EP1162424A2 - Process and device for argon recovery - Google Patents
Process and device for argon recovery Download PDFInfo
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- EP1162424A2 EP1162424A2 EP01113971A EP01113971A EP1162424A2 EP 1162424 A2 EP1162424 A2 EP 1162424A2 EP 01113971 A EP01113971 A EP 01113971A EP 01113971 A EP01113971 A EP 01113971A EP 1162424 A2 EP1162424 A2 EP 1162424A2
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- column
- argon
- pressure
- crude
- crude argon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
- F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04684—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser and a bottom re-boiler
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
- F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
- F25J3/048—Argon recovery
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
- F25J2235/58—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2240/00—Processes or apparatus involving steps for expanding of process streams
- F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
- F25J2290/12—Particular process parameters like pressure, temperature, ratios
Definitions
- the invention relates to a method and an apparatus for the production of argon, at the compressed, pre-cleaned and cooled air in a rectification system at least one rectification column and one crude argon column is broken down, according to the Features of the preamble of claims 1 and 6.
- Such a method with a device for the production of argon with up to 10 ppm Contamination content is known from EP 0 377 117 B2, in which one from the so-called argon belly area of a low-pressure column of a two-stage Rectification withdrawn argon-rich oxygen fraction one with one Raw argon condenser supplied equipped in raw argon column and in this same pressure conditions as in the low pressure column by means of at least 150 theoretical floors (levels) as well as structured packings or packing in gaseous raw argon and in a heavy-boiling first liquid residual fraction disassembled, the crude argon of a further fine cleaning in a conventional Way with bottoms and with a top condenser and with a sump evaporator equipped pure argon column for the production of pure argon.
- EP 0 628 777 B1 describes a method and an apparatus for Obtaining argon with up to 10 ppm residual oxygen known, in which the from the separation of air in a rectification system with at least one Rectification column obtained argon-containing oxygen fraction in a crude argon column and a semi-pure column equipped with a crude argon condenser into one Argon product is broken down, the residual fraction of the semi-pure column as Return liquid for the crude argon column is used, the number of to Argon rectification used theoretical soils in the form of conventional soils and / or ordered packings and / or packing in the crude argon / semi-pure column is at least 30 or 60, so that no crude argon condenser in the Crude argon column is required, which reduces the expenditure on equipment and the Operating costs can be reduced.
- the invention has for its object a method and an apparatus initially mentioned type with little equipment and low Operating costs available for the particularly economical extraction of raw argon to deliver.
- the raw argon present at the top of the raw argon column is replaced by indirect Heat exchange with a liquid removed from the process condenses and at least partially fed back into the columns as reflux liquid. A part the condensed crude argon fraction is withdrawn as a product and for further processing Treatment of the pure argon column.
- any liquid air fraction present is at least partially fed into the pressure column, since this measure also Reduced oxygen concentration in the bath of the top condenser of the crude argon column.
- the reflux conditions in the crude argon column are those in the lower column area liquid residual fraction (bottom product) evaporated at least partially.
- Sump heating can also be particularly advantageous in the air separation plant existing high pressure air flow from 10 to 100 bar before its relaxation and Allocation to other rectification columns can be used.
- the raw argon liquefied at the top of the raw argon column is subjected to a fine cleaning in one with a variable number of arranged in different areas conventional floors and / or ordered packings and / or packing, one Pure argon condenser and a bottom evaporator equipped pure argon column subjected to the raw argon in pure argon and in a second low-boiling Residual fraction is broken down.
- the gaseous nitrogen-argon mixture present at the top of the pure argon column is achieved through indirect heat exchange in the pure argon condenser (top condenser Pure argon column) liquefied, with the liquefied fraction returning to the Pure argon column fed and the non-liquefied portion as a gaseous flushing stream is blown off into the system environment.
- the invention also relates to a device for the production of argon according to the Features of claims 6 to 9.
- the argon production which is reduced in pressure according to the invention, can be significantly improved reduced number of theoretical floors in the form of in a variable number in conventional floors arranged in different areas of the crude argon column and / or orderly packings and / or fillers, thereby reducing the overall height the crude argon column significantly reduced and thus the apparatus and process engineering Effort is reduced, so that an inexpensive production of argon is guaranteed with 0.1 to 10 ppm residual oxygen.
- the figure of the drawing shows a process diagram of an argon production according to the invention.
- the crude argon 6 present at the top of the crude argon column 5 with 0.1 to 10 ppm Residual oxygen content is obtained through indirect heat exchange with one from the process withdrawn liquid condensed and at least partially as reflux liquid fed back into the raw argon column 5.
- condensation of crude argon 6 from the bottom of the pressure column 1 Liquid supplied via line 9 is used to do this via a valve in the room a raw argon condenser 10 is expanded into it.
- Part of the condensed Crude argon fraction is via line 15 as a low-oxygen crude argon precursor withdrawn and fed to a pure argon column 16 for further treatment.
