EP1558774B1 - 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
EP1558774B1
EP1558774B1 EP03773570A EP03773570A EP1558774B1 EP 1558774 B1 EP1558774 B1 EP 1558774B1 EP 03773570 A EP03773570 A EP 03773570A EP 03773570 A EP03773570 A EP 03773570A EP 1558774 B1 EP1558774 B1 EP 1558774B1
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EP
European Patent Office
Prior art keywords
reaction
titanium
metal
medium
faraday
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Expired - Lifetime
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EP03773570A
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German (de)
English (en)
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EP1558774A1 (fr
Inventor
Peter Jörg Plath
Elisabeth Swart
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PLATH, PETER JOERG
SWART, ELISABETH
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Individual
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    • 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 more particularly relates to the use of Faraday instabilities in carrying out a tribochemical reaction.
  • titanium tetrachloride is prepared by the Kroll process using coal and chlorine gas from the known titanium-containing minerals, e.g. Ilmenite or rutile in a rotary kiln or fluidized bed at temperatures of about 800 - 1000 ° C is produced.
  • the liquid titanium tetrachloride is then reduced after appropriate purification (crystallization and subsequent distillation at 136 ° C) with liquid magnesium at about 800 - 1000 ° C to titanium sponge.
  • the resulting magnesium chloride is washed out and electrolytically re-reduced to magnesium, which is recycled to the process.
  • the titanium sponge because of its large surface area, still binds larger amounts of oxygen which are not needed as an alloying ingredient in the intended metal to be produced.
  • the titanium sponge must be broken, crushed, pressed into electrodes and then remelted by arc melting in the arc to form compact metallic titanium. All the titanium process steps are carried out to avoid oxidation under inert gas (inert gas).
  • titanium tetrachloride which is obtained from titanium tetrachloride, is decomposed on thin, 1300 ° C. tungsten wires by the method of van Arkel and de Boer.
  • EP-A-744,234 describes a method for producing nanocrystalline metal powders.
  • the known method involves a painting or tribochemical activation of magnesium hydride.
  • the painting is carried out in a laboratory ball mill and using an organic solvent.
  • WO-A-95 08004 describes a method in which a nanostructured powder is produced by high-energy milling of ilmenite. To carry out the known method, a special form of ball mill is used.
  • the object of the invention is to provide an improved method and an improved apparatus for carrying out a tribochemical reaction in which the disadvantages of the prior art are avoided, in particular in titanium production.
  • the granular medium may either participate in the reaction or be inert to reaction products and starting materials.
  • the object of the invention is moreover, with the aid of the generation of Faraday instabilities in a granular (granules preferably with grain sizes of preferably 0.1 to 20 mm diameter) medium of the ores / minerals to produce a special tribochemical reaction situation, the direct conversion of Ore / mineral granules by reducing agent and halogen gas by heterogeneous catalytic reaction and oxidation of the reducing agent allowed.
  • the object of the invention in connection with the production of titanium is in particular, by means of the production of Faraday instabilities in a granular (granules preferably with grain sizes of 0.1 to 20 mm diameter) medium of the ores / minerals (eg ilmenite or rutile) to produce a special tribochemical reaction situation, which involves the direct conversion of the ore / mineral granules to metallic titanium, which preferably has only usual accompanying elements, by means of reducing agents 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 allowed.
  • reducing agents preferably carbon monoxide and halogen gas (preferably iodine or chlorine)
  • heterogeneous catalytic reaction preferably iodine or chlorine
  • the object of the invention in connection with the production of titanium dioxide is, with the help of the generation of Faraday instabilities in a granular (granules preferably with grain sizes of 0.1 to 20 mm diameter) medium of the ores / minerals (eg ilmenite or rutile) a produce special tribochemical reaction situation, which allows the direct conversion of ore / mineral granules to titanium dioxide by means of 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.
  • reducing agent preferably carbon monoxide and halogen gas (preferably chlorine)
  • the invention includes the idea of producing Faraday instabilities in granular or spherical media by means of up / down motions in carrying out a tribochemical reaction.
  • the granular medium is moved up and down the gravity field to enter To bring 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 created by moving a granular, granular or beaded medium up and down, forming tribochemical reaction conditions at the contact points / points of the constituents of the medium by means of Farady instabilities, at which the tribochemical reactions take place .
  • the use of Faraday instabilities in granular or spherical media for carrying out tribochemical reactions offers the advantage, compared to the classical method (Drekrohrofen or fluidized bed reactor) the advantage of being able to carry out the reaction in a thermodynamically much more favorable range.
  • the Faraday instabilities lead in the granular medium to a spatiotemporal pattern formation with zones of high mechanical energy. In these zones, even at relatively low temperatures, the tribochemical reactions in the area between or on the colliding particles of the granules or. the balls take place.
  • the advantage of using the Faraday instabilities for carrying out tribochemical reactions compared to the known fluidized bed method is in particular that in the granular, Faraday instabilities using fluidized bed energization areas arise in which the tribochemical reactions can proceed even at much lower temperatures than in a conventional Fluidized bed.
  • metal recovery process is that the reduction of metal oxide (ore) by coal and halogen gas is replaced by the much more effective heterogeneous catalytic gas-solid reaction between ore, reducing agent (eg carbon monoxide) and halogen gas to metal halide and carbon dioxide ,
  • An advantage of the process with regard to the production of titanium by the titanium tetraiodide process is that the very energy-consuming, multi-stage process of producing titanium from titanium ore (for example ilmenite or rutile) by means of a one-stage, very simple to handle titanium sponge. energy-saving process without an intermediate step is replaced by titanium sponge.
  • An advantage of the process with respect to the production of titanium white (titanium dioxide) according to the titanium tetrachloride method is that the multi-stage process can be replaced by a one-stage process (addition of oxygen to the titanium tetrachloride stream).
  • FIG. 1 shows a device 1 for utilizing Faraday instabilities for carrying out a tribochemical reaction.
  • the device 1 is particularly suitable for obtaining crude titanium (titanium tetrahalide) for further processing into titanium or titanium white (titanium dioxide) from titanium-containing ore / minerals.
  • the ore or minerals are applied to a horizontal plate or plate 9.
  • a moving device 5 By means of a moving device 5, the plate / the plate 9 is moved in the vertical direction.
  • a movement devices 5 in particular pneumatic, hydraulic cylinders or linear drives can be used.
  • the motion in the vertical is such that Faraday instability occurs in the granular ore or mineral.
  • the movement can take place in particular in a periodic or chaotic manner.
  • educt fluids can be introduced through bores in the reaction mixture.
  • these are gaseous halides and carbon monoxide as the reducing agent.
  • the reaction space of the device 1 is delimited from the environment. This is done in particular by a side wall of the reactor lower 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 reactor lower part 8.
  • the lid 3 can be flanged, while in the parting plane 4, a seal (not shown) is introduced.
  • at least one inlet 6 may be provided. This can be advantageously attached to the reactor base 8.
  • this is provided with at least one opening 2, which is advantageously attached to the lid 3 of the reactor.
  • heatable metal wires can be attached, in particular on the lid of the reactor, where titanium tetrahalide can precipitate and decompose.
  • titanium iodide these are, for example, tungsten wires.
  • a further opening may be provided to introduce oxygen to produce titanium dioxide from titanium tetrachloride into the reaction space.
  • this introduction can also be done only after the titanium tetrachloride has been removed from the reaction space after the reaction products have passed through the opening 2.
  • FIG. 2 shows a device 20 similar to the device 1 from FIG. 1 for using Faraday instabilities when carrying out tribochemical reactions. Same features marked with the same reference numerals.
  • 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 can not corrosive or otherwise damage the moving devices. When designing the movement device 5, the higher load must be taken into account in this case.
  • the ground ores / minerals are placed on a plate that swings up and down in the vertical direction in the gravitational field to a state in which the granular bed behaves similar to a liquid phase consisting of solid constituents.
  • Faraday instabilities are formed at the interface of this liquid, granular layer to the (protective) gas phase, for example in the form of spatially stable wave patterns.
  • Inert gases preferably noble gases, preferably argon and helium, are preferably used as protective gas. If individual granular particles collide in the particularly excited regions of this layer, the gases in the reaction space can react with each other in a tribochemical manner at the joints. If, for example, titanium ores, titanium minerals are processed, titanium / titanium oxide is the end product sought.
  • 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 evaporates as a gas.
  • the sublimate can be mixed with oxygen at high temperature and oxidized to titanium dioxide.
  • the resulting chlorine gas can be recycled to the process.
  • the sublimate / steam is decomposed, for example, on electrically heated tungsten wires at about 1300 ° C. to form compact titanium and iodine.
  • the iodine can in turn be recycled back into the process.
  • the described method and the illustrated devices 1 and 20 can be used for the carbon-free production of metal and metal oxide from metal-containing ore.
  • a metal salt resp. creates a complex.
  • This metal salt / complex can then be further processed. Solutions of several metal salts can be separated in this case, for example, by means of a method which in the international patent application PCT / DE02 / 01377 is described.
  • the process described is also suitable for recovering (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
  • 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 titanium sponge. However, the titanium tetraiodide is sublimed, and with thermal decomposition, the pure titanium is precipitated therefrom without sponging.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • 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)
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Claims (9)

