EP1162423A2 - Process and device for argon recovery - Google Patents

Process and device for argon recovery Download PDF

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Publication number
EP1162423A2
EP1162423A2 EP01113970A EP01113970A EP1162423A2 EP 1162423 A2 EP1162423 A2 EP 1162423A2 EP 01113970 A EP01113970 A EP 01113970A EP 01113970 A EP01113970 A EP 01113970A EP 1162423 A2 EP1162423 A2 EP 1162423A2
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EP
European Patent Office
Prior art keywords
argon
column
oxygen
separation
rectification
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.)
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Application number
EP01113970A
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German (de)
French (fr)
Other versions
EP1162423A3 (en
Inventor
Klaus-Peter Walter
Theo Sentis
Joachim Krey
Thorsten Möller
Jens Juckel
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Air Liquide AGS GmbH
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Messer AGS GmbH
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Publication date
Application filed by Messer AGS GmbH filed Critical Messer AGS GmbH
Publication of EP1162423A2 publication Critical patent/EP1162423A2/en
Publication of EP1162423A3 publication Critical patent/EP1162423A3/en
Withdrawn legal-status Critical Current

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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04642Recovering noble gases from air
    • F25J3/04648Recovering noble gases from air argon
    • F25J3/04654Producing crude argon in a crude argon column
    • F25J3/04666Producing 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
    • F25J3/04672Producing 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
    • F25J3/04703Producing 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 being arranged in more than one vessel
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04406Processes 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
    • F25J3/04412Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04642Recovering noble gases from air
    • F25J3/04648Recovering noble gases from air argon
    • F25J3/04654Producing crude argon in a crude argon column
    • F25J3/04666Producing 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
    • F25J3/04672Producing 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
    • F25J3/04678Producing 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04866Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04896Details of columns, e.g. internals, inlet/outlet devices
    • F25J3/04915Combinations of different material exchange elements, e.g. within different columns
    • F25J3/04921Combinations of different material exchange elements, e.g. within different columns within the same column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04866Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04896Details of columns, e.g. internals, inlet/outlet devices
    • F25J3/04933Partitioning walls or sheets
    • F25J3/04939Vertical, e.g. dividing wall columns
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/58Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2240/00Processes or apparatus involving steps for expanding of process streams
    • F25J2240/40Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval

