EP0947587A1 - Blow lance and process for its cooling - Google Patents

Blow lance and process for its cooling Download PDF

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Publication number
EP0947587A1
EP0947587A1 EP98104153A EP98104153A EP0947587A1 EP 0947587 A1 EP0947587 A1 EP 0947587A1 EP 98104153 A EP98104153 A EP 98104153A EP 98104153 A EP98104153 A EP 98104153A EP 0947587 A1 EP0947587 A1 EP 0947587A1
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EP
European Patent Office
Prior art keywords
lance
melt
gas
cooling
mixing 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.)
Withdrawn
Application number
EP98104153A
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German (de)
French (fr)
Inventor
Volkwin Köster
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.)
Techint Compagnia Tecnica Internazionale SpA
Original Assignee
Volkwin Köster
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 Volkwin Köster filed Critical Volkwin Köster
Priority to EP98104153A priority Critical patent/EP0947587A1/en
Priority to AU27268/99A priority patent/AU2726899A/en
Priority to PT99907572T priority patent/PT1062370E/en
Priority to EP99907572A priority patent/EP1062370B1/en
Priority to BR9908644-1A priority patent/BR9908644A/en
Priority to RU2000123357/02A priority patent/RU2221054C2/en
Priority to ES99907572T priority patent/ES2169599T3/en
Priority to DE59900496T priority patent/DE59900496D1/en
Priority to CA002321651A priority patent/CA2321651C/en
Priority to PCT/EP1999/001255 priority patent/WO1999046412A1/en
Priority to JP2000535778A priority patent/JP4430230B2/en
Priority to AT99907572T priority patent/ATE210195T1/en
Priority to CNB998038229A priority patent/CN1264995C/en
Priority to US09/623,005 priority patent/US6562287B1/en
Priority to KR1020007009862A priority patent/KR100633188B1/en
Publication of EP0947587A1 publication Critical patent/EP0947587A1/en
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • F27D9/00—Cooling of furnaces or of charges therein
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
    • C21C5/28—Manufacture of steel in the converter
    • C21C5/42—Constructional features of converters
    • C21C5/46—Details or accessories
    • C21C5/4606—Lances or injectors
    • 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
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
    • C22B9/103—Methods of introduction of solid or liquid refining or fluxing agents
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
    • C21C5/28—Manufacture of steel in the converter
    • C21C5/42—Constructional features of converters
    • C21C5/46—Details or accessories
    • C21C5/4606—Lances or injectors
    • C21C2005/4626—Means for cooling, e.g. by gases, fluids or liquids