- the one in the bottom Liquid residual fraction 7 present at least partially in the region of the crude argon column 5 evaporated in an evaporator by a process stream.
- Evaporating agent withdrawn from the bottom of the pressure column 1 oxygen-rich Use liquid only after passing the evaporator and before the entry into the crude argon condenser 10 is relaxed.
- An existing one in the air separation plant can also be particularly advantageous a pressure of 10 to 100 bar air flow to operate the bottom evaporator 11 are used in the raw argon column 5. This high pressure air flow is relaxed only after passing the evaporator and on the pressure and Low pressure column 1, 2 divided. The portion not evaporated in the crude argon column 5 liquid residual fraction 7 is fed back by means of a conveyor 14 via a Line 13 fed back into the low pressure column 2.
- a part of the raw argon 6 liquefied in the raw argon condenser 10 is called low-oxygen argon precursor with a residual oxygen content of 0.1 to 10 ppm fed via line 15 into the pure argon column 16.
- the pure argon column 16 is arranged so far below the crude argon condenser 10 that the geodetic height of the liquid column of pure argon the pressure difference between the crude argon and pure argon column 5, 16 and that during transport of the liquid compensates for any pressure losses.
- the pure argon column 16 is variable Number of differently arranged conventional floors and / or ordered Packings and / or fillers equipped and separates the incoming low-oxygen Crude argon product in an argon-nitrogen mixture 17 and in an oxygen and low nitrogen pure argon product, which is a liquid pure argon product 27 from the Bottom of the pure argon column 16 is withdrawn.
- the gaseous argon-nitrogen mixture present at the top of the pure argon column 16 17 is partially by indirect heat exchange in a pure argon condenser 21 liquefied, the liquefied fraction as reflux back into the pure argon column 16 is fed and the non-liquefied portion as a gaseous nitrogen purge stream is blown off into the plant environment via a line 22.
- a pure argon condenser 21 finds one from the pressure column 1 via a line 23 supplied gaseous fraction use, which is initially in a Pure argon evaporator 24 condenses before one with one over one Relaxation valve 25 provided line 26 into the pure argon condenser 21 is relaxed.
- a liquid residual fraction 18 obtained in the bottom of the pure argon column 16 becomes partial evaporated in the pure argon evaporator 24 and the non-evaporated liquid portion as liquid pure argon product 27 deducted.
- the argon production according to the invention is with or without additional crude argon column bottom evaporation in all common air separation plants with one Rectification system with at least one rectification column and one crude argon column with the advantages shown.
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Abstract
Description
Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Gewinnung von Argon, bei
dem verdichtete, vorgereinigte und abgekühlte Luft in einem Rektifikationssystem mit
mindestens einer Rektifiziersäule und einer Rohargonsäule zerlegt wird, nach den
Merkmalen des Oberbegriffs von Anspruch 1 und 6.The invention relates to a method and an apparatus for the production of argon, at
the compressed, pre-cleaned and cooled air in a rectification system
at least one rectification column and one crude argon column is broken down, according to the
Features of the preamble of
Ein derartiges Verfahren mit Vorrichtung zur Gewinnung von Argon mit bis zu 10 ppm Verunreinigungsanteil ist durch EP 0 377 117 B2 bekannt, bei welchen eine aus dem sogenannten Argonbauch-Bereich einer Niederdrucksäule einer zweistufigen Rektifikation abgezogene argonreiche Sauerstofffraktion einer mit einem Rohargonkondensator ausgerüsteten Rohargonsäule zugeführt und in dieser bei gleichen Druckverhältnissen wie in der Niederdrucksäule mittels von mindestens 150 theoretischen Böden (Stufen) sowie strukturierten Packungen oder Füllkörpern in gasförmiges Rohargon und in eine schwerersiedende erste flüssige Restfraktion zerlegt, wobei das Rohargon einer weiteren Feinreinigung in einer auf konventionelle Weise mit Böden und mit einem Kopfkondensator sowie mit einem Sumpfverdampfer ausgerüsteten Reinargonsäule zur Gewinnung von Reinargon unterzogen wird.Such a method with a device for the production of argon with up to 10 ppm Contamination content is known from EP 0 377 117 B2, in which one from the so-called argon belly area of a low-pressure column of a two-stage Rectification withdrawn argon-rich oxygen fraction one with one Raw argon condenser supplied equipped in raw argon column and in this same pressure conditions as in the low pressure column by means of at least 150 theoretical floors (levels) as well as structured packings or packing in gaseous raw argon and in a heavy-boiling first liquid residual fraction disassembled, the crude argon of a further fine cleaning in a conventional Way with bottoms and with a top condenser and with a sump evaporator equipped pure argon column for the production of pure argon.