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 4.
  • 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 a top condenser equipped raw argon column supplied and in this at the same Pressure ratios as in the low pressure column using 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 bottom 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 a maximum of 10 ppm residual oxygen known, in which that 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 top condenser to an argon product is broken down, the residual fraction of the semi-pure column as reflux liquid for the Crude argon column is used, the number of argon rectification used theoretical floors in the form of conventional floors and / or ordered packings and / or packing in the crude argon / semi-pure column can be reduced at least 30 or 60, so that no head capacitor in the Crude argon column is required, which reduces the expenditure on equipment and the Operating costs can be reduced.
  • the rectification columns are usually like this made that the separation section takes up the entire column diameter, the size of which depends on the amount of gas flowing in the column.
  • the invention has for its object a method and an apparatus initially mentioned type with little equipment and low Operating costs for the particularly economical extraction of raw argon are available to deliver.
  • the invention takes place in the low pressure column below the argon side gas discharge area one spatially separated from the nitrogen-oxygen separation Argon-oxygen pre-separation takes place, whereby the argon portion in the crude argon column withdrawn argon-oxygen side gas increased to about 80% and thus the subsequent separation effort in the crude argon column is significantly reduced.
  • the nitrogen-oxygen pre-separation is preferably concentric enclosing outer argon-oxygen pre-separation by means of a partition in their upper range from the nitrogen-oxygen separation and from that above the Argon-oxygen pre-separation and nitrogen-oxygen separation arranged Section of the low pressure column separated gastight.
  • the gas-tight separation of the argon-oxygen pre-separation according to the invention from the Nitrogen-oxygen separation and these two separation devices from the a gaseous fraction up to 40% above the separation section Section of the low pressure column containing nitrogen is required to the Raw argon column a low-nitrogen argon side vent to a trouble-free, to be able to perform optimal operation of the crude argon condenser.
  • the result of rectification of the argon side gas in the crude argon column as Gaseous top product crude argon is the crude argon product from the Raw argon column deducted and by means of the overhead condenser by indirect Heat exchange preferably against from the pressure column of the rectification column Bottom liquid fed in to return liquid and liquid raw argon condensed.
  • the liquid crude argon product can be withdrawn from the crude argon column or one further fine cleaning in a pure argon column to obtain pure argon product with 0.1 to 10 ppm residual oxygen content.
  • the top condenser of the crude argon column sucks process gas from below argon-oxygen pre-separation and nitrogen-oxygen separation arranged so-called argon enrichment section of the low pressure column, by condensing the top argon product of the crude argon column and so on Pressure drop generated.
  • the suction power of the top condenser of the crude argon column is regulated either by pressure control on the bath side or via that on the side of the Argon side gas flows are available and by throttling the return
  • the condensation area of the crude argon top condenser can be enlarged or reduced.
  • the invention also relates to a device for the production of argon according to the Features of claims 4 to 9.
  • the number of separation stages in the crude argon column can be reduced in such a way that without a complete section and thus the argon-oxygen separation can be carried out economically in a column and thus the apparatus and procedural effort is significantly reduced, making it cost-effective and thus economic production of argon is guaranteed.
  • the figure of the drawing shows a in a schematic side section arrangement Low pressure column 1 of a rectification system of an air separation plant, which a line network 11, 12, 16, 17 with a crude argon column 10 for the extraction of Oxygen, nitrogen and argon are connected.
  • upper section of the low pressure column 1 is through a partition 3 from an outer, arranged below the upper section Argon-oxygen pre-separation 4 and an internal one, from the argon-oxygen pre-separation 4 preferably concentrically enclosed nitrogen-oxygen separation 5 arranged gas-tight separated.
  • the spatially separated argon-oxygen pre-separation 4 and nitrogen-oxygen separation 5 are with rectifying devices, shown only schematically in the form of differently arranged ordered packings and / or packing equipped.
  • the separation section of the low pressure column 1 also has conventionally arranged and trained liquid collector / distributor 6,7,9 and one with line 11 connected raw argon side deduction.
  • argon-oxygen pre-separation 4 and the nitrogen-oxygen separation 5 comprehensive separation section of the low pressure column 1 is one, only partially shown argon enrichment section 8 arranged.
  • the connected to the low-pressure column 1 via the line assembly 11, 12, 16, 17 and a line 13 for the crude argon discharge, a line 15 for supplying Top product and a line 18 for supplying cooling medium and one Head condenser 14 having crude argon column 10 is only schematic with shown conventional, arranged differently in several sections Bottoms and / or ordered packings and / or packing.
  • the pressure column of the rectification system is the pre-compressed, cleaned and cooled Air pre-decomposed, 1 liquid evaporates in the bottom of the low pressure column, which after flowing through the argon enrichment section 8 on the internal nitrogen-oxygen separation 5 and the outer argon-oxygen pre-separation 4 and so on using the rectifiers into a gaseous argon-oxygen fraction and in a nitrogen-oxygen gas mixture with residual contents Argon is further decomposed by about 2%.
  • the argon-oxygen gas mixture rectified in the argon-oxygen pre-separation 4 with an argon content of up to about 80 vol.% is preferred over that with a Throttle-equipped line 11 in the lower region of the crude argon column 10 fed in and in this by means of rectifying via line 15 removable head product disassembled.
  • the gaseous argon overhead of the crude argon column 10 is by means of indirect heat exchange preferred with relaxed sump liquid from the Pressure column of the rectification system fed raw argon condenser 14 at least partly to reflux liquid and a crude argon product with 0.01 ppm to 3% Residual oxygen content condensed.
  • the crude argon product obtained in this way can be obtained as a liquid crude argon product from the Raw argon column 10 deducted and / or a further fine cleaning in one Pure argon column to obtain pure argon product.
  • the sump liquid is in the Line 12 arranged conveyor 19 as a return for the external argon-oxygen pre-separation 4 transported to the low pressure column 1 while out of the room of the raw argon condenser 14 both a line 16 for rinsing liquid and one Lead gas line 17 to low-pressure column 1 and there above the internal nitrogen-oxygen separation 5 are arranged.
  • a line 16 for rinsing liquid and one Lead gas line 17 to low-pressure column 1 and there above the internal nitrogen-oxygen separation 5 are arranged.
  • At the top of the crude argon column 10 takes place over the line 18 an additional feed of cooling medium, preferably from the Bottom of the pressure column, not shown, removed and precooled liquid.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

A separate rectification of an argon-oxygen mixture using recycled liquid from the crude argon column (10) is carried out in the low pressure column (1). Recovering argon in an air decomposition plant comprises decomposing compressed, pre-purified cooled air in a rectification system equipped with a rectification column and a crude argon column (10). An argon-oxygen mixture formed in a low pressure column (1) of the rectification system having rectifying devices and injected into the crude argon column equipped with rectification devices and a head condenser (14) is decomposed to crude argon head product and a sump liquid. A separate rectification of an argon-oxygen mixture using recycled liquid from the crude argon column (10) is carried out in the low pressure column (1). An Independent claim is also included for an apparatus for recovering argon.

