EP1989336B1 - Reactor intended for titanium production - Google Patents

Reactor intended for titanium production Download PDF

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Publication number
EP1989336B1
EP1989336B1 EP06742216A EP06742216A EP1989336B1 EP 1989336 B1 EP1989336 B1 EP 1989336B1 EP 06742216 A EP06742216 A EP 06742216A EP 06742216 A EP06742216 A EP 06742216A EP 1989336 B1 EP1989336 B1 EP 1989336B1
Authority
EP
European Patent Office
Prior art keywords
melting
reactor
titanium
section
chamber
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.)
Not-in-force
Application number
EP06742216A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP1989336A1 (en
Inventor
Jaroslav Vladik
Oleg Lysytchuk
Miroslav Sotornik
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.)
Individual
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Individual
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Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of EP1989336A1 publication Critical patent/EP1989336A1/en
Application granted granted Critical
Publication of EP1989336B1 publication Critical patent/EP1989336B1/en
Not-in-force legal-status Critical Current
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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
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/08—Apparatus
    • 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
    • C22B34/1268—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 alkali or alkaline-earth metals or amalgams
    • C22B34/1272—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 alkali or alkaline-earth metals or amalgams reduction of titanium halides, e.g. Kroll process
    • 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
    • C22B34/1295—Refining, melting, remelting, working up of titanium
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B3/00—Hearth-type furnaces, e.g. of reverberatory type; Tank furnaces
    • F27B3/04—Hearth-type furnaces, e.g. of reverberatory type; Tank furnaces of multiple-hearth type; of multiple-chamber type; Combinations of hearth-type furnaces
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/16—Introducing a fluid jet or current into the charge
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D3/00—Charging; Discharging; Manipulation of charge
    • F27D3/18—Charging particulate material using a fluid carrier
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/02—Supplying steam, vapour, gases, or liquids