  1. Procédé pour la réalisation d'une réaction tribochimique, caractérisé en ce qu'un milieu granulaire, granuleux ou formé de billes est soumis à un mouvement de va-et-vient dans l'espace de manière à générer des instabilités de Faraday, étant donné que des réactions tribochimiques sont réalisées à l'aide des instabilités de Faraday à des points de contact de particules du milieu.
  2. Procédé selon la revendication 1, caractérisé en ce que des corps de moule ne prenant pas part à la réaction, en particulier des billes, sont utilisés comme milieu pour la réalisation de la réaction.
  3. Procédé selon la revendication 1 ou 2, caractérisé en ce que des billes métalliques inertes, en particulier des billes en acier spécial, sont utilisées.
  4. Procédé selon la revendication 1, caractérisé en ce que des milieux qui prennent eux-mêmes part à la réaction, en particulier des minerais, sont utilisés comme milieux pour la réalisation de la réaction.
  5. Utilisation d'un procédé selon l'une quelconque des revendications 1 à 4 pour la fabrication sans carbone de métal et d'oxyde métallique.
  6. Utilisation d'un procédé selon l'une quelconque des revendications 1 à 4 pour la fabrication sans carbone de titane et de dioxyde de titane.
  7. Utilisation d'un procédé selon l'une quelconque des revendications 1 à 4 pour la fabrication sans carbone de complexes métalliques.
  8. Utilisation du procédé selon l'une quelconque des revendications 1 à 4 pour la fabrication sans carbone d'un métal et d'un oxyde métallique, étant donné que des fractions individuelles du matériau produit à partir du minerai sont séparées afin d'être utilisées pour produire un métal, un sel métallique ou un oxyde métallique.
  9. Dispositif pour la réalisation d'un procédé selon l'une quelconque des revendications 1 à 4 avec un espace réactionnel enveloppé dans lequel est formée au sein d'un couvercle (3) une surface d'appui (9) horizontale pour un milieu granulaire, granuleux ou formé de billes, étant donné que la surface d'appui (9) horizontale est couplée à un dispositif de mouvement avec lequel le milieu granulaire, granuleux ou formé de billes peut être soumis à un mouvement de va-et-vient pour générer des instabilités de Faraday sur des particules du milieu pour une réaction tribochimique, et étant donné qu'au moins une des caractéristiques suivantes est en outre prévue : un orifice (2) dans le couvercle (3) qui est configuré pour extraire des produits de réaction de l'espace réactionnel, et des fils métalliques chauffants sur lesquels du tétrahalogénure de titane peut se déposer et se décomposer, fils métalliques qui sont facultativement montés sur le couvercle (3).
EP03773570A 2002-10-22 2003-10-22 Procede et dispositif pour effectuer une reaction tribochimique Expired - Lifetime EP1558774B1 (fr)