Description

Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Gewinnung von Argon, bei dem verdichtete, vorgereinigte und abgekühlte Luft in einem Rektifiziersystem mit mindestens einer Rektifiziersäule und einer Rohargonsäule zerlegt wird, nach den Merkmalen des Oberbegriffs von Anspruch 1 und 4.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 4.

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 Kopfkondensator 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 Sumpfver-dampfer 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 a top condenser equipped raw argon column supplied and in this at the same Pressure ratios as in the low pressure column using 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 bottom 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 maximal 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 Kopfkondensator 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 theoretischen Böden in Form von konventionellen Böden und/oder geordneten Packungen und/oder Füllkörpern in der Rohargon-/Halbreinsäule auf mindestens 30 bzw. 60 verringert werden kann, sodass kein Kopfkondensator 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 a maximum of 10 ppm residual oxygen known, in which that 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 top condenser to an argon product is broken down, the residual fraction of the semi-pure column as reflux liquid for the Crude argon column is used, the number of argon rectification used theoretical floors in the form of conventional floors and / or ordered packings and / or packing in the crude argon / semi-pure column can be reduced at least 30 or 60, so that no head capacitor in the Crude argon column is required, which reduces the expenditure on equipment and the Operating costs can be reduced.

Bei derartigen Luftzerlegungsanlagen sind die Rektifiziersäulen in der Regel so ausgeführt, dass die Trennsektion den gesamten Kolonnen-Durchmesser einnimmt, dessen Grösse von der in der Kolonne aufströmenden Gasmenge abhängig ist.In such air separation plants, the rectification columns are usually like this made that the separation section takes up the entire column diameter, the size of which depends on the amount of gas flowing in the column.

Bei einer herkömmlichen Niederdrucksäule des Rektifiziersystems wird etwa ein Drittel des Gasstroms im Bereich des sogenannten Argonbauchs zur Rohargonkolonne abgezogen, die restlichen zwei Drittel des Gasstroms durchströmen die oberhalb des Argonbauchs angeordneten Niederdrucksäulen-Bereiche.In a conventional low pressure column of the rectification system, about a third of the gas flow in the area of the so-called argon belly to the crude argon column deducted, the remaining two thirds of the gas stream flow through the above the Argon belly arranged low pressure column areas.

Bei herkömmlichen Niederdruckkolonnen, die mit geordneten Packungen ausgeführt werden, muss durch zusätzliche bauliche Maßnahmen der Tatsache Rechnung getragen werden, dass die Sektion oberhalb des Seitengasabzuges und unterhalb der Gasrückleitung vom Rohargonkondensator mit etwa ein Drittel weniger Gas beaufschlagt wird, indem entweder der Kolonnendurchmesser oder der freie Strömungsquerschnitt der betroffenen Sektion durch zusätzliche Einbauten bei gleichbleibendem Kolonnendurchmesser verkleinert wird. Beide Maßnahmen erhöhen den baulichen Aufwand der Kolonne in beträchtlichem Umfang.With conventional low-pressure columns, which are carried out with orderly packing must be taken into account by additional structural measures that the section above the side gas vent and below the Gas return from the crude argon condenser with about a third less gas is applied by either the column diameter or the free Flow cross section of the affected section through additional internals constant column diameter is reduced. Increase both measures the construction effort of the column to a considerable extent.

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 for the particularly economical extraction of raw argon are available to deliver.

Diese Aufgabe wird durch ein Verfahren und eine Vorrichtung mit den Merkmalen von Anspruch 1 und 4 gelöst.This object is achieved by a method and a device with the features of Claims 1 and 4 solved.

Erfindungsgemäß findet in der Niederdrucksäule unterhalb des Argon-Seitengas-Abzugsbereiches eine von der Stickstoff-Sauerstoff-Trennung räumlich getrennte Argon-Sauerstoff-Vortrennung statt, wodurch der Argon-Anteil im zur Rohargon-kolonne abgezogenen Argon-Sauerstoff-Seitengas bis auf etwa 80% erhöht und damit der nachfolgende Trennungsaufwand in der Rohargonsäule wesentlich gesenkt wird.According to the invention takes place in the low pressure column below the argon side gas discharge area one spatially separated from the nitrogen-oxygen separation Argon-oxygen pre-separation takes place, whereby the argon portion in the crude argon column withdrawn argon-oxygen side gas increased to about 80% and thus the subsequent separation effort in the crude argon column is significantly reduced.

Durch die Nutzung der Niederdruckkolonne zur Vortrennung des in der Rohargon-kolonne weiter zu verarbeitenden Argon-Sauerstoff-Gemisches wird die Wirtschaftlichkeit der Argon-Gewinnung wesentlich verbessert.By using the low pressure column to pre-separate the crude argon column further processing of the argon-oxygen mixture will result in economy the argon production improved significantly.