Definitions

  • the invention relates to a method for cooling a Introducing a medium into a melt and / or for measuring lance provided by properties of the melt as well as a lance suitable for performing this procedure.
  • Lances for blowing media in the interior of metallurgical vessels such as Furnaces or converters and as a support for instruments for Measuring properties of the melt are known. you will be For example, to oxygenate a pig iron melt, for Blowing in media during steel treatment (e.g. coal for Foaming of the slag) and for measuring the temperature of the melt used.
  • the invention has for its object a method and to create a lance of the type mentioned in the introduction, the or that enable effective and safe lance cooling.
  • the method according to the invention is characterized in that that in a closed towards the melt-side lance end Cooling circuit a gas / liquid mixture as a cooling medium to be led.
  • the melt-side lance end denotes that end of the Lance that faces the melt during operation or, if applicable, in this dips. It is the thermally highly stressed Lance end.
  • the cooling circuit is for the melt side Lance end closed. There is none in this area Coolant leakage takes place, the coolant is in instead returned to a region of the lance spaced from the melt and exits the lance there.
  • the coolant circuit overall can either be completely closed but you can also use an open cooling circuit which is spaced from the melt-side end the heated cooling medium emerging from the lance is not reused becomes.
  • the gas content of the mixture used according to the invention is preferably air or an inert gas (for example nitrogen or argon), the liquid portion prefers water.
  • the method according to the invention requires considerably for cooling smaller amounts of liquid than that known in the prior art Water cooling.
  • the gas / liquid flow is preferably set so that the liquid content in the area of thermally particularly stressed melt-side lance end largely or completely evaporated. This has two advantages. On the one hand, you don't just use the heat capacity for cooling liquid (water), but also the essential greater heat of vaporization for the phase transition Liquid vapor and maintains even at relatively low Liquid flows have a high cooling capacity.
  • the liquid portion of the invention used cooling medium water. If you choose operating conditions, where the water content in the area of the melt side Part of the lance is largely or completely evaporated the cooling circuit is preferably fed with deionized water, for limescale deposits in the corresponding area of the Avoid cold room. Demineralized water is not available Available and the cooling circuit must be fed with ordinary tap or raw water Gas / liquid flow preferably so that at most a low proportion of water in the area of the melt side Lance end evaporates. Unwanted limescale deposits will be so largely avoided.
  • the gas / liquid mixture can be produced outside the lance and are already supplied as a mixture to the lance.
  • the lance has a mixing chamber connected to the cooling circuit, has the connections for a gas and liquid supply and designed to produce a gas / liquid mixture is.
  • the mixing chamber is preferably spaced from the melt side Lance end arranged. It is preferred in the part of the protruding from the furnace or converter Lance.
  • the gas / liquid mixture is preferred by the mixing chamber with a pressure of 2 to 6 bar, more preferably about 4 bar, through a pressure line to the melt-side lance end led out.
  • a two-component nozzle arranged, from which the mixture in one In the area of the lance tip, the cooling chamber is relaxed.
  • That relaxed and warmed Mixture is through a second line from the melt side Lance end led away and occurs preferentially at one connection from the lance arranged outside the converter out again.
  • the pressure of the mixture after exiting the or the two-component nozzles is preferably slightly above atmospheric pressure.
  • the lance is used in diving operation it should be greater than the back pressure of the lance tip surrounding liquid melt. It comes because of from malfunctions to melting of the lance tip and melt breakthrough into the cold room the overpressure prevailing in it the further penetration of Melt or possibly slag.
  • the mixing chamber advantageously has two concentric, the lance tube surrounding ring chambers in their radial partition connecting holes or openings are arranged.
  • lance tube means that for the introduction of gas and / or solid into the melt provided inner tube of the entire lance assembly.
  • the inner one The annular chamber can, for example, with water from its end face are applied, the outer annular chamber becomes circumferential pressurized with compressed air. Through the holes in the radial partition, compressed air is mixed into the water. The resulting mixture is on the melt side end removed and removed from the mixing chamber.
  • the pressure line for connecting the mixing chambers and the two-fluid nozzle the lance tube is preferably concentric surrounding ring line.
  • the return of the relaxed mixture preferably takes place from the melt-side lance end also through a ring line, which as a the pressure line concentrically surrounding second ring line is formed can be.
  • a preferred field of application of the invention is treatment of or performing measurements on metallurgical Melting, e.g. pig iron or steel melting.
  • metallurgical Melting e.g. pig iron or steel melting.
  • the invention is not for use in molten metals limited, but can be used for further melt flows high temperature (e.g. glass melting) can be used.
  • the lance according to the invention has an inner lance tube 1 on, through the solids and / or gases supplied to the melt become. These media escape into the melt at the melt end of the lance 2.
  • the lance tube 1 is surrounded by a cooling device described in more detail below.
  • connection piece 3 cooling water is the lance tube 1 surrounding annular chamber 4 supplied.
  • the inner annular chamber 5 is from an outer one Annular chamber 6 surrounded by a connector 7 with Compressed air is fed. Form the two annular chambers 5,6 together the mixing chamber.
  • the radial partition 8 between the annular chambers 5 and 6 have connection holes indicated at 9 on. Compressed air and water mix together, the mixture is drawn axially into the interior Annular chamber 5 connecting ring line (pressure line) 10 to Lance end on the melt side.
  • the pressure of the mixture in the pressure line 10 is approximately 4 bar.
  • the ring line 10 is in the region of the melt-side end 2 of the lance to six evenly over the lance circumference distributed two-component nozzles 11 formed.
  • the water / air mixture relaxes when exiting the two-component nozzles into the annular cooling space 12.
  • the water is through this relaxation process torn into very fine droplets.
  • the high surface of the water supplied favors one rapid heat absorption and thus a high cooling capacity.
  • the Forming the ring line 10 to six two-component nozzles 11 allowed the operation of the lance with tap or process water as part of the cooling medium.
  • the clear width of the two-substance nozzles 11 enables the passage of, if necessary, in the process water contained impurities or particles.
  • the lance should only be operated with deionized water can, the ring line 10 in the area of the cooling chamber the cooling chamber 12 to an annular gap with a clear Width of about 0.5 mm can be narrowed, making the lance tube 1 rotationally symmetrical surrounds.
  • This annular gap forms a single one Dual-substance nozzle.
  • the formation of several discrete two-component nozzles 11 is not required in this case.
  • the mixture emerging from the two-substance nozzles 11 hits on opposite (melt-side) end of the cooling chamber 12 on a curved cooling surface 13 through which it is in its Direction of movement deflected and the second ring line 14 trained coolant discharge line is supplied.
  • the water content of the supplied mixture evaporates in the Cooling chamber 12 preferably completely. It comes with special Operating conditions at exceptionally high temperatures in the cooling chamber 12, the cooling effect may supported are caused by the strongly endothermic decay of part of the Water in molecular hydrogen and oxygen.
  • the cooling chamber 12 to Melt opens out due to the use of the fine Aerosols as a cooling medium practically no danger that yet liquid water is enclosed by the melt and then evaporated explosively.
  • the cold room 12 preferably set an overpressure sufficient to Diving operation of the lance possibly into the cooling chamber 12 to push back through molten metal or slag and prevent further intrusion.
  • the cooling medium flowing back through the ring line 14 becomes via an annular chamber 15 and a connecting piece 16 from the Lance removed. It can either be rejected (more open Cooling circuit) or returned to the cooling circuit again become.
  • the annular chamber 15 has a second connection 17 which with a safety pressure relief valve, not shown in the drawing connected is.
  • the lance can also be used to introduce media into the melt also used to measure properties of the melt become.
  • the melt side End 2 measuring instruments not shown in the drawing to be ordered.
  • a radiation pyrometer can For example, the temperature of the melt can be measured.
  • a Steel melt can, for example, by means of laser-induced emission spectroscopy a multi-element analysis can be carried out. In this way, for example, a steel finishing process can be measured be followed and ended at the desired stage.
  • the lance with the attached measuring instrument in the area of the surface of the steel bath.
  • Blown compressed air or an inert gas such as nitrogen Blown compressed air or an inert gas such as nitrogen, which on the one hand keeps the lance opening free and on the other hand removes slag from the steel bath surface.
  • the lance according to the invention is through an opening in the wall or cover inserted into the converter or furnace.
  • the connections for supply and discharge of the cooling media and the mixing chamber are preferably located outside of the converter in a correspondingly cooler area.

Abstract

The invention relates to a method for cooling a lance provided for converting a medium into a molten mass and/or for measuring the properties of the molten mass. A gas/liquid mixture is fed as a cooling medium into a cooling circuit which is closed up to the lance end (2) situated on the melting side. The invention provides that the gas/liquid mixture or the components thereof is/are fed and permitted to expand under pressure up to the area of the lance end (2) situated on the melting side. The invention also relates to a lance which has a mixing chamber (5, 6) connected to the cooling circuit. The mixing chamber has the connections (3, 7) for a gas and liquid supply which is designed to produce the gas/liquid mixture, whereby the mixing chamber (5, 6) is connected via a pressure line (10) to at least one two-component nozzle (11) arranged in the area of the lance end (2) which is situated on the melting side.

Description

Die Erfindung betrifft ein Verfahren zum Kühlen einer zum Einbringen eines Mediums in eine Schmelze und/oder zum Messen von Eigenschaften der Schmelze vorgesehenen Lanze sowie eine zum Durchführen dieses Verfahrens geeignete Lanze.The invention relates to a method for cooling a Introducing a medium into a melt and / or for measuring lance provided by properties of the melt as well as a lance suitable for performing this procedure.

