloride.
  • this introduction can also only take place downstream - after the titanium tetrachloride has been drawn off from the reaction space - after the reaction products have passed through the opening 2.
  • FIG. 2 shows a device 20, similar to device 1 from FIG. 1, for using Faraday instabilities when carrying out tribochemical reactions. Identical features are identified by the same reference symbols.
  • the device 20 in FIG. 2 differs in particular from the device 1 according to FIG. 1 in that the movement device 5 is realized outside the reaction chamber of the device 20. This has the advantage that reaction products, intermediates and products cannot damage the movement devices in a corrosive or other way. In this case, the higher load must be taken into account when designing the movement device 5.
  • the ground ores / minerals are brought into a state on a plate which swings up and down in the vertical direction in the gravitational field, in which the granular bed behaves similarly to a liquid phase which consists of solid components.
  • granular layer with the (protective) gas phase Faraday instabilities form, for example in the form of spatially stable wave patterns.
  • Inert gases preferably noble gases, preferably argon and helium, are preferably used as the protective gas. If individual granular particles collide in the particularly excited areas of this layer, the gases in the reaction space can react catalytically with one another tribochemically at the joints. If, for example, titanium ores and titanium minerals are processed, titanium / titanium oxide will be the end product.
  • the product of this reaction is initially a metal salt or complex.
  • the product of this reaction with titanium ores / titanium minerals is a titanium tetrahalide, which sublimes or vaporizes as a gas.
  • the sublimate can be mixed with oxygen at high temperature and oxidized to titanium dioxide.
  • the resulting chlorine gas can be returned to the process.
  • the sublimate / steam is decomposed, for example on electrically heated tungsten wires, at approximately 1300 ° C to form compact titanium and iodine.
  • the iodine can in turn be returned to the process.
  • the described method and the explained devices 1 and 20 can be used for the carbon-free production of metal and metal oxide from metal-containing ore.
  • a metal salt or. created a complex In a heterogeneous gas-solid reaction, a metal salt or. created a complex. This metal salt / complex can then be processed further. Solutions of several metal salts can be separated here, for example, using a method which is described in the international patent application PCT / DE02 / 01377.
  • the process described is also suitable for the extraction of (raw) titanium and titanium dioxide from the known titanium-containing minerals, for example ilmenite and rutile.
  • a reducing agent preferably carbon monoxide
  • a halogen preferably chlorine or iodine
  • chlorine or iodine is advantageously used as halogen in the gas-solid reaction in addition to carbon monoxide
  • the titanium tetrachloride or titanium tetraiodide is formed.
  • the titanium tetrachloride can then be processed in the known, traditional manner with magnesium to titanium in the form of a titanium sponge. However, the titanium tetraiodide is sublimed and the pure titanium is deposited therefrom with thermal decomposition, without the formation of sponges.

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

Abstract

L'invention concerne un procédé et un dispositif permettant d'effectuer une réaction tribochimique. Des instabilités de Faraday sont produites, du fait qu'un milieu grené, granuleux ou à base de billes est déplacé en va-et-vient. Des conditions de réaction tribochimiques sont induites à l'aide des instabilités de Faraday, en des points de contact de particules du milieu. A cet effet, le milieu peut participer à la réaction ou avoir un comportement inerte vis-à-vis d'autres éduits. Ledit procédé s'utilise dans la production de titane (brut) et de dioxyde de titane à partir de minéraux à base de titane, par exemple l'ilménite et le rutile.
PCT/DE2003/003525 2002-10-22 2003-10-22 Procede et dispositif pour effectuer une reaction tribochimique WO2004038048A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
AU2003281966A AU2003281966A1 (en) 2002-10-22 2003-10-22 Method and device for carrying out a tribochemical reaction
EP03773570A EP1558774B1 (fr) 2002-10-22 2003-10-22 Procede et dispositif pour effectuer une reaction tribochimique
DE50309132T DE50309132D1 (de) 2002-10-22 2003-10-22 Verfahren und vorrichtung zum durchführen einer tribochemiscen reaktion