Definitions

  • the invention comes within the scope of metallurgy of nonferrous metals and deals with the reactor construction that is intended for one-stage processing of titanium tetrachloride with use of natrium or magnesium.
  • reactors There are known the constructions of reactors described in patent specifications US 2004/0103791 , GB 1202581 or GB 1429333 comprising a variety of reaction zones into which a reduction gas is introduced. These reactors produce titanium dioxide; however, they cannot be used to produce pure titanium.
  • Specification GB 1260021 describes continual processing of titanic iron ore with use of hydrochlorid acid in the equipment containing two or more arranged in cascades and mutually connected reactors which comprise mixing devices. The temperature in each of the reactor vessels is produced as a result of exothermic reactions of titanium chloride and is stabilized by regulation of flow of reagents passing through the equipment. Titanium dioxide is produced by hydrolysis after final solid suspension extraction is performed.
  • the reactor is destined for primary processing of titanic iron ore into TiCl 4 with subsequent TiO 2 production and does not refer to the production of pure titanium.
  • Fabrication of pyrogenic TiO 2 with finely dispersed particles is described in patent specification GB 1187864 , where the reaction of gaseous TiCl 4 with oxygen is used to produce a gas mixture containing TiO 2 , which is consequently subjected to electrical field generated by electrodes and located in the reactor chamber at temperatures from 400 to 800°C. Said electrical field prevents accretion forming on the walls of reactor. After cooling the mixture down TiO 2 is separated either mechanically or with use of electrostatic dust extraction.
  • Construction of the reactor producing titanium is referred to in patent specification GB 814181 , describing continual processing of TiCl 4 vapours in the presence of alkaline substances or alkaline earth metals, dissolved in a melt containing halides or other metals, the reaction vessel being designed so that its construction prevents unmelted reduction metal from coming into contact with TiO 2 vapours. Titanium formed in the reaction chamber settles down at the bottom and can be released as a suspension in a salt melt or can be pulled out as a cooled block of salt containing titanium. Weak point of this equipment is low manufacturing capacity and the fact that final product is not pure titanium but just a suspension in a salt melt or a cooled block of salt containing titanium.
  • a reactor as defined in claim 1 intended for titanium production, comprising a body whose tubular jacket is cooled by a refrigerant and which is equipped with melting electrodes and comprises other systems designed to introduce gaseous medium containing titanium, to introduce liquid reduction agent and fluxing agents and to discharge by-pass products and to collect finished titanium.
  • Subject matter of the invention consists in division of the interior of the reactor into two sections, namely reduction and melting ones, divided one from another with use of a barrier equipped with a by pass aperture, where the melting section comprises a melting chamber including main melting electrodes and a hopper for introducing fluxing agents; and where the reduction section comprises a reaction chamber into which reaction channels open being directed from mixing chambers; and comprises channels for delivering gaseous titanium-content medium being open into the reaction channels in their upper part and at the same time comprises a funnel chamber delivering the liquid reduction agent being connected with the reaction channels.
  • reaction channels are introduced into the reaction chamber in an upward manner, at an angle and symmetrically one against another, and in a convenient version they decline at an angle of 30-60° with respect to horizontal plane and they have a rectangular section.
  • the melting section is equipped with an outlet pipe designed for releasing vapour and a siphon outlet terminated with a melting pan designed to discharge condensed liquid portion and clinker as by-pass products of the productions.
  • hearth crystallizers arranged at the bottom part of the melting chamber which are equipped with drawing devices intended to catch and pull out cooled titanium ingots, or the melting section can be equipped with a discharging unit connected to the melting chamber through an outlet opening and a siphon outlet comprising auxiliary melting electrodes and opening into a discharging channel.
  • the new invention's efficiency is based on the fact that due to kinetic energy of the high-speed gasflow blown through the reaction channels and reaction chamber the regime of turbulent diffusion arises, which significantly favours practically immediate proceeding of pyrometallurgical reactions taking place at high rates and allowing material to melt quickly, thus the typical weak point of metallurgical equipment (converter, reflex furnaces) mutual interaction between final products and reagents is eliminated.
  • the apparatus has quite a simple design and at the same time it exhibits unusually high manufacturing productivity; another advantage is that all magnesium introduced into the reduction section is almost restlessly utilized.
  • the rate of reactions taking place at high temperatures is controlled through the transport speed regulation which means that speed of introducing reagents into reactor and speed of releasing products from the reaction zone influence the speed of reaction.
  • the reactor comprises a shaped body 1, whose tubular jacket consists of the reduction section 2 and the melting section 3 , which are divided one from another with a barrier 4 equipped with a by pass aperture 41 creating a temperature divide between the two zones, when the temperature in the reduction section 2 amounts to about 650°C and the temperature in the melting section can range from 1500 to 1750°C.
  • the tubular jacket of the body 1 is cooled by a cooling agent; for example a mixture of nitrites and nitrates KNO 3 , NaNO 3 and NaNO 2 , being introduced and drawn off through the cooling pipeline 101 .
  • the reduction section 2 comprises a reaction chamber 21 into which reaction channels 22 open in an upward manner, at an angle and situated symmetrically one against another; the channels for delivering gaseous titanium-content medium 24 , e.g. gaseous TiCl 4 , being open into the reaction channels in their upper part and at the same time the funnel 25 delivering the liquid reduction agent, e.g. magnesium or natrium, equipped with funnel mouthing 26 , being connected with the reaction channels.
  • the reaction channels 22 have longitudinal, preferably rectangular section; they decline at an angle of 30-60° with respect to horizontal plane and they are designed so that optimum operating figures are as follows: - velocity of gasflow in channels 50-300 m/s - specific consumption of refining gas melt 0.5-3 kg/m
  • the melting section 3 comprises the melting chamber 31 , where the sets of main melting electrodes 5 are situated, and which is at its upper part equipped with a charging hopper 32 designed to introduce fluxing agents, for example CaF 2 , and also with purging nozzles 34 designed to introduce and release argon intended for establishing inert atmosphere during melting processes.
  • a charging hopper 32 designed to introduce fluxing agents, for example CaF 2
  • purging nozzles 34 designed to introduce and release argon intended for establishing inert atmosphere during melting processes.
  • hearth crystallizers 33 are arranged which are equipped with drawing devices 6 intended to catch and pull out the cooled titanium ingots.
  • the melting section 3 is further equipped with an outlet pipeline 35 intended to discharge MgCl 2 vapours and sidewardly educed siphon outlet 36 terminated with a pan 37 designed to discharge condensed liquid portion of MgCl 2 and the clinker.
  • the whole reactor Prior to starting manufacturing process the whole reactor is purged with argon; the gas being introduced into the inner space of the reactor through the nozzles 34 until there is no atmosphere containing oxygen present within the reactor.
  • the drawing devices 6 are pulled up into the upper position and the cold titanium ingots 7 are located into the hearth crystallizers 33 as a first charge in order to allow further continuous drawing the titanium ingots 7 out of the melting section 31 during routine operation.
  • the pyrometallurgical reactions are accelerated in the reaction chamber 21 where the gasflows from the reaction channels 22 containing drops of liquid magnesium, remains of gaseous TiCl 4 and titanium particles encounter each other.
  • the velocity is increased due to strong turbulence taking place within the flow of gas and melt, the latter being disaggregated into small drops with size of about 50-400 ⁇ m and foam with active highly developed heterogeneous surface.
  • the solid titanium particles and MgCl 2 melt are discharged from the reaction chamber 21 through the by pass aperture 41 between the dividing barrier 4 and the jacket 1 to the melting section 3 .
  • Approximately half of the MgCl 2 vapour is continuously discharged from the melting chamber 31 through the outlet pipeline 35 and the rest of MgCl 2 condensates and is discharged as a liquid, which means it is casted through the siphon outlet 36 with use of pan 37 .
  • the manufacturing process proceeds in the melting section 3 particularly in the melting chamber 31 into which the solid material intended for melting including fluxing agents, e.g. CaF 2 , is charged through the hopper 32 , and where the main melting electrodes 5 are located.
  • the electrodes 5 are connected to the alternating current supply (not shown in the picture) and dived into the melt of salt MgCl 2 and the clinker.
  • the melt including suspended solid titanium particles is heated up to 1500-1750°C and melted titanium settles down at the bottom part of the melting chamber 31 where it melts on the ingots 7 and after cooling, and depending on the level of solid structure formation, it is discharged from the reactor by the drawing devices 6 and subsequently it is cut by laser cutting tools (not shown in the picture).
  • a protective layer of molten slag 9 consisting of titanium particles, MgCl 2 and titanium chlorides, is formed on the inner surface of the cooled jacket of the melting section 3 and on the cooled barrier 4 .
  • the present layer 9 ensures a long term operation of the reactor without need for special refractory lining.
  • the layer is about 3-50cm thick, 10-20cm on average, depending on the heat flow and heat output of the reactor.
  • the described construction of the reactor is not the only possible technical solution of the invention, but as it is shown on picture 4 , in case periodical or continuous liquid titanium discharge is required, it is possible to replace the hearth crystallizers 33 with a discharging section 8 connected through the outlet opening 38 in the melting section 3 and comprising a siphon discharge 81 in which the auxiliary melting electrodes 82 are located and which opens into the discharging channel 83.
  • the reactor comprising constructional features presented in the invention can be used in metallurgy of nonferrous metals for the purposes of titanium production.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
EP06742216A 2006-02-17 2006-05-15 Reactor intended for titanium production Not-in-force EP1989336B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CZ20060104A CZ300346B6 (cs) 2006-02-17 2006-02-17 Reaktor, zejména pro výrobu titanu
PCT/CZ2006/000032 WO2007093135A1 (en) 2006-02-17 2006-05-15 Reactor primarily intended for titanium production