Lanzen zum Einblasen von Medien (insbesondere Feststoffen und/oder Gasen) in den Innenraum metallurgischer Gefäße wie Öfen oder Konverter sowie als Träger von Instrumenten zum Messen von Eigenschaften der Schmelze sind bekannt. Sie werden bspw. zum Sauerstofffrischen einer Roheisenschmelze, zum Einblasen von Medien bei der Stahlbehandlung (bspw. Kohle zum Schäumen der Schlacke) und zur Temperaturmessung der Schmelze verwendet.Lances for blowing media (especially solids and / or gases) in the interior of metallurgical vessels such as Furnaces or converters and as a support for instruments for Measuring properties of the melt are known. you will be For example, to oxygenate a pig iron melt, for Blowing in media during steel treatment (e.g. coal for Foaming of the slag) and for measuring the temperature of the melt used.

Der der Schmelze zugewandte Endbereich einer solchen Lanze unterliegt einer hohen thermischen Beanspruchung. Aus offenkundiger Vorbenutzung ist es bekannt, Stahlrohrlanzen zu verwenden, deren schmelzeseitiges Ende im Betrieb kontinuierlich abbrennt, die Lanze muß entsprechend nachgefahren werden. Bekannt sind ferner gekühlte Lanzen mit geschlossenen Wasserkühlkreisläufen. Der Betrieb dieser Lanzen ist gefährlich, da bei einem Leck im Kühlkreislauf ein Kontakt der Schmelze mit Kühlwasser zu explosionsartigen Reaktionen führen kann. Sofern Wasser von der Schmelze eingeschlossen wird, kann die dann erfolgende Verdampfung und Expansion des Wassers die Schmelze explosionsartig auseinander reißen. Auch die chemische Zersetzung des Wassers und eine anschließende Knallgasreaktion sind nicht auszuschließen.The end region of such a lance facing the melt is subject to high thermal stress. Obviously Prior use, it is known to use tubular steel lances their melt-side end in operation continuously burns, the lance must be moved accordingly. Known are also cooled lances with closed water cooling circuits. The operation of these lances is dangerous because in the event of a leak in the cooling circuit, contact of the melt with Cooling water can lead to explosive reactions. Provided Water can be trapped by the melt then the water evaporates and expands Tear the melt apart explosively. Even the chemical one Decomposition of the water and a subsequent detonating gas reaction cannot be ruled out.

Es ist daher bereits vorgeschlagen worden (DE 35 43 836 C2), zwei Lanzen zu verwenden, die wechselweise in die Betriebsstellung gefahren werden. Die in der Betriebsstellung befindliche Lanze wird mit einem Gas gekühlt. Da eine ausreichende Kühlwirkung so nicht erzielt wird, wird die Lanze nach einer gewissen Betriebszeit aus dem Ofen herausgefahren und in dieser von der Schmelze weit beabstandeten Stellung mit Wasser rückgekühlt. Während dieser Zeit führt die zweite Lanze den Betrieb weiter. Ein solcher wechselweiser Betrieb mit zwei Lanzen ist aufwendig.It has therefore already been proposed (DE 35 43 836 C2) to use two lances, which alternately in the operating position be driven. The one in the operating position The lance is cooled with a gas. Because a sufficient If the cooling effect is not achieved, the lance will certain operating time out of the oven and in this position far away from the melt with water recooled. During this time the second lance carries the Operation continues. Such an alternate operation with two Lances are expensive.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren und eine Lanze der eingangs genannten Art zu schaffen, das bzw. die eine wirksame und sichere Lanzenkühlung ermöglichen.The invention has for its object a method and to create a lance of the type mentioned in the introduction, the or that enable effective and safe lance cooling.

Das erfindungsgemäße Verfahren ist dadurch gekennzeichnet, daß in einem zum schmelzeseitigen Lanzenende hin geschlossenen Kühlkreislauf ein Gas/Flüssigkeitsgemisch als Kühlmedium geführt wird.The method according to the invention is characterized in that that in a closed towards the melt-side lance end Cooling circuit a gas / liquid mixture as a cooling medium to be led.

Das schmelzeseitige Lanzenende bezeichnet dasjenige Ende der Lanze, das im Betrieb der Schmelze zugewandt ist bzw. ggf. in diese eintaucht. Es handelt sich um das thermisch hochbelastete Lanzenende. Der Kühlkreislauf ist zum schmelzeseitigen Lanzenende hin geschlossen. Es findet in diesem Bereich kein Kühlmittelaustritt statt, das Kühlmittel wird statt dessen in einem von der Schmelze beabstandeten Bereich der Lanze zurückgeführt und tritt dort aus der Lanze aus. Der Kühlmittelkreislauf insgesamt kann entweder vollständig geschlossen sein, man kann jedoch auch einen offenen Kühlkreislauf verwenden, bei dem das beabstandet vom schmelzeseitigen Ende aus der Lanze austretende erwärmte Kühlmedium nicht wiederverwendet wird.The melt-side lance end denotes that end of the Lance that faces the melt during operation or, if applicable, in this dips. It is the thermally highly stressed Lance end. The cooling circuit is for the melt side Lance end closed. There is none in this area Coolant leakage takes place, the coolant is in instead returned to a region of the lance spaced from the melt and exits the lance there. The coolant circuit overall can either be completely closed but you can also use an open cooling circuit which is spaced from the melt-side end the heated cooling medium emerging from the lance is not reused becomes.

Der Gasanteil des erfindungsgemäß verwendeten Gemischs ist bevorzugt Luft oder ein Inertgas (bspw. Stickstoff oder Argon), der Flüssigkeitsanteil bevorzugt Wasser.The gas content of the mixture used according to the invention is preferably air or an inert gas (for example nitrogen or argon), the liquid portion prefers water.