Dazu ist die, die Stickstoff-Sauerstoff-Vortrennung bevorzugt konzentrisch umschließende, äußere Argon-Sauerstoff-Vortrennung mittels einer Trennwand in ihrem oberen Bereich von der Stickstoff-Sauerstoff-Trennung und von der oberhalb der Argon-Sauerstoff-Vortrennung und Stickstoff-Sauerstoff-Trennung angeordneten Sektion der Niederdrucksäule gasdicht abgetrennt.For this purpose, the nitrogen-oxygen pre-separation is preferably concentric enclosing outer argon-oxygen pre-separation by means of a partition in their upper range from the nitrogen-oxygen separation and from that above the Argon-oxygen pre-separation and nitrogen-oxygen separation arranged Section of the low pressure column separated gastight.

Die den bisher bei den herkömmlichen Niederdrucksäulen vorhandenen Säuleneinschnürungsbereich nutzende Argon-Sauerstoff-Vortrennung ist - ebenso wie die Stickstoff-Sauerstoff-Trennung - mit Rektifiziereinrichtungen in Form von unterschiedlich angeordneten konventionellen Böden, vorzugsweise Rundlaufbögen, und/oder geordneten Packungen und/oder Füllkörpern ausgebildet.The column constriction area that was previously available with conventional low pressure columns argon-oxygen pre-separation is - just like that Nitrogen-oxygen separation - with rectifiers in the form of different arranged conventional floors, preferably circular arches, and / or ordered packings and / or packing.

In der Stickstoff-Sauerstoff-Trennung der Niederdrucksäule wird Sauerstoff von dem oberen zum unteren Säulenbereich angereichert, wobei aufgrund der unterschiedlichen Siedetemperaturen von Sauerstoff und Stickstoff die Eintrittstemperatur des Gasgemisches deutlich höher ist als die Austrittstemperatur.In the nitrogen-oxygen separation of the low pressure column, oxygen is removed from the enriched upper to lower pillar area, due to the different Boiling temperatures of oxygen and nitrogen the inlet temperature of the Gas mixture is significantly higher than the outlet temperature.

Aufgrund der sich nicht stark unterscheidenden Siedetemperaturen von Argon und Sauerstoff entsteht in der äußeren Argon-Sauerstoff-Vortrennung der Niederdrucksäule kein so großes Temperaturgefälle wie in der inneren Stickstoff-Sauerstoff-Trennung der Niederdrucksäule.Due to the not very different boiling temperatures of argon and Oxygen is generated in the outer argon-oxygen pre-separation of the low pressure column not as great a temperature gradient as in the internal nitrogen-oxygen separation of the Low pressure column.

Obwohl die Temperatur zwischen der inneren Stickstoff-Sauerstoff-Trennung und der äußeren Argon-Sauerstoff-Vortrennung differieren, werden über die Trennungswand von beiden Trennungseinrichtungen nur so geringe Wärmemengen transportiert, dass die Stickstoff-Sauerstoff-Trennung in der Niederdrucksäule nur unwesentlich beeinflusst wird.Although the temperature between the internal nitrogen-oxygen separation and the Outer argon-oxygen pre-separation will differ across the partition only so small amounts of heat are transported by both separation devices that the nitrogen-oxygen separation in the low pressure column is only insignificant being affected.

Die erfindungsgemäße gasdichte Trennung der Argon-Sauerstoff-Vortrennung von der Stickstoff-Sauerstoff-Trennung und dieser beiden Trennungseinrichtungen von der oberhalb der Trennungssektion angeordneten, eine gasförmige Fraktion mit bis zu 40% Stickstoffanteil enthaltenen Sektion der Niederdrucksäule ist erforderlich, um der Rohargonsäule einen stickstoffarmen Argon-Seitenabzug zu einem störungs-freien, optimalen Betrieb des Rohargonkondensators zuführen zu können.The gas-tight separation of the argon-oxygen pre-separation according to the invention from the Nitrogen-oxygen separation and these two separation devices from the a gaseous fraction up to 40% above the separation section Section of the low pressure column containing nitrogen is required to the Raw argon column a low-nitrogen argon side vent to a trouble-free, to be able to perform optimal operation of the crude argon condenser.

Als Rücklauf zur separaten Argon-Sauerstoff-Vortrennung in der Niederdrucksäule findet Sumpfprodukt aus der Rohargonsäule Verwendung.As a return to the separate argon-oxygen pre-separation in the low pressure column swamp product from the raw argon column is used.