Des Weiteren ist durch die EP 0 628 777 B1 ein Verfahren und eine Vorrichtung zur Gewinnung von Argon mit bis zu 10 ppm Sauerstoffrestanteil bekannt, bei welchen die aus der Zerlegung von Luft in einem Rektifiziersystem mit mindestens einer Rektifiziersäule gewonnene argonhaltige Sauerstofffraktion in einer Rohargonsäule und einer mit einem Rohargonkondensator ausgerüsteten Halbreinsäule zu einem Argonprodukt zerlegt wird, wobei die Restfraktion der Halbreinsäule als Rücklaufflüssigkeit für die Rohargonsäule Verwendung findet, wobei die Anzahl der zur Argonrektifikation verwendeten theoretische Böden in Form von konventionellen Böden und/oder geordneten Packungen und/oder Füllkörpern in der Rohargon-/Halbreinsäule mindestens 30 bzw. 60 beträgt, sodass kein Rohargonkondensator in der Rohargonsäule erforderlich ist, wodurch der apparative Aufwand verringert und die Betriebskosten gesenkt werden.Furthermore, EP 0 628 777 B1 describes a method and an apparatus for Obtaining argon with up to 10 ppm residual oxygen known, in which the from the separation of air in a rectification system with at least one Rectification column obtained argon-containing oxygen fraction in a crude argon column and a semi-pure column equipped with a crude argon condenser into one Argon product is broken down, the residual fraction of the semi-pure column as Return liquid for the crude argon column is used, the number of to Argon rectification used theoretical soils in the form of conventional soils and / or ordered packings and / or packing in the crude argon / semi-pure column is at least 30 or 60, so that no crude argon condenser in the Crude argon column is required, which reduces the expenditure on equipment and the Operating costs can be reduced.
Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren und eine Vorrichtung der eingangs genannten Art mit einem geringen apparativen Aufwand und niedrigen Betriebskosten zur besonders wirtschaftlichen Gewinnung von Rohargon zur Verfügung zu stellen.The invention has for its object a method and an apparatus initially mentioned type with little equipment and low Operating costs available for the particularly economical extraction of raw argon to deliver.
Diese Aufgabe wird durch ein Verfahren und eine Vorrichtung nach Anspruch 1 und 6
gelöst.This object is achieved by a method and an apparatus according to
Erfindungsgemäß wird der aus der Niederdrucksäule der zweistufigen Rektifiziersäule im Bereich eines sogenannten Argonbauchs unter einem Druck von 1,2 - 1,6 bar abgezogene argonhaltige Sauerstoffstrom durch eine, in der die Niederducksäule mit der Rohargonsäule verbindenden Leitung angeordnete Drossel auf einen Druck von etwa 0,9 - 1,1 bar reduziert und unter diesem Druck in der Rohargonsäule unter Verwendung einer variablen Anzahl von in unterschiedlichen Bereichen angeordneten konventionellen Böden und/oder geordneten Packungen und/oder Füllkörpern zu gasförmiges Rohargon und einer ersten schwerersiedenden flüssigen Restfraktion (Sumpfprodukt) zerlegt.According to the invention from the low pressure column of the two-stage rectification column in the area of a so-called argon belly under a pressure of 1.2-1.6 bar deducted argon-containing oxygen flow through one in which the low pressure column with the line connecting the crude argon column arranged to a pressure of about 0.9 - 1.1 bar reduced and under this pressure in the crude argon column Using a variable number of arranged in different areas conventional floors and / or ordered packings and / or packing gaseous crude argon and a first heavy-boiling liquid residual fraction (Bottom product) disassembled.
Das am Kopf der Rohargonsäule vorliegende Rohargon wird durch indirekten Wärmetausch mit einer aus dem Prozess entnommenen Flüssigkeit kondensiert und zumindest teilweise als Rücklaufflüssigkeit wieder in die Kolonnen eingespeist. Ein Teil der kondensierten Rohargonfraktion wird als Produkt abgezogen und zur weiteren Behandlung der Reinargonsäule zugeführt.The raw argon present at the top of the raw argon column is replaced by indirect Heat exchange with a liquid removed from the process condenses and at least partially fed back into the columns as reflux liquid. A part the condensed crude argon fraction is withdrawn as a product and for further processing Treatment of the pure argon column.
Wie vorab bereits beschrieben, ist die Verwendung der aus der Hochdrucksäule entnommenen sauerstoffreichen Flüssigkeit als Kühlmedium für den Rohargonkondensator von Vorteil.As previously described, is the use of the high pressure column withdrawn oxygen-rich liquid as a cooling medium for the Raw argon condenser is an advantage.