Das erfindungsgemäße Verfahren benötigt zum Kühlen erheblich geringere Flüssigkeitsmengen als die im Stand der Technik bekannte Wasserkühlung. Bevorzugt stellt man den Gas/Flüssigkeitsstrom so ein, daß der Flüssigkeitsanteil im Bereich des thermisch besonders belasteten schmelzeseitigen Lanzenendes großenteils oder vollständig verdampft. Dies hat zwei Vorteile. Zum einen nutzt man zur Kühlung so nicht nur die Wärmekapazität der Flüssigkeit (des Wassers), sondern auch die wesentlich größere Verdampfungswärme für den Phasenübergang Flüssigkeit-Dampf und erhält selbst bei verhältnismäßig geringen Flüssigkeitsströmen eine hohe Kühlleistung. Sofern es bei Betriebsstörungen im Bereich des schmelzeseitigen Endes zu einem Leck in der Kühlmittelleitung kommt, bewirkt die große Oberfläche des als Aerosol zugeführten Gas/Flüssigkeitsgemischs, daß es in jedem Fall zu einer sehr schnellen Verdampfung des Flüssigkeitsanteils kommt, noch bevor die Schmelze Flüssigkeitstropfen einschließen kann.The method according to the invention requires considerably for cooling smaller amounts of liquid than that known in the prior art Water cooling. The gas / liquid flow is preferably set so that the liquid content in the area of thermally particularly stressed melt-side lance end largely or completely evaporated. This has two advantages. On the one hand, you don't just use the heat capacity for cooling liquid (water), but also the essential greater heat of vaporization for the phase transition Liquid vapor and maintains even at relatively low Liquid flows have a high cooling capacity. Unless it is in the event of malfunctions in the area of the melt-side end If there is a leak in the coolant line, it causes large surface area of the gas / liquid mixture supplied as an aerosol, that in any case it is very quick Evaporation of the liquid portion comes before the Melt can include liquid drops.

In der Regel ist der Flüssigkeitsanteil des erfindungsgemäß verwendeten Kühlmediums Wasser. Wählt man Betriebsbedingungen, bei denen der Wasseranteil im Bereich des schmelzeseitigen Lanzenteils großenteils oder vollständig verdampft, wird der Kühlkreislauf vorzugsweise mit vollentsalztem Wasser gespeist, um Kalkablagerungen in dem entsprechenden Bereich des Kühlraums zu vermeiden. Steht vollentsalztes Wasser nicht zur Verfügung und muß der Kühlkreislauf mit gewöhnlichem Leitungs- oder Rohwasser gespeist werden, stellt man den Gas/Flüssigkeitsstrom vorzugsweise so ein, daß allenfalls ein geringer Anteil des Wassers im Bereich des schmelzeseitigen Lanzenendes verdampft. Unerwünschte Kalkablagerungen werden so weitgehend vermieden.As a rule, the liquid portion of the invention used cooling medium water. If you choose operating conditions, where the water content in the area of the melt side Part of the lance is largely or completely evaporated the cooling circuit is preferably fed with deionized water, for limescale deposits in the corresponding area of the Avoid cold room. Demineralized water is not available Available and the cooling circuit must be fed with ordinary tap or raw water Gas / liquid flow preferably so that at most a low proportion of water in the area of the melt side Lance end evaporates. Unwanted limescale deposits will be so largely avoided.

Das Gas/Flüssigkeitsgemisch kann außerhalb der Lanze hergestellt und bereits als Gemisch der Lanze zugeführt werden. Bevorzugt ist im Rahmen der Erfindung jedoch, daß die Lanze eine mit dem Kühlkreislauf verbundene Mischkammer aufweist, die Anschlüsse für eine Gas- und Flüssigkeitszufuhr besitzt und zum Herstellen eines Gas/Flüssigkeitsgemischs ausgebildet ist. Die Mischkammer ist bevorzugt beabstandet vom schmelzeseitigen Lanzenende angeordnet. Sie befindet sich bevorzugt in dem aus dem Ofen bzw. Konverter herausragenden Teil der Lanze.The gas / liquid mixture can be produced outside the lance and are already supplied as a mixture to the lance. However, it is preferred in the context of the invention that the lance has a mixing chamber connected to the cooling circuit, has the connections for a gas and liquid supply and designed to produce a gas / liquid mixture is. The mixing chamber is preferably spaced from the melt side Lance end arranged. It is preferred in the part of the protruding from the furnace or converter Lance.

Das Gas/Flüssigkeitsgemisch wird von der Mischkammer bevorzugt mit einem Druck von 2 bis 6 bar, weiter vorzugsweise etwa 4 bar, durch eine Druckleitung zum schmelzeseitigen Lanzenende hin geführt. Im Bereich dieses Endes ist bevorzugt eine Zweistoffdüse angeordnet, aus der das Gemisch in einen im Bereich der Lanzenspitze angeordneten Kühlraum entspannt. Bei Austritt aus der Düse wird der Flüssigkeitsanteil des Gemischs in feine Tröpfchen zerrissen. Das entspannte und erwärmte Gemisch wird durch eine zweite Leitung vom schmelzeseitigen Lanzenende weggeführt und tritt an einem bevorzugt außerhalb des Konverters angeordneten Anschluß aus der Lanze wieder aus. Der Druck des Gemischs nach dem Austritt aus der bzw. den Zweistoffdüsen liegt bevorzugt etwas über dem Atmosphärendruck. Sofern die Lanze im Tauchbetrieb eingesetzt wird, sollte er größer sein, als der Gegendruck der die Lanzenspitze umgebenden flüssigen Schmelze. Kommt es aufgrund von Betriebsstörungen zu einem Abschmelzen der Lanzenspitze und einem Durchbruch von Schmelze in den Kühlraum, verhindert der darin herrschende Überdruck das weitere Eindringen von Schmelze bzw. ggf. Schlacke.The gas / liquid mixture is preferred by the mixing chamber with a pressure of 2 to 6 bar, more preferably about 4 bar, through a pressure line to the melt-side lance end led out. In the area of this end is preferred a two-component nozzle arranged, from which the mixture in one In the area of the lance tip, the cooling chamber is relaxed. As it emerges from the nozzle, the liquid portion of the mixture torn into fine droplets. That relaxed and warmed Mixture is through a second line from the melt side Lance end led away and occurs preferentially at one connection from the lance arranged outside the converter out again. The pressure of the mixture after exiting the or the two-component nozzles is preferably slightly above atmospheric pressure. If the lance is used in diving operation it should be greater than the back pressure of the lance tip surrounding liquid melt. It comes because of from malfunctions to melting of the lance tip and melt breakthrough into the cold room the overpressure prevailing in it the further penetration of Melt or possibly slag.