Das in der Argon-Sauerstoff- Vortrennung der Niederdrucksäule gebildete, einen Argonanteil bis zu 80 Vol.-% aufweisende Rohargon wird oberhalb des Sumpfes der mit unterschiedlich angeordneten geordneten Packungen und/oder Füllkörpem und einem Kopfkondensator ausgerüsteten Rohargonsäule eingespeist und in dieser unter üblichen Prozessbedingungen zu gasförmiges Rohargonprodukt und zu einer ersten schwerersiedenden flüssigen Fraktion rektifiziert.The one formed in the argon-oxygen pre-separation of the low pressure column Raw argon containing up to 80 vol differently arranged ordered packings and / or packing and one Capacitor equipped raw argon column and fed into this usual process conditions for gaseous crude argon product and for a first one heavy boiling liquid fraction rectified.

Das im Ergebnis der Rektifikation des Argon-Seitengases in der Rohargonsäule als gasförmiges Kopfprodukt vorliegende Rohargon wird als Rohargonprodukt aus der Rohargonsäule abgezogen und mittels des Kopfkondensators durch indirekten Wärmeaustausch bevorzugt gegen aus der Drucksäule der Rektifiziersäule eingespeiste Sumpfflüssigkeit zu Rücklaufflüssigkeit und zu flüssigem Rohargon kondensiert.The result of rectification of the argon side gas in the crude argon column as Gaseous top product crude argon is the crude argon product from the Raw argon column deducted and by means of the overhead condenser by indirect Heat exchange preferably against from the pressure column of the rectification column Bottom liquid fed in to return liquid and liquid raw argon condensed.

Das flüssige Rohargonprodukt kann aus der Rohargonsäule abgezogen oder einer weiteren Feinreinigung in einer Reinargonsäule zur Gewinnung von Reinargon-produkt mit 0,1 bis 10 ppm Restsauerstoffanteil unterzogen werden.The liquid crude argon product can be withdrawn from the crude argon column or one further fine cleaning in a pure argon column to obtain pure argon product with 0.1 to 10 ppm residual oxygen content.

Dazu saugt der Kopfkondensator der Rohargonsäule Prozessgas aus der, unterhalb der Argon-Sauerstoff-Vortrennung und der Stickstoff-Sauerstoff-Trennung angeordneten sogenannten Argon-Anreicherungsektion der Niederdrucksäule an, indem er das Argon-Kopfprodukt der Rohargonsäule kondensiert und so ein Druckgefälle erzeugt.For this purpose, the top condenser of the crude argon column sucks process gas from below argon-oxygen pre-separation and nitrogen-oxygen separation arranged so-called argon enrichment section of the low pressure column, by condensing the top argon product of the crude argon column and so on Pressure drop generated.

Die Regulierung der Saugleistung des Kopfkondensators der Rohargonsäule erfolgt entweder durch Druckkontrolle auf dessen Badseite oder über die auf der Seite des Argon-Seitengastroms zur Verfügung stehenden und durch Androsseln den Rücklauf vergrößer- bzw. verkleinerbaren Kondensationsfläche des Rohargon-Kopfkondensators.The suction power of the top condenser of the crude argon column is regulated either by pressure control on the bath side or via that on the side of the Argon side gas flows are available and by throttling the return The condensation area of the crude argon top condenser can be enlarged or reduced.

Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von Argon nach den Merkmalen der Patentansprüche 4 bis 9.The invention also relates to a device for the production of argon according to the Features of claims 4 to 9.

Durch die erfindungsgemäße Argon-Sauerstoff-Vortrennung in der Niederdrucksäule kann die Anzahl der Trennstufen in der Rohargonsäule derart verringert werden, dass auf eine komplette Sektion verzichtet und so die Argon-Sauerstoff-Trennung wirtschaftlich in einer Kolonne ausgeführt werden kann und somit der apparative und verfahrenstechnische Aufwand wesentlich gesenkt wird, wodurch eine kosten-günstige und damit wirtschaftliche Gewinnung von Argon gewährleistet ist. Due to the argon-oxygen pre-separation according to the invention in the low pressure column the number of separation stages in the crude argon column can be reduced in such a way that without a complete section and thus the argon-oxygen separation can be carried out economically in a column and thus the apparatus and procedural effort is significantly reduced, making it cost-effective and thus economic production of argon is guaranteed.

Die Erfindung wird im folgenden anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispieles näher erläutert.The invention is illustrated below with reference to one in the drawing illustrated embodiment explained in more detail.

Die Figur der Zeichnung zeigt in einer schematischen Seitenschnitt-Anordnung eine Niederdrucksäule 1 eines Rektifiziersystems einer Luftzerlegungsanlage, welche über ein Leitungsverbund 11, 12, 16, 17 mit einer Rohargonsäule 10 zur Gewinnung von Sauerstoff, Stickstoff und Argon verbunden ist.The figure of the drawing shows a in a schematic side section arrangement Low pressure column 1 of a rectification system of an air separation plant, which a line network 11, 12, 16, 17 with a crude argon column 10 for the extraction of Oxygen, nitrogen and argon are connected.