Im Zusammenhang mit der Erfindung ist es besonders vorteilhaft, wenn die gesamte zur Verfügung stehende Sumpfflüssigkeit der Drucksäule zum Rohargonkondensator (Kopfkondensator Rohargonsäule)) gefahren wird, da in diesem Fall die Sauerstoffkonzentration des Flüssigbades, in dem der Rohargonkondensator aufgehangen ist, sinkt und somit die Kondensation des Rohargons bei tieferen Temperaturen und damit bei einem niedrigeren Druck in der Rohargonsäule ermöglicht.In connection with the invention, it is particularly advantageous if the entire Sump liquid available from the pressure column to the crude argon condenser (Top condenser crude argon column)) is driven, because in this case the oxygen concentration the liquid bath in which the crude argon condenser is suspended, decreases and thus the condensation of the raw argon at lower temperatures and thus at a lower pressure in the crude argon column.
Zudem ist es besonders vorteilhaft, wenn eventuell vorhandene Flüssigluftfraktion zumindest teilweise in die Drucksäule eingespeist wird, da auch diese Maßnahme die Sauerstoffkonzentration im Bad des Kopfkondensators der Rohargonsäule absenkt. In addition, it is particularly advantageous if any liquid air fraction present is at least partially fed into the pressure column, since this measure also Reduced oxygen concentration in the bath of the top condenser of the crude argon column.
In einer vorteilhaften Ausführungsform der Erfindung wird zur Verbesserung der Rücklaufverhältnisse in der Rohargonsäule die im unteren Säulenbereich vorliegende flüssige Restfraktion (Sumpfprodukt) mindestens teilweise verdampft.In an advantageous embodiment of the invention is used to improve the The reflux conditions in the crude argon column are those in the lower column area liquid residual fraction (bottom product) evaporated at least partially.
Zum erfindungsgemäßen Verdampfen des Sumpfprodukts der Rohargonsäule findet bevorzugt die aus dem Sumpf der Hochdrucksäule abgezogene, eventuell noch durch indirekten Wärmeaustausch vorgekühlte sauerstoffreiche Flüssigkeit Verwendung, die nach dem Passieren der Sumpfheizung entspannt und als Kühlmedium dem Rohargonkondensator zugeführt wird.To evaporate the bottom product of the crude argon column according to the invention prefers the one withdrawn from the sump of the high-pressure column, possibly through indirect heat exchange pre-cooled oxygen-rich liquid use that relaxed after passing through the sump heater and as the cooling medium Raw argon condenser is supplied.
Als zusätzliches oder alternatives Heizmedium für die vorab beschriebene Sumpfheizung kann besonders vorteilhaft auch ein in der Luftzerlegungsanlage vorhandener Hochdruckluftstrom von 10 bis 100 bar vor seiner Entspannung und Aufteilung auf weitere Rektifiziersäulen verwendet werden.As an additional or alternative heating medium for the previously described Sump heating can also be particularly advantageous in the air separation plant existing high pressure air flow from 10 to 100 bar before its relaxation and Allocation to other rectification columns can be used.
Der Vorteil dieser erfindungsgemäßen zusätzlichen Sumpfverdampfung in der Rohargonsäule unter Verwendung von aus der Drucksäule eingespeisten Sauerstoff besteht insbesondere darin, dass die Rektifikationsverhältnisse in der Rohargonsäule ohne negative Beeinflussung des Rektifikationsprozesses in der Niederdrucksäule wesentlich verbessert werden.The advantage of this additional bottom evaporation according to the invention in the Crude argon column using oxygen fed from the pressure column is in particular that the rectification ratios in the crude argon column without negatively influencing the rectification process in the low pressure column be significantly improved.
Dabei wird die Auftriebsgasmenge und damit das Rücklaufverhältnis in der Rohargonsäule erhöht, ohne dass der aus der Niederdrucksäule abgezogene argonhaltige Sauerstoffstrom zur Beschickung der Rohargonsäule vergrößert werden muss.The amount of buoyancy gas and thus the reflux ratio in the Crude argon column increases without the one withdrawn from the low pressure column Argon-containing oxygen flow for feeding the raw argon column can be increased got to.
Folglich wird auch der aus der Niederdrucksäule im abgezogenen Seitengas enthaltene Stickstoffanteil nicht zusätzlich erhöht, wodurch die bisher am Kopf der Rohargonsäule zu verzeichnende Stickstoffanreicherung (Faktor 28-36) und damit eine den störungsfreien Betrieb des Rohargonkondensators beeinträchtigende sowie eine die Weiterbearbeitung erschwerende Stickstoffanreicherung im Rohargon-produkt vermieden wird.Consequently, the low pressure column in the extracted side gas nitrogen content contained is not additionally increased, whereby the previously at the head of Nitrogen enrichment (factor 28-36) and thus a the uninterrupted operation of the raw argon condenser and a further processing complicates nitrogen enrichment in the raw argon product is avoided.