Die Mischkammer weist vorteilhafterweise zwei zueinander konzentrische, das Lanzenrohr umgebende Ringkammern auf, in deren radialer Trennwand Verbindungsbohrungen bzw. -öffnungen angeordnet sind. Der Begriff Lanzenrohr bezeichnet das für die Einleitung von Gas und/oder Feststoff in die Schmelze vorgesehene innere Rohr der gesamten Lanzenanordnung. Die innere Ringkammer kann bspw. von ihrer Stirnseite her mit Wasser beaufschlagt werden, die äußere Ringkammer wird umfangsseitig mit Druckluft beaufschlagt. Durch die Bohrungen in der radialen Trennwand wird Druckluft in das Wasser eingemischt. Das entstandene Gemisch wird an der schmelzeseitigen Stirnseite der Mischkammer entnommen und abgeführt.The mixing chamber advantageously has two concentric, the lance tube surrounding ring chambers in their radial partition connecting holes or openings are arranged. The term lance tube means that for the introduction of gas and / or solid into the melt provided inner tube of the entire lance assembly. The inner one The annular chamber can, for example, with water from its end face are applied, the outer annular chamber becomes circumferential pressurized with compressed air. Through the holes in the radial partition, compressed air is mixed into the water. The resulting mixture is on the melt side end removed and removed from the mixing chamber.

Die Druckleitung zur Verbindung von Mischkammern und Zweistoffdüse ist vorzugsweise eine das Lanzenrohr konzentrisch umgebende Ringleitung. Die Rückführung des entspannten Gemischs vom schmelzeseitigen Lanzenende erfolgt vorzugsweise ebenfalls durch eine Ringleitung, die als eine die Druckleitung konzentrisch umgebende zweite Ringleitung ausgebildet sein kann. The pressure line for connecting the mixing chambers and the two-fluid nozzle the lance tube is preferably concentric surrounding ring line. The return of the relaxed mixture preferably takes place from the melt-side lance end also through a ring line, which as a the pressure line concentrically surrounding second ring line is formed can be.

Ein bevorzugtes Anwendungsgebiet der Erfindung ist die Behandlung von bzw. die Durchführung von Messungen an metallurgischen Schmelzen, bspw. Roheisen oder Stahlschmelzen. Die Erfindung ist jedoch nicht auf die Anwendung bei Metallschmelzen beschränkt, sondern kann für weitere Schmelzflüsse hoher Temperatur (bspw. Glasschmelzen) verwendet werden.A preferred field of application of the invention is treatment of or performing measurements on metallurgical Melting, e.g. pig iron or steel melting. The However, the invention is not for use in molten metals limited, but can be used for further melt flows high temperature (e.g. glass melting) can be used.

Ein Ausführungsbeispiel der Erfindung wird im folgenden anhand der Zeichnung erläutert. Darin zeigen:

Fig. 1
einen Längsschnitt durch eine erfindungsgemäße Lanze;
Fig. 2
einen Querschnitt entlang der Ebene A-A der Fig. 1
An embodiment of the invention is explained below with reference to the drawing. In it show:
Fig. 1
a longitudinal section through a lance according to the invention;
Fig. 2
2 shows a cross section along the plane AA of FIG. 1

Die erfindungsgemäße Lanze weist ein inneres Lanzenrohr 1 auf, durch das Feststoffe und/oder Gase der Schmelze zugeführt werden. Der Austritt dieser Medien in die Schmelze erfolgt am schmelzeseitigen Lanzenende 2. Das Lanzenrohr 1 ist von einer nachfolgend näher beschriebenen Kühleinrichtung umgeben.The lance according to the invention has an inner lance tube 1 on, through the solids and / or gases supplied to the melt become. These media escape into the melt at the melt end of the lance 2. The lance tube 1 is surrounded by a cooling device described in more detail below.

Durch einen Anschlußstutzen 3 wird Kühlwasser einer das Lanzenrohr 1 umgebenden Ringkammer 4 zugeführt. Die Stirnseiten der Ringkammer 4 und der inneren Kammer 5 der sich axial anschließenden Mischkammer sind miteinander verbunden, so daß diese innere Ringkammer 5 aus der Ringkammer 4 mit Wasser gespeist wird. Die innere Ringkammer 5 ist von einer äußeren Ringkammer 6 umgeben, die durch einen Anschlußstutzen 7 mit Druckluft gespeist wird. Die beiden Ringkammern 5,6 bilden zusammen die Mischkammer. Die radiale Trennwand 8 zwischen den Ringkammern 5 und 6 weist bei 9 angedeutete Verbindungsbohrungen auf. Druckluft und Wasser vermischen sich miteinander, das Gemisch wird durch die sich axial in die innere Ringkammer 5 anschließende Ringleitung (Druckleitung) 10 zum schmelzeseitigen Lanzenende hin geführt. Der Druck des Gemisches in der Druckleitung 10 beträgt etwa 4 bar.Through a connection piece 3 cooling water is the lance tube 1 surrounding annular chamber 4 supplied. The end faces the annular chamber 4 and the inner chamber 5 of the axially adjoining Mixing chamber are connected to each other so that this inner annular chamber 5 fed from the annular chamber 4 with water becomes. The inner annular chamber 5 is from an outer one Annular chamber 6 surrounded by a connector 7 with Compressed air is fed. Form the two annular chambers 5,6 together the mixing chamber. The radial partition 8 between the annular chambers 5 and 6 have connection holes indicated at 9 on. Compressed air and water mix together, the mixture is drawn axially into the interior Annular chamber 5 connecting ring line (pressure line) 10 to Lance end on the melt side. The pressure of the mixture in the pressure line 10 is approximately 4 bar.