Die nur teilweise bildlich dargestellte, mit üblichen Rektifiziereinrichtungen in Form von unterschiedlich angeordneten geordneten Packungen und/oder Füllkörpern und einen Flüssigkeitsverteiler 2 ausgerüstete, obere Sektion der Niederdrucksäule 1 ist durch eine Trennwand 3 von einer, unterhalb der oberen Sektion angeordneten, äußeren Argon-Sauerstoff-Vortrennung 4 und einer inneren, von der Argon-Sauerstoff-Vortrennung 4 bevorzugt konzentrisch umschlossenen Stickstoff-Sauerstoff-Trennung 5 gasdicht abgetrennt angeordnet.The only partially illustrated, with conventional rectification in the form of differently arranged ordered packings and / or packing and one Liquid distributor 2 equipped, upper section of the low pressure column 1 is through a partition 3 from an outer, arranged below the upper section Argon-oxygen pre-separation 4 and an internal one, from the argon-oxygen pre-separation 4 preferably concentrically enclosed nitrogen-oxygen separation 5 arranged gas-tight separated.

Die räumlich voneinander getrennte Argon-Sauerstoff-Vortrennung 4 und StickstoffSauerstoff-Trennung 5 sind mit, nur schematisch dargestellten Rektifizierein-richtungen in Form von unterschiedlich angeordneten geordneten Packungen und/oder Füllkörpern ausgerüstet.The spatially separated argon-oxygen pre-separation 4 and nitrogen-oxygen separation 5 are with rectifying devices, shown only schematically in the form of differently arranged ordered packings and / or packing equipped.

Die Trennsektion der Niederdrucksäule 1 weist zudem herkömmlich angeordnete und ausgebildete Flüssigkeitssammler/-verteiler 6,7,9 und einen mit der Leitung 11 verbundenen Rohargon-Seitenabzug auf.The separation section of the low pressure column 1 also has conventionally arranged and trained liquid collector / distributor 6,7,9 and one with line 11 connected raw argon side deduction.

Unterhalb der die Argon-Sauerstoff-Vortrennung 4 und die Stickstoff-Sauerstoff-Trennung 5 umfassenden Trennsektion der Niederdrucksäule 1 ist eine, nur teilweise dargestellte Argon-Anreicherungssektion 8 angeordnet.Below the the argon-oxygen pre-separation 4 and the nitrogen-oxygen separation 5 comprehensive separation section of the low pressure column 1 is one, only partially shown argon enrichment section 8 arranged.

Die über den Leitungsverbund 11, 12, 16, 17 mit der Niederdrucksäule 1 verbundene und eine Leitung 13 für den Rohargonabzug, eine Leitung 15 zur Zuführung von Kopfprodukt und eine Leitung 18 zur Zuführung von Kühlmedium und einen Kopfkondensator 14 aufweisende Rohargonsäule 10 ist mit nur schematisch dargestellten, in mehreren Sektionen unterschiedlich angeordneten konventionellen Böden und/oder geordneten Packungen und/oder Füllkörpern ausgerüstet.The connected to the low-pressure column 1 via the line assembly 11, 12, 16, 17 and a line 13 for the crude argon discharge, a line 15 for supplying Top product and a line 18 for supplying cooling medium and one Head condenser 14 having crude argon column 10 is only schematic with shown conventional, arranged differently in several sections Bottoms and / or ordered packings and / or packing.

In einer nicht dargestellten mit der Niederdrucksäule 1 thermisch gekoppelten Drucksäule des Rektifiziersystems wird die vorverdichtete, gereinigte und abgekühlte Luft vorzerlegt, wobei im Sumpf der Niederdrucksäule 1 Flüssigkeit verdampft, die sich nach dem Durchströmen der Argon-Anreicherungsektion 8 auf die innere Stickstoff-Sauerstoff-Trennung 5 und die äussere Argon-Sauerstoff-Vortrennung 4 aufteilt und so unter Verwendung der Rektifiziereinrichtungen in eine gasförmige Argon-Sauerstofffraktion und in ein Stickstoff-Sauerstoff-Gasgemisch mit Restgehalten an Argon von etwa 2 % weiterzerlegt wird.In a thermally coupled with the low pressure column 1, not shown The pressure column of the rectification system is the pre-compressed, cleaned and cooled Air pre-decomposed, 1 liquid evaporates in the bottom of the low pressure column, which after flowing through the argon enrichment section 8 on the internal nitrogen-oxygen separation 5 and the outer argon-oxygen pre-separation 4 and so on using the rectifiers into a gaseous argon-oxygen fraction and in a nitrogen-oxygen gas mixture with residual contents Argon is further decomposed by about 2%.