Applications Claiming Priority (3)

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

Publications (2)

Publication Number Publication Date
EP1558774A1 EP1558774A1 (fr) 2005-08-03
EP1558774B1 true EP1558774B1 (fr) 2008-02-06

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EP03773570A Expired - Lifetime EP1558774B1 (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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US8329626B2 (en) * 2010-06-24 2012-12-11 Johnson & Johnson Consumer Companies, Inc. Low-irritating, clear cleansing compositions with relatively low pH

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ZA947050B (en) * 1993-09-13 1995-08-07 Univ Australian Limenite processing using cold milling.
JP2885098B2 (ja) * 1994-10-07 1999-04-19 株式会社栗本鐵工所 スポンジチタン粉の処理方法
ES2140733T3 (es) * 1995-05-26 2000-03-01 Goldschmidt Ag Th Proceso para la preparacion de polvo metalico amorfo a los rayos x y nanocristalino.
DE10291568D2 (de) * 2001-04-12 2004-04-15 Mir Chem Gmbh Verfahren und Vorrichtung zum Extrahieren und Separieren von Stoffen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MELO F.; UMBANHOWAR P.B.; SWINNEY H.L.: "Hexagons, Kinks, and Disorder in Oscillated Granular Layers", PHYSICAL REVIEW LETTERS, vol. 75, no. 21, 20 November 1995 (1995-11-20), pages 3838 - 3842 *

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Publication number Publication date
ATE385523T1 (de) 2008-02-15
CN1726294A (zh) 2006-01-25
CN100493784C (zh) 2009-06-03
AU2003281966A1 (en) 2004-05-13
DE50309132D1 (de) 2008-03-20
DE10249163A1 (de) 2004-05-06
EP1558774A1 (fr) 2005-08-03
WO2004038048A1 (fr) 2004-05-06

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