Die Ringleitung 10 ist im Bereich des schmelzeseitigen Endes 2 der Lanze zu sechs gleichmäßig über den Lanzenumfang verteilten Zweistoffdüsen 11 ausgeformt. Das Wasser/Luftgemisch entspannt sich beim Austritt aus den Zweistoffdüsen in den ringförmigen Kühlraum 12 hinein. Das Wasser wird durch diesen Entspannungsvorgang in sehr feine Tröpfchen zerrissen. Die hohe Oberfläche des zugeführten Wassers begünstigt eine schnelle Wärmeaufnahme und damit eine hohe Kühlleistung. Die Ausformung der Ringleitung 10 zu sechs Zweistoffdüsen 11 erlaubt den Betrieb der Lanze mit Leitungs- bzw. Betriebswasser als Bestandteil des Kühlmediums. Die lichte Weite der Zweistoffdüsen 11 ermöglicht den Durchtritt von ggf. in dem Betriebswasser enthaltenen Verunreinigungen bzw. Partikeln. Soll die Lanze ausschließlich mit vollentsalztem Wasser betrieben werden, kann die Ringleitung 10 im Bereich der Kühlkammer des Kühlraums 12 zu einem Ringspalt mit einer lichten Weite von etwa 0,5 mm verengt sein, der das Lanzenrohr 1 rotationssymmetrisch umgibt. Dieser Ringspalt bildet eine einzige Zweistoffdüse. Die Ausformung mehrerer diskreter Zweistoffdüsen 11 ist in diesem Fall nicht erforderlich.The ring line 10 is in the region of the melt-side end 2 of the lance to six evenly over the lance circumference distributed two-component nozzles 11 formed. The water / air mixture relaxes when exiting the two-component nozzles into the annular cooling space 12. The water is through this relaxation process torn into very fine droplets. The high surface of the water supplied favors one rapid heat absorption and thus a high cooling capacity. The Forming the ring line 10 to six two-component nozzles 11 allowed the operation of the lance with tap or process water as part of the cooling medium. The clear width of the two-substance nozzles 11 enables the passage of, if necessary, in the process water contained impurities or particles. The lance should only be operated with deionized water can, the ring line 10 in the area of the cooling chamber the cooling chamber 12 to an annular gap with a clear Width of about 0.5 mm can be narrowed, making the lance tube 1 rotationally symmetrical surrounds. This annular gap forms a single one Dual-substance nozzle. The formation of several discrete two-component nozzles 11 is not required in this case.

Das aus den Zweistoffdüsen 11 austretende Gemisch trifft am gegenüberliegenden (schmelzeseitigen) Stirnende der Kühlkammer 12 auf eine gekrümmte Kühlfläche 13, durch die es in seiner Bewegungsrichtung umgelenkt und der als zweite Ringleitung 14 ausgebildeten Kühlmittelabfuhrleitung zugeführt wird. Der Wasseranteil des zugeführten Gemischs verdampft in der Kühlkammer 12 vorzugsweise vollständig. Kommt es bei besonderen Betriebsbedingungen zu außergewöhnlich hohen Temperaturen in der Kühlkammer 12, kann die Kühlwirkung u.U. unterstützt werden durch den stark endothermen Zerfall eines Teils des Wassers in molekularen Wasserstoff und Sauerstoff.The mixture emerging from the two-substance nozzles 11 hits on opposite (melt-side) end of the cooling chamber 12 on a curved cooling surface 13 through which it is in its Direction of movement deflected and the second ring line 14 trained coolant discharge line is supplied. The water content of the supplied mixture evaporates in the Cooling chamber 12 preferably completely. It comes with special Operating conditions at exceptionally high temperatures in the cooling chamber 12, the cooling effect may supported are caused by the strongly endothermic decay of part of the Water in molecular hydrogen and oxygen.

Sofern bei Betriebsstörungen die Lanze im Bereich des schmelzeseitigen Endes 2 abbrennt und sich die Kühlkammer 12 zur Schmelze hin öffnet, besteht aufgrund der Verwendung des feinen Aerosols als Kühlmedium praktisch keine Gefahr, daß noch flüssiges Wasser von der Schmelze eingeschlossen wird und anschließend explosionsartig verdampft. Im Kühlraum 12 wird vorzugsweise ein Überdruck eingestellt, der ausreicht, um bei Tauchbetrieb der Lanze möglicherweise in die Kühlkammer 12 durchbrechende Metallschmelze oder Schlacke zurückzudrängen und ein weiteres Eindringen zu verhindern.If the lance is in the area of the melt side in the event of malfunctions End 2 burns and the cooling chamber 12 to Melt opens out due to the use of the fine Aerosols as a cooling medium practically no danger that yet liquid water is enclosed by the melt and then evaporated explosively. In the cold room 12 preferably set an overpressure sufficient to Diving operation of the lance possibly into the cooling chamber 12 to push back through molten metal or slag and prevent further intrusion.

Das durch die Ringleitung 14 zurückströmende Kühlmedium wird über eine Ringkammer 15 und einen Anschlußstutzen 16 aus der Lanze abgeführt. Es kann entweder verworfen werden (offener Kühlkreislauf) oder aber von neuem in den Kühlkreislauf zurückgeführt werden.The cooling medium flowing back through the ring line 14 becomes via an annular chamber 15 and a connecting piece 16 from the Lance removed. It can either be rejected (more open Cooling circuit) or returned to the cooling circuit again become.

Die Ringkammer 15 weist einen zweiten Anschluß 17 auf, der mit einem in der Zeichnung nicht dargestellten Sicherheits-Überdruckventil verbunden ist.The annular chamber 15 has a second connection 17 which with a safety pressure relief valve, not shown in the drawing connected is.