Das in der Argon-Sauerstoff-Vortrennung 4 rektifizierte Argon-Sauerstoff-Gas- gemisch mit einem Argon-Anteil von bis zu etwa 80 Vol.-% wird bevorzugt über die mit einer Drossel ausgerüstete Leitung 11 in den unteren Bereich der Rohargon-säule 10 eingespeist und in dieser mittels Rektifiziereinrichtungen zu über die Leitung 15 abziehbarem Kopfprodukt zerlegt.The argon-oxygen gas mixture rectified in the argon-oxygen pre-separation 4 with an argon content of up to about 80 vol.% is preferred over that with a Throttle-equipped line 11 in the lower region of the crude argon column 10 fed in and in this by means of rectifying via line 15 removable head product disassembled.

Das gasförmige Argon-Kopfprodukt der Rohargonsäule 10 wird mittels des durch indirekten Wärmeaustausch bevorzugt mit entspannter Sumpfflüssigkeit aus der Drucksäule des Rektifiziersystems gespeisten Rohargonkondensators 14 zumindest teilweise zu Rücklaufflüssigkeit und einem Rohargonprodukt mit 0,01 ppm bis 3 % Restsauerstoffgehalt kondensiert.The gaseous argon overhead of the crude argon column 10 is by means of indirect heat exchange preferred with relaxed sump liquid from the Pressure column of the rectification system fed raw argon condenser 14 at least partly to reflux liquid and a crude argon product with 0.01 ppm to 3% Residual oxygen content condensed.

Das derart gewonnene Rohargonprodukt kann als flüssiges Rohargonprodukt aus der Rohargonsäule 10 abgezogen und/oder einer weiteren Feinreinigung in einer Reinargonkolonne zur Gewinnung von Reinargonprodukt unterzogen werden.The crude argon product obtained in this way can be obtained as a liquid crude argon product from the Raw argon column 10 deducted and / or a further fine cleaning in one Pure argon column to obtain pure argon product.

Aus dem Sumpf der Rohargonsäule 10 wird die Sumpfflüssigkeit mittels einer in der Leitung 12 angeordneten Fördereinrichtung 19 als Rücklauf für die äussere Argon-Sauerstoff-Vortrennung 4 zur Niederdrucksäule 1 transportiert, während aus dem Raum des Rohargonkondensators 14 sowohl eine Leitung 16 für Spülflüssigkeit als auch eine Gasleitung 17 zur Niederdrucksäule 1 führen und dort oberhalb der inneren Stickstoff-Sauerstoff-Trennung 5 angeordnet sind. Am Kopf der Rohargonsäule 10 erfolgt über die Leitung 18 eine zusätzliche Einspeisung von Kühlmedium, vorzugsweise aus dem Sumpf der nicht dargestellten Drucksäule entnommene und vorgekühlte Flüssigkeit.From the bottom of the crude argon column 10, the sump liquid is in the Line 12 arranged conveyor 19 as a return for the external argon-oxygen pre-separation 4 transported to the low pressure column 1 while out of the room of the raw argon condenser 14 both a line 16 for rinsing liquid and one Lead gas line 17 to low-pressure column 1 and there above the internal nitrogen-oxygen separation 5 are arranged. At the top of the crude argon column 10 takes place over the line 18 an additional feed of cooling medium, preferably from the Bottom of the pressure column, not shown, removed and precooled liquid.

Claims (9)

