EP0384483B1 - Air rectification process and apparatus - Google Patents

Air rectification process and apparatus Download PDF

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Publication number
EP0384483B1
EP0384483B1 EP90103572A EP90103572A EP0384483B1 EP 0384483 B1 EP0384483 B1 EP 0384483B1 EP 90103572 A EP90103572 A EP 90103572A EP 90103572 A EP90103572 A EP 90103572A EP 0384483 B1 EP0384483 B1 EP 0384483B1
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EP
European Patent Office
Prior art keywords
nitrogen
pressure
compressed
stage
pressure stage
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Expired - Lifetime
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EP90103572A
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German (de)
French (fr)
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EP0384483A2 (en
EP0384483A3 (en
Inventor
Dietrich Dipl.-Ing. Rottmann
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Linde GmbH
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Linde GmbH
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Priority to DE19893905521 priority Critical patent/DE3905521A1/en
Priority to DE3905521 priority
Priority to EP19890113815 priority patent/EP0383994A3/en
Priority to EP89113815 priority
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP0384483A2 publication Critical patent/EP0384483A2/en
Publication of EP0384483A3 publication Critical patent/EP0384483A3/en
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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
    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04769Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854Safety aspects of operation
    • F25J3/0486Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
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    • 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
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    • 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
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    • 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
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    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/0423Subcooling of liquid process streams
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    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
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    • F25J3/04315Lowest pressure or impure nitrogen, so-called waste nitrogen expansion
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    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
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    • F25J3/04327Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of argon or argon enriched stream
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    • 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
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    • 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
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    • 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
    • F25J3/04709Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
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    • F25J2200/20Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
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    • F25J2230/52Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being oxygen enriched compared to air, e.g. "crude oxygen"
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    • 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
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    • F25J2250/40One fluid being air
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    • F25J2250/30External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50One fluid being oxygen
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00Refrigeration
    • Y10S62/923Inert gas
    • Y10S62/924Argon

Description

  • Die Erfindung betrifft ein Verfahren zur Luftzerlegung durch Rektifikation, bei dem Luft verdichtet, vorgereinigt, abgekühlt und in der Druckstufe einer zweistufigen Rektifikation in eine stickstoffreiche Fraktion und in eine sauerstoffreiche Flüssigkeit vorzerlegt wird und die beiden Fraktionen mindestens teilweise der Mitteldruckstufe der Rektifikation zugeführt und in Sauerstoff und Stickstoff zerlegt werden, wobei mindestens eine gasförmige Stickstofffraktion aus der Mitteldruckstufe herausgeführt, angewärmt und mindestens teilweise verdichtet wird. Gegenstand der Erfindung ist außerdem eine Vorrichtung zur Durchfürung des Verfahrens mit den Merkwalen des ersten Teils des Anspruchs 6.The invention relates to a method for air separation by rectification, in which air is compressed, pre-cleaned, cooled and pre-separated in the pressure stage of a two-stage rectification into a nitrogen-rich fraction and an oxygen-rich liquid, and the two fractions are at least partially fed to the medium-pressure stage of the rectification and in oxygen and nitrogen are broken down, with at least one gaseous nitrogen fraction being led out of the medium pressure stage, heated and at least partially compressed. The invention also relates to a device for carrying out the method with the flagpoles of the first part of claim 6.
  • Ein derartiges Verfahren und eine solche Vorrichtung sind aus der US-PS 2 666 303 bekannt. Hier wird Stickstoff aus der Mitteldruckstufe einer zweistufigen Rektifikation auf etwa Umgebungstemperatur angewärmt, verdichtet und anschließend als Produkt abgezogen. Dadurch kann der Stickstoff unter einem erhöhtem Druck abgegeben werden. Das vorbekannte Verfahren weist den Nachteil auf, daß auch bei relativ hohem Druck der Mitteldruckstufe die Druckdifferenz gegenüber der Atmosphäre nicht zur Kälteerzeugung ausgenützt werden kann. Verfahrenskälte wird hier vielmehr durch Entspannung eines Teils der Zerlegungsluft gewonnen, was eine Luftverdichtung auf sehr hohen Druck voraussetzt und daher wegen des entsprechenden Energieverbrauchs wirtschaftlich nicht zufriedenstellend ist.Such a method and such a device are known from US Pat. No. 2,666,303. Here, nitrogen from the medium pressure stage of a two-stage rectification is warmed up to about ambient temperature, compressed and then removed as a product. This allows the nitrogen to be released under an increased pressure. The known method has the disadvantage that the pressure difference with respect to the atmosphere cannot be used to generate cold, even at a relatively high pressure of the medium pressure stage. Process cold is rather obtained here by relaxing part of the decomposition air, which requires air compression at very high pressure and is therefore economically unsatisfactory due to the corresponding energy consumption.