Die Lanze kann außer zum Einbringen von Medien in die Schmelze auch zum Messen von Eigenschaften der Schmelze verwendet werden. Zu diesem Zweck können im Bereich des schmelzeseitigen Endes 2 in der Zeichnung nicht dargestellte Meßinstrumente angeordnet werden. Mit einem Strahlungspyrometer kann bspw. die Temperatur der Schmelze gemessen werden. Bei einer Stahlschmelze kann bspw. mittels laserinduzierter Emissionsspektroskopie eine Multielementanalyse durchgeführt werden. Auf diese Weise kann bspw. ein Stahlveredelungsprozeß meßtechnisch verfolgt und im gewünschten Stadium beendet werden.The lance can also be used to introduce media into the melt also used to measure properties of the melt become. For this purpose, the melt side End 2 measuring instruments not shown in the drawing to be ordered. With a radiation pyrometer can For example, the temperature of the melt can be measured. At a Steel melt can, for example, by means of laser-induced emission spectroscopy a multi-element analysis can be carried out. In this way, for example, a steel finishing process can be measured be followed and ended at the desired stage.

Zur Durchführung solcher Messungen wird die Lanze mit dem daran angeordneten Meßinstrument in den Bereich der Oberfläche des Stahlbads geführt. Durch das Lanzenrohr 1 wird vorzugsweise Druckluft oder ein Inertgas wie Stickstoff geblasen, das zum einen die Lanzenöffnung freihält und zum anderen die Stahlbadoberfläche von Schlacke befreit.To carry out such measurements, the lance with the attached measuring instrument in the area of the surface of the steel bath. Through the lance tube 1 is preferred Blown compressed air or an inert gas such as nitrogen, which on the one hand keeps the lance opening free and on the other hand removes slag from the steel bath surface.

Die erfindungsgemäße Lanze wird durch eine Öffnung in Wand oder Deckel in den Konverter bzw. Ofen eingeführt. Die Anschlüsse für Zu- und Abfuhr der Kühlmedien sowie die Mischkammer befinden sich vorzugsweise außerhalb des Konverters in einem entsprechend kühleren Bereich.The lance according to the invention is through an opening in the wall or cover inserted into the converter or furnace. The connections for supply and discharge of the cooling media and the mixing chamber are preferably located outside of the converter in a correspondingly cooler area.

Claims (10)

Verfahren zum Kühlen einer zum Einbringen eines Mediums in eine Schmelze und/oder zum Messen von Eigenschaften der Schmelze vorgesehenen Lanze, dadurch gekennzeichnet, daß in einem zum schmelzeseitigen Lanzenende (2) hin geschlossenen Kühlkreislauf ein Gas/Flüssigkeitsgemisch als Kühlmedium geführt wird.Method for cooling one for introducing a medium into a melt and / or for measuring properties the lance provided for the melt, characterized in that that in a closed towards the melt-side lance end (2) Cooling circuit as a gas / liquid mixture Coolant is led. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß das Gas/Flüssigkeitsgemisch in einer vom schmelzeseitigen Lanzenende (2) beabstandet angeordneten Mischkammer (5,6) der Lanze hergestellt wird.A method according to claim 1, characterized in that the gas / liquid mixture in one from the melt side Lance end (2) spaced mixing chamber (5,6) the lance is made. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das Gas/Flüssigkeitsgemisch unter Druck bis in den Bereich des schmelzeseitigen Lanzenendes (2) geführt und dort entspannen gelassen wird.A method according to claim 1 or 2, characterized in that that the gas / liquid mixture under pressure into the Area of the melt-side lance end (2) guided and is left there to relax. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß das Gas/Flüssigkeitsgemisch unter einem Druck von 2 bis 6 bar, vorzugsweise etwa 4 bar zum schmelzeseitigen Lanzenende (2) geführt wird.A method according to claim 3, characterized in that the gas / liquid mixture under a pressure of 2 to 6 bar, preferably about 4 bar to the melt end of the lance (2) is performed. Lanze zum Durchführen des Verfahrens nach einem der Ansprüche 1 bis 4, mit einem zum schmelzeseitigen Lanzenende (2) hin geschlossenen Kühlkreislauf, gekennzeichnet durch eine mit dem Kühlkreislauf verbundene Mischkammer (5,6), die Anschlüsse (3,7) für eine Gas- und Flüssigkeitszufuhr aufweist und zum Herstellen eines Gas/Flüssigkeitsgemisches ausgebildet ist.Lance for performing the method according to one of the claims 1 to 4, with one to the melt-side lance end (2) closed cooling circuit, marked through a mixing chamber connected to the cooling circuit (5,6), the connections (3,7) for a gas and liquid supply has and for producing a gas / liquid mixture is trained. Lanze nach Anspruch 5, dadurch gekennzeichnet, daß die Mischkammer (5,6) beabstandet vom schmelzeseitigen Lanzenende (2) angeordnet ist.Lance according to claim 5, characterized in that the Mixing chamber (5,6) spaced from the melt-side lance end (2) is arranged. Lanze nach Anspruch 5 oder 6, dadurch gekennzeichnet, daß die Mischkammer (5,6) zwei zueinander konzentrische, das Lanzenrohr umgebende Ringkammern (5,6) aufweist, in deren radialer Trennwand (8) Verbindungsbohrungen (9) angeordnet sind.Lance according to claim 5 or 6, characterized in that the mixing chamber (5,6) two concentric to each other, that Lance tube surrounding ring chambers (5,6), in their radial partition (8) connecting holes (9) arranged are. Lanze nach einem der Ansprüche 5 bis 7, dadurch gekennzeichnet, daß die Mischkammer (5,6) über eine Druckleitung (10) mit wenigstens einer im Bereich des schmelzeseitigen Endes (2) der Lanze angeordneten Zweistoffdüse (11) verbunden ist.Lance according to one of claims 5 to 7, characterized in that that the mixing chamber (5,6) via a pressure line (10) with at least one in the area of the melt side End (2) of the lance arranged two-fluid nozzle (11) is connected. Lanze nach Anspruch 8, dadurch gekennzeichnet, daß die Druckleitung eine das Lanzenrohr konzentrisch umgebende Ringleitung (10) ist.Lance according to claim 8, characterized in that the Pressure line concentrically surrounding the lance tube Ring line (10) is. Lanze nach Anspruch 9, dadurch gekennzeichnet, daß zur Rückführung des entspannten Gas/Flüssigkeitsgemischs vom schmelzeseitigen Lanzenende (2) zum Auslaß (16) des Gemischs aus der Lanze eine die Druckleitung (10) konzentrisch umgebende zweite Ringleitung (14) vorgesehen ist.Lance according to claim 9, characterized in that for Return of the expanded gas / liquid mixture from Lance end (2) on the melt side to the outlet (16) of the mixture from the lance the pressure line (10) concentric surrounding second ring line (14) is provided.
EP98104153A 1998-03-09 1998-03-09 Blow lance and process for its cooling Withdrawn EP0947587A1 (en)