Verfahren zur Gewinnung von Argon, bei dem verdichtete, vorgereinigte und abgekühlte Luft in einem Rektifiziersystem mit mindestens einer Rektifizier-säule und einer Rohargonsäule zerlegt wird, wobei ein in einer mit Rektifiziereinrichtungen ausgerüstete Niederdrucksäule des Rektifiziersystems gebildetes und in die mit Rektifiziereinrichtungen und einem Kopfkondensator ausgerüstete Rohargonsäule eingespeistes Argon-Sauerstoff-Gemisch zu Rohargon-Kopfprodukt und Sumpfflüssigkeit zerlegt wird,
gekennzeichnet dadurch, dass in der Niederdrucksäule (1) eine separate Rektifizierung des Argon-Sauerstoff-Gemisches unter Verwendung von Rücklaufflüssigkeit der Rohargonsäule (10) erfolgt.
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 a crude argon column, a crude argon column formed in a low-pressure column of the rectification system equipped with rectifiers and into which is equipped with rectifiers and a top condenser the fed argon-oxygen mixture is broken down into crude argon top product and bottom liquid,
characterized in that a separate rectification of the argon-oxygen mixture takes place in the low pressure column (1) using the reflux liquid of the crude argon column (10).
Verfahren nach Anspruch 1,
dadurch gekennzeichnet, dass das in der Argon-Sauerstoff-Vortrennung (4) der Niederdrucksäule (1) das Argon-Sauerstoff-Gasgemisch bis zu einem Argon-Anteil von 80 Vol.-% zerlegt wird.
Method according to claim 1,
characterized in that the argon-oxygen gas mixture in the argon-oxygen pre-separation (4) of the low-pressure column (1) is broken down to an argon content of 80% by volume.
Verfahren nach Anspruch 1 oder 2,
dadurch gekennzeichnet, dass in der Niederdrucksäule (1) die Argon-Sauerstoff-Vortrennung (4) und Stickstoff-Sauerstoff-Trennung (5) unter annähernd gleichen Temperatur- und Druckverhältnissen erfolgen.
The method of claim 1 or 2,
characterized in that in the low pressure column (1) the argon-oxygen pre-separation (4) and nitrogen-oxygen separation (5) take place under approximately the same temperature and pressure conditions.
Vorrichtung zur Gewinnung von Argon nach einem der Ansprüche 1 bis 3 mit einem Rektifiziersystem mit mindestens einer Rektifiziersäule und einer Rohargonsäule, wobei die Rektifiziersäule im wesentlichen aus mindestens einer mit einer Drucksäule durch einen Hauptkondensator thermisch gekoppelten und mit unterschiedlich angeordneten geordneten Packungen und/oder Füllkörpern ausgerüsteten Niederdrucksäule besteht, welche mittels Produktleitungen mit der konventionelle Böden und/oder geordnete Packungen und/oder Füllkörper und einen Kopfkondensator aufweisenden Rohargonsäule verbunden ist,
dadurch gekennzeichnet, dass die Niederdrucksäule (1) eine Argon-Sauerstoff-Vortrennung (4) und eine Stickstoff-Sauerstoff-Trennung (5) aufweist.
Device for the production of argon according to one of claims 1 to 3 with a rectification system with at least one rectification column and a crude argon column, the rectification column consisting essentially of at least one thermally coupled to a pressure column by a main condenser and equipped with differently arranged ordered packings and / or packing elements Low pressure column, which is connected by means of product lines to the conventional trays and / or ordered packings and / or packing and a crude argon column having a top condenser,
characterized in that the low pressure column (1) has an argon-oxygen pre-separation (4) and a nitrogen-oxygen separation (5).
Vorrichtung nach Anspruch 4,
dadurch gekennzeichnet, dass die Argon-Sauerstoff-Vortrennung (4) und die Stickstoff-Sauerstoff-Trennung (5) in der gleichen Sektion der Niederdrucksäule (1) angeordnet sind.
Device according to claim 4,
characterized in that the argon-oxygen pre-separation (4) and the nitrogen-oxygen separation (5) are arranged in the same section of the low-pressure column (1).
Vorrichtung nach Anspruch 4 oder 5,
gekennzeichnet dadurch, dass die Argon-Sauerstoff-Vortrennung (4) die Stickstoff-Sauerstoff-Trennung (5) vorzugsweise umschließt.
Device according to claim 4 or 5,
characterized in that the argon-oxygen pre-separation (4) preferably encloses the nitrogen-oxygen separation (5).
Vorrichtung nach Anspruch 6,
dadurch gekennzeichnet, dass die Argon-Sauerstoff-Vortrennung (4) die Stickstoff-Sauerstoff-Trennung (5) vorzugsweise konzentrisch umschließt.
Device according to claim 6,
characterized in that the argon-oxygen pre-separation (4) preferably surrounds the nitrogen-oxygen separation (5) concentrically.
Vorrichtung nach einem der Ansprüche 4 bis 7,
dadurch gekennzeichnet, dass die Argon-Sauerstoff-Vortrennung (4) und die Stickstoff-Sauerstoff-Trennung (5) in ihrem oberen Bereich mittels einer Trennwand (3) voneinander und von einer oberhalb angeordneten Sektion der Niederdrucksäule (1) gasdicht abgetrennt angeordnet sind.
Device according to one of claims 4 to 7,
characterized in that the argon-oxygen pre-separation (4) and the nitrogen-oxygen separation (5) are arranged in a gas-tight manner in their upper region by means of a partition (3) from one another and from a section of the low-pressure column (1) arranged above.
Vorrichtung nach einem der Ansprüche 4 bis 8,
gekennzeichnet dadurch, dass die Niederdrucksäule (1) einen konstanten Säulen-Durchmesser aufweist.
Device according to one of claims 4 to 8,
characterized in that the low pressure column (1) has a constant column diameter.
EP01113970A 2000-06-10 2001-06-08 Process and device for argon recovery Withdrawn EP1162423A3 (en)

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