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10249163A DE10249163A1 (de) 2002-10-22 2002-10-22 Verfahren und Vorrichtung zur Nutzung von Faraday-Instabilitäten zur Durchführung von tribochemischen Reaktionen
DE10249163.1 2002-10-22

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WO2004038048A1 true WO2004038048A1 (fr) 2004-05-06

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PCT/DE2003/003525 WO2004038048A1 (fr) 2002-10-22 2003-10-22 Procede et dispositif pour effectuer une reaction tribochimique

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EP (1) EP1558774B1 (fr)
CN (1) CN100493784C (fr)
AT (1) ATE385523T1 (fr)
AU (1) AU2003281966A1 (fr)
DE (2) DE10249163A1 (fr)
WO (1) WO2004038048A1 (fr)

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* Cited by examiner, † Cited by third party
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US8329626B2 (en) * 2010-06-24 2012-12-11 Johnson & Johnson Consumer Companies, Inc. Low-irritating, clear cleansing compositions with relatively low pH

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995008004A1 (fr) * 1993-09-13 1995-03-23 The Australian National University Traitement de l'ilmenite par broyage a froid
EP0744234A1 (fr) * 1995-05-26 1996-11-27 Th. Goldschmidt AG Procédé pour la fabrication de poudres métalliques nanocristallines et amorphes aux rayons X
US5582629A (en) * 1994-10-07 1996-12-10 Kurimoto, Ltd. Treatment process of sponge titanium powder
WO2002083261A2 (fr) * 2001-04-12 2002-10-24 Mir-Chem Gmbh Procede et dispositif pour extraire et separer des substances

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1995008004A1 (fr) * 1993-09-13 1995-03-23 The Australian National University Traitement de l'ilmenite par broyage a froid
US5582629A (en) * 1994-10-07 1996-12-10 Kurimoto, Ltd. Treatment process of sponge titanium powder
EP0744234A1 (fr) * 1995-05-26 1996-11-27 Th. Goldschmidt AG Procédé pour la fabrication de poudres métalliques nanocristallines et amorphes aux rayons X
WO2002083261A2 (fr) * 2001-04-12 2002-10-24 Mir-Chem Gmbh Procede et dispositif pour extraire et separer des substances

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
GERASIMOV K B ET AL: "TRIBOCHEMICAL EQUILIBRIUM IN MECHANICAL ALLOYING OF METALS", JOURNAL OF MATERIALS SCIENCE, CHAPMAN AND HALL LTD. LONDON, GB, vol. 26, no. 9, 1 May 1991 (1991-05-01), pages 2495 - 2500, XP000430909, ISSN: 0022-2461 *
POPOVICH A A ET AL: "Mechanisms governing tribochemical reduction of metals and non-metals from their oxides", J ALLOYS COMPD;JOURNAL OF ALLOYS AND COMPOUNDS JAN 11 1993, vol. 190, no. 2, 11 January 1993 (1993-01-11), pages 143 - 147, XP002270629 *
POPOVICH A A: "Microstructure and properties of titanium carbide and titanium carbide-based alloys obtained by tribochemical synthesis", J ALLOYS COMPD;JOURNAL OF ALLOYS AND COMPOUNDS MAY 24 1993, vol. 196, no. 1-2, 24 May 1993 (1993-05-24), pages 97 - 104, XP002270630 *

Also Published As

Publication number Publication date
AU2003281966A1 (en) 2004-05-13
CN100493784C (zh) 2009-06-03
DE10249163A1 (de) 2004-05-06
ATE385523T1 (de) 2008-02-15
DE50309132D1 (de) 2008-03-20
EP1558774A1 (fr) 2005-08-03
EP1558774B1 (fr) 2008-02-06
CN1726294A (zh) 2006-01-25

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