Priority Applications (15)

Application Number Priority Date Filing Date Title
EP98104153A EP0947587A1 (en) 1998-03-09 1998-03-09 Blow lance and process for its cooling
AU27268/99A AU2726899A (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof
PT99907572T PT1062370E (en) 1998-03-09 1999-02-26 LUG TO INSUFLATE WITH GAS / LIQUID MIXING COMPARTMENT AND EXPANSION COOLING PROCESS
EP99907572A EP1062370B1 (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof
BR9908644-1A BR9908644A (en) 1998-03-09 1999-02-26 Process for cooling a spear intended for the introduction of a medium in a melt and / or for the measurement of melt properties, and, spear for carrying out the process
RU2000123357/02A RU2221054C2 (en) 1998-03-09 1999-02-26 Blowing tuyere with gas and liquid mixing chamber (versions) and method of expansion cooling of tuyere
ES99907572T ES2169599T3 (en) 1998-03-09 1999-02-26 BLOW LAUNCH WITH GAS / LIQUID BLEND CHAMBER AND PROCEDURE FOR EXPANSION COOLING.
DE59900496T DE59900496D1 (en) 1998-03-09 1999-02-26 BLOWING LAMP WITH GAS / LIQUID MIXING CHAMBER AND METHOD FOR THEIR EXPANSION COOLING
CA002321651A CA2321651C (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof
PCT/EP1999/001255 WO1999046412A1 (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof
JP2000535778A JP4430230B2 (en) 1998-03-09 1999-02-26 Method for cooling a lance for introducing a medium into the melt and / or for measuring the properties of the melt, and a lance for carrying out this method
AT99907572T ATE210195T1 (en) 1998-03-09 1999-02-26 BLOWING LANCE WITH GAS/LIQUID MIXING CHAMBER AND METHOD FOR EXPANSION COOLING THEREOF
CNB998038229A CN1264995C (en) 1998-03-09 1999-02-26 Blasting lance with gas/liquid mixing chamber and method for expansion cooling thereof
US09/623,005 US6562287B1 (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof
KR1020007009862A KR100633188B1 (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and method for expansion cooling thereof

Applications Claiming Priority (1)

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EP98104153A EP0947587A1 (en) 1998-03-09 1998-03-09 Blow lance and process for its cooling

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EP0947587A1 true EP0947587A1 (en) 1999-10-06

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EP98104153A Withdrawn EP0947587A1 (en) 1998-03-09 1998-03-09 Blow lance and process for its cooling
EP99907572A Expired - Lifetime EP1062370B1 (en) 1998-03-09 1999-02-26 Blasting lance with a gas/liquid mixing chamber and a method for the expansion cooling thereof

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EP (2) EP0947587A1 (en)
JP (1) JP4430230B2 (en)
KR (1) KR100633188B1 (en)
CN (1) CN1264995C (en)
AT (1) ATE210195T1 (en)
AU (1) AU2726899A (en)
BR (1) BR9908644A (en)
CA (1) CA2321651C (en)
DE (1) DE59900496D1 (en)
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US7140765B2 (en) * 2001-10-30 2006-11-28 Techint Compagnia Tecnica Internazionale S.P.A. Device and method for discrete and continuous measurement of the temperature of molten metal in a furnace or recepient for its production or treatment
EP3879216A4 (en) * 2018-10-18 2022-02-23 Jiangsu New Chunxing Resource Recycling Co. Ltd Side blowing lance for smelting furnace and use method

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WO2006105578A1 (en) * 2004-10-18 2006-10-12 Technological Resources Pty Limited Apparatus for injecting solid particulate material into a vessel
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US10138151B2 (en) * 2013-05-22 2018-11-27 Johns Manville Submerged combustion burners and melters, and methods of use

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US7140765B2 (en) * 2001-10-30 2006-11-28 Techint Compagnia Tecnica Internazionale S.P.A. Device and method for discrete and continuous measurement of the temperature of molten metal in a furnace or recepient for its production or treatment
WO2004046391A1 (en) * 2002-11-16 2004-06-03 Vai Fuchs Gmbh Method and device for cooling blowing lances
CN1320131C (en) * 2002-11-16 2007-06-06 韦富克斯有限公司 Method and device for cooling blowing lances
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EP3879216A4 (en) * 2018-10-18 2022-02-23 Jiangsu New Chunxing Resource Recycling Co. Ltd Side blowing lance for smelting furnace and use method

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DE59900496D1 (en) 2002-01-17
EP1062370A1 (en) 2000-12-27
JP4430230B2 (en) 2010-03-10
KR20010041658A (en) 2001-05-25
AU2726899A (en) 1999-09-27
ATE210195T1 (en) 2001-12-15
CN1292831A (en) 2001-04-25
CN1264995C (en) 2006-07-19
JP2002506124A (en) 2002-02-26
ES2169599T3 (en) 2002-07-01
PT1062370E (en) 2002-05-31
WO1999046412A1 (en) 1999-09-16
CA2321651C (en) 2007-05-08
BR9908644A (en) 2000-11-14
CA2321651A1 (en) 1999-09-16
EP1062370B1 (en) 2001-12-05
KR100633188B1 (en) 2006-10-11
RU2221054C2 (en) 2004-01-10
US6562287B1 (en) 2003-05-13

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