Zur Gewinnung von gasförmigen und flüssigen Argon mit 0,1 bis 10 ppm Restsauerstoff wird das am Kopf der Rohargonsäule verflüssigte Rohargon einer Feinreinigung in einer mit einer variablen Anzahl von in unterschiedlichen Bereichen angeordneten konventionellen Böden und/oder geordneten Packungen und/oder Füllkörpern, einem Reinargonkondensator und einem Sumpfverdampfer ausgerüsteten Reinargonsäule unterzogen, bei der das Rohargon in Reinargon und in eine zweite leichtersiedende Restfraktion zerlegt wird.For the extraction of gaseous and liquid argon with 0.1 to 10 ppm residual oxygen the raw argon liquefied at the top of the raw argon column is subjected to a fine cleaning in one with a variable number of arranged in different areas conventional floors and / or ordered packings and / or packing, one Pure argon condenser and a bottom evaporator equipped pure argon column subjected to the raw argon in pure argon and in a second low-boiling Residual fraction is broken down.
Das am Kopf der Reinargonsäule vorliegende gasförmige Stickstoff-Argon-Gemisch wird durch indirekten Wärmeaustausch im Reinargonkondensator (Kopfkondensator Reinargonsäule) verflüssigt, wobei die verflüssigte Fraktion als Rücklauf wieder in die Reinargonsäule eingespeist und der nicht verflüssigte Anteil als gasförmiger Spülstrom in die Anlagenumgebung abgeblasen wird.The gaseous nitrogen-argon mixture present at the top of the pure argon column is achieved through indirect heat exchange in the pure argon condenser (top condenser Pure argon column) liquefied, with the liquefied fraction returning to the Pure argon column fed and the non-liquefied portion as a gaseous flushing stream is blown off into the system environment.
Zum Kühlen des Reinargonkondensators findet ein aus der Hochdrucksäule entnommener gasförmiger Strom Verwendung, der zunächst im Verdampfer der Reinargonsäule kondensiert und anschließend in den Reinargonkondensator hinein entspannt wird.To cool the pure argon condenser, one finds from the high pressure column withdrawn gaseous stream use, which is initially in the evaporator Pure argon column condensed and then into the pure argon condenser is relaxed.
Zur Erzeugung des für den Betrieb der Reinargonsäule benötigten Auftriebgases wird das im Säulensumpf anfallende Flüssigprodukt durch indirekten Wärmetausch im Verdampfer der Reinargonsäule teilweise verdampft. Der nicht verdampfte Anteil an Sumpfflüssigkeit kann als flüssiges Reinargonprodukt abgezogen werden.To generate the buoyancy gas required for operating the pure argon column the resulting liquid product in the column sump through indirect heat exchange in the Evaporator of the pure argon column partially evaporated. The portion not evaporated Bottom liquid can be withdrawn as a liquid pure argon product.
Zur Erzeugung des für die Feinreinigung des Rohargons in der Reinargonsäule benötigten Druckes wird das aufgrund der zwischen der Roh- und Reinargonsäule bestehenden Höhendifferenz aufgebaute hydrostatische Potential genutzt.For the production of the fine cleaning of the raw argon in the pure argon column required pressure will be due to the between the raw and pure argon column existing hydrostatic potential is used.
Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von Argon nach den
Merkmalen der Patentansprüche 6 bis 9.The invention also relates to a device for the production of argon according to the
Features of
Die erfindungsgemäß druckreduzierte Argon-Gewinnung kann mit einer wesentlich verringerten Anzahl von theoretischen Böden in Form von in einer variablen Anzahl in unterschiedlichen Bereichen der Rohargonsäule angeordneten konventionellen Böden und/oder geordneten Packungen und/oder Füllkörper erfolgen, wodurch die Bauhöhe der Rohargonsäule wesentlich verringert und damit der apparative und verfahrenstechnische Aufwand gesenkt wird, sodass eine kostengünstige Gewinnung von Argon mit 0,1 bis 10 ppm Restsauerstoffanteil gewährleistet wird.The argon production, which is reduced in pressure according to the invention, can be significantly improved reduced number of theoretical floors in the form of in a variable number in conventional floors arranged in different areas of the crude argon column and / or orderly packings and / or fillers, thereby reducing the overall height the crude argon column significantly reduced and thus the apparatus and process engineering Effort is reduced, so that an inexpensive production of argon is guaranteed with 0.1 to 10 ppm residual oxygen.
Die Erfindung wird im folgenden anhand eines in der Zeichnung dargestellten Ausführungsbeispieles näher erläutert. The invention is described below with reference to one in the drawing Embodiment explained in more detail.
Die Figur der Zeichnung zeigt ein Verfahrensschema einer erfindungsgemäßen Argon-Gewinnung.The figure of the drawing shows a process diagram of an argon production according to the invention.