  • Daneben ist aus der DE-B-25 48 222 ein Verfahren mit einem Stickstoff-Kältekreislauf bekannt, in dem Stickstoff aus der Druckstufe auf einen höheren Druck verdichtet, anschließend teilweise arbeitsleistend in etwa auf Druckstufendruck entspannt und in die Druckstufe zurückgespeist wird. Hierdurch kann zwar ein beträchtlicher Teil des Kältebedarfs der Luftzerlegungsanlage gedeckt werden, allerdings steht der Stickstoff nicht unter dem hohen Druck als Produkt zur Verfügung, sondern wird als Rücklauf in Druck- und Mitteldruckstufe der Rektifikation benötigt. Dieses Verfahren besitzt also ebenfalls Nachteile hinsichtlich seiner Wirtschaftlichkeit, insbesondere dann, wenn Stickstoff unter erhöhtem Druck gewonnen werden soll.In addition, from DE-B-25 48 222 a method with a nitrogen refrigeration cycle is known in which nitrogen is compressed from the pressure stage to a higher pressure, then expanded in a partially work-performing manner to approximately the pressure stage pressure and fed back into the pressure stage. Although this can cover a considerable part of the cooling requirements of the air separation plant, the nitrogen is not available as a product under the high pressure, but is required as a return flow in the pressure and medium pressure stage of the rectification. This process also has disadvantages with regard to its economy, especially when nitrogen is to be obtained under increased pressure.
  • Der Erfindung liegt die Aufgabe zugrunde, die Wirtschaftlichkeit des Verfahrens und der Vorrichtung der eingangs genannten Art zu verbessern und insbesondere auf besonders günstige Weise Verfahrenskälte zur Verfügung zu stellen, ohne dabei die Weiterverwendung der gasförmigen Stickstofffraktion, insbesondere für Anwendungen, die ein erhöhtes Druckniveau erfordern, einzuschränken.The object of the invention is to improve the economy of the method and the device of the type mentioned at the outset and, in particular, to provide process cooling in a particularly advantageous manner without the reuse of the gaseous nitrogen fraction, in particular for applications which require an increased pressure level, restrict.
  • Diese Aufgabe wird dadurch gelöst, daß der Stickstoff vor der Verdichtung arbeitsleistend entspannt und erneut angewärmt wird, wobei die beim Entspannen gewonnene Kälte an einen oder mehrere andere Prozeßströme abgegeben wird und mindestens ein Teil der beim Entspannen gewonnenen Arbeit zum Verdichten des Stickstoffs verwendet wird.This object is achieved in that the nitrogen is relieved of work prior to compression and reheated, the cold obtained during the expansion being given off to one or more other process streams and at least part of the work obtained during expansion being used to compress the nitrogen.
  • Besonders günstig ist die arbeitsleistende Entspannung mit Rückverdichtung bei Luftzerlegungsanlagen anzuwenden, die unter erhöhtem Druck betrieben werden, da hier auch der Druck am Eingang der Entspannungsturbine relativ hoch ist und somit ein günstiger Wirkungsgrad erzielt werden kann. Dies gilt insbesondere für Luftzerleger, die im Verbund mit Kraftwerken stehen, die gemeinsam mit einer Kohle- oder Schwerölvergasung betrieben werden.The work-relieving expansion with recompression is particularly favorable to use in air separation plants which are operated under increased pressure, since the pressure at the inlet of the expansion turbine is also relatively high here and a favorable efficiency can thus be achieved. This applies in particular to air separators that are connected to power plants that are operated together with coal or heavy oil gasification.
  • Es erweist sich als vorteilhaft, wenn ein Teil der Leistung beim Verdichten durch von außerhalb des Verfahrens importierte Energie aufgebracht wird. Dadurch kann der entspannte Stickstoffanteil wieder auf seinen ursprünglichen Druck (vor dem Entspannen) oder auf einen höheren Druck gebracht werden, falls er mit den entsprechenden Parametern weiterverwendet werden soll. Beispielsweise kann der rückverdichtete Stickstoff bei einem Verbund zwischen Luftzerlegungsanlage und Kohlevergasungskraftwerk in die in der Regel unter erhöhtem Druck stehende Brennkammer geführt werden.It proves to be advantageous if part of the power during compression is applied by energy imported from outside the process. As a result, the expanded nitrogen content can be brought back to its original pressure (before the expansion) or to a higher pressure if it is to be used further with the appropriate parameters. For example, in the case of a network between the air separation plant and the coal gasification power plant, the recompressed nitrogen can be fed into the combustion chamber, which is generally under increased pressure.