Publications (2)

Publication Number Publication Date
EP1989336A1 EP1989336A1 (en) 2008-11-12
EP1989336B1 true EP1989336B1 (en) 2011-11-16

Family

ID=37075134

Family Applications (1)

Application Number Title Priority Date Filing Date
EP06742216A Not-in-force EP1989336B1 (en) 2006-02-17 2006-05-15 Reactor intended for titanium production

Country Status (4)

Country Link
EP (1) EP1989336B1 (cs)
AT (1) ATE533868T1 (cs)
CZ (1) CZ300346B6 (cs)
WO (1) WO2007093135A1 (cs)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11150021B2 (en) 2011-04-07 2021-10-19 Ati Properties Llc Systems and methods for casting metallic materials
US9050650B2 (en) 2013-02-05 2015-06-09 Ati Properties, Inc. Tapered hearth

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB814181A (en) * 1955-12-31 1959-06-03 Mini Of Supply Improvements in or relating to the production of titanium
US2816828A (en) * 1956-06-20 1957-12-17 Nat Res Corp Method of producing refractory metals
US3549140A (en) * 1967-06-22 1970-12-22 Dal Y Ingersoll Apparatus for producing titanium and other reactive metals
JPH0747787B2 (ja) * 1989-05-24 1995-05-24 株式会社エヌ・ケイ・アール チタン粉末またはチタン複合粉末の製造方法
JP3821746B2 (ja) * 2002-04-19 2006-09-13 新日本製鐵株式会社 バッチ式のスポンジチタン製造方法
US6824585B2 (en) * 2002-12-03 2004-11-30 Adrian Joseph Low cost high speed titanium and its alloy production

Also Published As

Publication number Publication date
CZ300346B6 (cs) 2009-04-29
ATE533868T1 (de) 2011-12-15
EP1989336A1 (en) 2008-11-12
CZ2006104A3 (cs) 2007-08-29
WO2007093135A1 (en) 2007-08-23

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