Ein aus einer, in einem Rektifiziersystem mit einer Drucksäule 1 durch einen
Kondensator thermisch gekoppelten Niederdrucksäule 2 im Bereich des
sogenannten Argonbauches unter einen Druck von etwa 1,2 bis 1,6 bar und einem
Argongehalt von 8-14 % über eine Leitung 3 abgezogener Sauerstoffstrom wird durch
eine in der Leitung 3 angeordnete, beispielsweise als Ventil oder Klappe ausgebildete
Drossel 4 auf einen Druck von etwa 0,9 bis 1,1 bar reduziert und unter diesem Druck in
eine Rohargonsäule 5 eingespeist und in dieser unter Verwendung einer variablen
Anzahl von unterschiedlich angeordneten konventionellen Böden und/oder geordneten
Packungen und/oder Füllkörpern in gasförmiges Rohargon 6 (Kopffraktion) und in eine
erste flüssige Restfraktion 7 (Sumpfprodukt) rektifiziert.One from one, in a rectification system with a pressure column 1 through one
Condenser thermally coupled
Das am Kopf der Rohargonsäule 5 vorliegende Rohargon 6 mit 0,1 bis 10 ppm
Restsauerstoffgehalt wird durch indirekten Wärmetausch mit einer aus dem Prozess
entnommenen Flüssigkeit kondensiert und zumindest teilweise als Rücklaufflüssig-keit
wieder in die Rohargonsäule 5 eingespeist.The
In der Regel wird zur Kondensation des Rohargons 6 aus dem Sumpf der Drucksäule 1
über Leitung 9 zugeführte Flüssigkeit verwendet, die dazu über ein Ventil in den Raum
eines Rohargonkondensators 10 hinein entspannt wird. Ein Teil der kondensierten
Rohargonfraktion wird über Leitung 15 als sauerstoffarmes Rohargonvorprodukt
abgezogen und zur weiteren Behandlung einer Reinargonsäule 16 zugeführt.In general, condensation of
Zur Optimierung der Rücklaufverhältnisse in der Rohargonsäule 5 wird die im unteren
Bereich der Rohargonsäule 5 vorliegende flüssige Restfraktion 7 zumindest teilweise
in einem Verdampfer durch einen Prozeßstrom verdampft. Vorteilhaft findet als
Verdampfungsmittel aus dem Sumpf der Drucksäule 1 abgezogene sauerstoffreiche
Flüssigkeit Verwendung, welche erst nach dem Passieren des Verdampfers und vor
dem Eintritt in den Rohargonkondensator 10 entspannt wird.To optimize the reflux conditions in the
Besonders vorteilhaft kann auch ein in der Luftzerlegungsanlage vorhandener, unter
einem Druck von 10 bis 100 bar stehender Luftstrom zum Betrieb des Sumpfverdampfers
11 in der Rohargonsäule 5 Verwendung finden. Dieser Hochdruckluftstrom
wird erst nach dem Passieren des Verdampfers entspannt und auf die Druck- und
Niederdrucksäule 1, 2 aufgeteilt. Der in der Rohargonsäule 5 nicht verdampfte Anteil an
flüssiger Restfraktion 7 wird als Rücklauf mittels einer Fördereinrichtung 14 über eine
Leitung 13 wieder in die Niederdrucksäule 2 eingespeist.An existing one in the air separation plant can also be particularly advantageous
a pressure of 10 to 100 bar air flow to operate the
Ein Teil des im Rohargonkondensator 10 verflüssigten Rohargons 6 wird als
sauerstoffarmes Argonvorprodukt mit einem Restsauerstoffgehalt von 0,1 bis 10 ppm
über die Leitung 15 in die Reinargonsäule 16 eingespeist. Die Reinargonsäule 16 ist
dabei so weit unterhalb des Rohargonkondensators 10 angeordnet, dass die
geodätische Höhe der Flüssigkeitssäule von Reinargon den Druckunterschied zwischen
der Rohargon- und Reinargonsäule 5, 16 sowie die beim Transport der Flüssigkeit
entstehenden Druckverluste ausgleicht. Die Reinargonsäule 16 ist mit einer variablen
Anzahl von unterschiedlich angeordneten konventionellen Böden und/oder geordneten
Packungen und/oder Füllkörpern ausgerüstet und trennt das eintretende sauerstoffarme
Rohargonprodukt in ein Argon-Stickstoff-Gemisch 17 und in ein sauerstoff- und
stickstoffarmes Reinargonprodukt, das als flüssiges Reinargonprodukt 27 aus dem
Sumpf der Reinargonsäule 16 abgezogen wird.A part of the
Das am Kopf der Reinargonsäule 16 vorliegende gasförmige Argon-Stickstoff-Gemisch
17 wird durch indirekten Wärmetausch in einem Reinargonkondensator 21 teilweise
verflüssigt, wobei die verflüssigte Fraktion als Rücklauf wieder in die Reinargonsäule
16 eingespeist wird und der nicht verflüssigte Anteil als gasförmiger Stickstoff-Spülstrom
über eine Leitung 22 in die Anlagenumgebung abgeblasen wird. Zum Kühlen
des Reinargonkondensators 21 findet eine aus der Drucksäule 1 über eine Leitung 23
zugeführte gasförmige Fraktion Verwendung, welche zunächst in einem
Reinargonverdampfer 24 kondensiert, bevor diese über eine mit ein an einem
Entspannungsventil 25 versehene Leitung 26 in den Reinargonkondensator 21 hinein
entspannt wird.The gaseous argon-nitrogen mixture present at the top of the
Eine im Sumpf der Reinargonsäule 16 anfallende flüssige Restfraktion 18 wird teilweise
im Reinargonverdampfer 24 verdampft und der nicht verdampfte Flüssigkeitsanteil als
flüssiges Reinargonprodukt 27 abgezogen.A liquid
Die erfindungsgemäße Argon-Gewinnung ist mit oder ohne zusätzlicher Rohargonsäulen-Sumpfverdampfung in allen gebräuchlichen Luftzerlegungsanlagen mit einem Rektifiziersystem mit mindestens einer Rektifiziersäule und einer Rohargonsäule mit den aufgezeigten Vorteilen einsetzbar.The argon production according to the invention is with or without additional crude argon column bottom evaporation in all common air separation plants with one Rectification system with at least one rectification column and one crude argon column with the advantages shown.
Claims (9)
der Druck in der Rohargonsäule (5) geringer ist als der Druck in der Niederdrucksäule (2).Process for the production of argon, in which compressed, pre-cleaned and cooled air is broken down in a rectification system with at least one rectification column and one crude argon column, wherein
the pressure in the crude argon column (5) is lower than the pressure in the low pressure column (2).
dadurch gekennzeichnet, dass
der argonhaltige Sauerstoffstrom in der Rohargonsäule (5) unter einem Druck von etwa 0,9 bis 1,1 bar rektifiziert wird.Method according to claim 1,
characterized in that
the argon-containing oxygen flow in the crude argon column (5) is rectified under a pressure of about 0.9 to 1.1 bar.
dadurch gekennzeichnet, dass
die Druckreduzierung des aus der Niederdrucksäule (2) abgezogenen argonhaltigen Sauerstoffstroms vor dessen Einspeisung in die Rohargonsäule (5) erfolgt. The method of claim 1 or 2,
characterized in that
the pressure reduction of the argon-containing oxygen stream drawn off from the low-pressure column (2) takes place before it is fed into the crude argon column (5).
dadurch gekennzeichnet, dass
die im unteren Bereich der Rohargonsäule (5) vorliegende flüssige Restfraktion (7) zumindestens teilweise durch einen-aus der Drucksäule (1) zugeführten Prozeßstrom verdampft wird.Method according to one of claims 1 to 3,
characterized in that
the liquid residual fraction (7) present in the lower region of the crude argon column (5) is at least partially evaporated by a process stream supplied from the pressure column (1).
dadurch gekennzeichnet, dass
als Prozeßstrom zum Verdampfen der flüssigen Restfraktion (7) in der Rohargonsäule (5) aus dem Sumpf der Drucksäule (1) abgezogener und gekühlter sauerstoffreicher Flüssigstrom Verwendung findet.Method according to claim 4,
characterized in that
as the process stream for evaporating the liquid residual fraction (7) in the crude argon column (5) from the bottom of the pressure column (1) and cooled and oxygen-rich liquid stream is used.
dadurch gekennzeichnet, dass
die die Niederdrucksäule (2) mit der Rohargonsäule (5) verbindende Leitung (3) ein Mittel zur Druckreduzierung des argonhaltigen Sauerstoffstroms aufweist.Device for the production of argon according to one of claims 1 to 5 with a rectification system with at least one rectification column and a crude argon column, wherein a low-pressure column of the rectification system with a line for feeding an argon-containing oxygen stream into the with a variable number of differently arranged conventional trays and / or ordered packs and / or packing and a condenser equipped raw argon column, which through a line for feeding raw argon into a variable number of differently arranged conventional trays and / or ordered packing and / or packing, a condenser and a sump evaporator as well as the Raw and pure argon columns are connected to the rectification column by means of a line system via at least one heat exchanger,
characterized in that
the line (3) connecting the low-pressure column (2) to the crude argon column (5) has a means for reducing the pressure of the argon-containing oxygen stream.
dadurch gekennzeichnet, dass
das in der Leitung (3) angeordnete Mittel zur Druckreduzierung eine, vorzugsweise als Ventil oder Klappe ausgebildete Drossel (4) ist. Apparatus according to claim 6,
characterized in that
the means for reducing the pressure arranged in the line (3) is a throttle (4), preferably designed as a valve or flap.
gekennzeichnet dadurch, dass
die Rohargonsäule (5) einen im Bereich einer flüssigen Restfraktion (7) angeordneten Sumpfverdampfer (11) aufweist.Apparatus according to claim 6 or 7,
characterized in that
the crude argon column (5) has a bottom evaporator (11) arranged in the region of a liquid residual fraction (7).
gekennzeichnet dadurch, dass
der durch eine Leitung (26) mit dem Reinargonkondensator (21) der Reinargonsäule (16) verbundene Reinargonverdampfer (24) über eine Leitung (23) mit einer Drucksäule (1) verbunden ist.Device according to one of claims 6 to 8,
characterized in that
the pure argon evaporator (24) connected to the pure argon condenser (21) of the pure argon column (16) by a line (26) is connected to a pressure column (1) via a line (23).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10028871A DE10028871A1 (en) | 2000-06-10 | 2000-06-10 | Process and apparatus for the production of argon |
| DE10028871 | 2000-06-10 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP1162424A2 true EP1162424A2 (en) | 2001-12-12 |
| EP1162424A3 EP1162424A3 (en) | 2002-01-09 |
| EP1162424B1 EP1162424B1 (en) | 2009-02-25 |
Family
ID=7645424
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP01113971A Expired - Lifetime EP1162424B1 (en) | 2000-06-10 | 2001-06-08 | Process and device for argon recovery |
Country Status (3)
| Country | Link |
|---|---|
| EP (1) | EP1162424B1 (en) |
| AT (1) | ATE423951T1 (en) |
| DE (2) | DE10028871A1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007192466A (en) * | 2006-01-19 | 2007-08-02 | Nippon Steel Corp | Cryogenic air separation plant and its control method |
| FR3107341A1 (en) * | 2020-02-18 | 2021-08-20 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for air separation by cryogenic distillation |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0341512A1 (en) * | 1988-04-29 | 1989-11-15 | Air Products And Chemicals, Inc. | Control method to maximize argon recovery from cryogenic air separation units |
| EP0538520A1 (en) * | 1991-10-22 | 1993-04-28 | Odessky Institut Nizkotemperaturnoi Tekhniki I Energetiki | Method of air separation |
| EP0594214A1 (en) * | 1992-10-23 | 1994-04-27 | Praxair Technology, Inc. | Cryogenic rectification system with thermally integrated argon column |
| EP0684437A1 (en) * | 1994-05-27 | 1995-11-29 | The BOC Group plc | Air separation |
| US5592833A (en) * | 1994-02-24 | 1997-01-14 | Linde Aktiengesellschaft | Process and apparatus for the recovery of pure argon |
| EP0786633A1 (en) * | 1995-06-20 | 1997-07-30 | Nippon Sanso Corporation | Method and apparatus for separating argon |
| EP1055891A1 (en) * | 1999-05-25 | 2000-11-29 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Cryogenic distillation system for air separation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4406051A1 (en) * | 1994-02-24 | 1995-08-31 | Linde Ag | Fractional distillation of argon from air, with increased purity and economy, |
-
2000
- 2000-06-10 DE DE10028871A patent/DE10028871A1/en not_active Ceased
-
2001
- 2001-06-08 EP EP01113971A patent/EP1162424B1/en not_active Expired - Lifetime
- 2001-06-08 AT AT01113971T patent/ATE423951T1/en not_active IP Right Cessation
- 2001-06-08 DE DE50114720T patent/DE50114720D1/en not_active Expired - Lifetime
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0341512A1 (en) * | 1988-04-29 | 1989-11-15 | Air Products And Chemicals, Inc. | Control method to maximize argon recovery from cryogenic air separation units |
| EP0538520A1 (en) * | 1991-10-22 | 1993-04-28 | Odessky Institut Nizkotemperaturnoi Tekhniki I Energetiki | Method of air separation |
| EP0594214A1 (en) * | 1992-10-23 | 1994-04-27 | Praxair Technology, Inc. | Cryogenic rectification system with thermally integrated argon column |
| US5592833A (en) * | 1994-02-24 | 1997-01-14 | Linde Aktiengesellschaft | Process and apparatus for the recovery of pure argon |
| EP0684437A1 (en) * | 1994-05-27 | 1995-11-29 | The BOC Group plc | Air separation |
| EP0786633A1 (en) * | 1995-06-20 | 1997-07-30 | Nippon Sanso Corporation | Method and apparatus for separating argon |
| EP1055891A1 (en) * | 1999-05-25 | 2000-11-29 | L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Cryogenic distillation system for air separation |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007192466A (en) * | 2006-01-19 | 2007-08-02 | Nippon Steel Corp | Cryogenic air separation plant and its control method |
| FR3107341A1 (en) * | 2020-02-18 | 2021-08-20 | L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude | Method and apparatus for air separation by cryogenic distillation |
Also Published As
| Publication number | Publication date |
|---|---|
| DE10028871A1 (en) | 2001-12-20 |
| EP1162424B1 (en) | 2009-02-25 |
| EP1162424A3 (en) | 2002-01-09 |
| DE50114720D1 (en) | 2009-04-09 |
| ATE423951T1 (en) | 2009-03-15 |
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