  • Dabei ist es insbesondere vorteilhaft, wenn gemäß weiteren Merkmalen der Erfindung der arbeitsleistend entspannte Stickstoff auf einen Druck verdichtet wird, der im wesentlichen gleich dem Druck vor der arbeitsleistenden Entspannung ist, und außerdem der entspannte und wieder verdichtete Stickstoff wieder dem nicht entspannten Teil der gasförmigen Stickstofffraktion aus der Mitteldruckstufe zugeführt wird.It is particularly advantageous if, according to further features of the invention, the nitrogen which has been relieved of work is compressed to a pressure which is substantially equal to the pressure prior to the relaxation of work, and the relaxed and re-compressed nitrogen is again the non-expanded part of the gaseous nitrogen fraction is fed from the medium pressure stage.
  • Mit Hilfe dieser Verfahrensweise steht auch bei der erfindungsgemäßen Art der Kältegewinnung die gesamte gasförmige Stickstofffraktion unter dem (im allgemeinen erhöhten) Druck der Mitteldruckstufe zur Verfügung und kann beispielsweise in der Brennkammer eines Kohlevergasungskraftwerkes weiterverwendet werden.With the aid of this procedure, the entire gaseous nitrogen fraction is also available under the (generally increased) pressure of the medium pressure stage in the type of cold generation according to the invention and can be used, for example, in the combustion chamber of a coal gasification power plant.
  • Besonders bei solchen Anwendungen, bei denen die gesamte Luftzerlegung und insbesondere die Mitteldruckstufe bei relativ hohen Drücken gefahren werden muß, sind die erzielten Produktreinheiten oft nicht befriedigend. Dies gilt für den erzeugten Stickstoff, in besonderem Maße jedoch für das Sauerstoffprodukt.The product purities achieved are often unsatisfactory, particularly in those applications in which the entire air separation and in particular the medium pressure stage must be carried out at relatively high pressures. This applies to the nitrogen produced, but particularly to the oxygen product.
  • Aus diesem Grunde ist es in bestimmten Fällen günstig, wenn gemäß einem weiteren Aspekt der Erfindung der Mitteldruckstufe eine weitere Stickstofffraktion am Kopf entnommen, angewärmt, verdichtet, anschließend wieder abgekühlt und in die Druckstufe eingeführt wird. Die (Rein-)Stickstofffraktion wird also mindestens teilweise in einem sogenannten Verstärkungskreislauf geführt. Die über den Verstärkungskreislauf in die Druckstufe geleitete Stickstoffmenge wird in indirektem Wärmetausch mit Sumpfflüssigkeit der Mitteldruckstufe kondensiert, flüssig abgezogen und als zusätzliche Rücklaufmenge auf die Mitteldruckstufe aufgegeben. Dadurch wird - ohne Beeinflussung des Stoffaustausches in der Druckstufe - der Umsatz in der Mitteldruckstufe erhöht, so daß die Produktströme höhere Reinheiten aufweisen.For this reason, it is advantageous in certain cases if, according to a further aspect of the invention, a further nitrogen fraction is removed from the head of the medium pressure stage, heated, compressed, then cooled again and introduced into the pressure stage. The (pure) nitrogen fraction is therefore at least partially carried out in a so-called amplification circuit. The amount of nitrogen passed through the boost circuit into the pressure stage is condensed in indirect heat exchange with sump liquid of the medium pressure stage, drawn off in liquid form and added to the medium pressure stage as an additional return flow. As a result - without influencing the mass exchange in the pressure stage - the conversion in the medium pressure stage is increased so that the product streams have higher purities.
  • Die Erfindung betrifft auch eine Vorrichtung zur Durchführung des Verfahrens gemäß den Patentansprüchen 6 und 7 .The invention also relates to a device for carrying out the method according to claims 6 and 7.
  • Anhand der Zeichnung, in welcher eine Ausführungsform des erfindungsgemäßen Verfahrens schematisch dargestellt ist, werden die Erfindung und weitere Einzelheiten der Erfindung näher erläutert.The invention and further details of the invention are explained in more detail with reference to the drawing, in which an embodiment of the method according to the invention is shown schematically.
  • Über Leitung 1 wird verdichtete und vorgereinigte Luft herangeführt, in einem Hauptwärmetauscher 17 in indirektem Wärmeaustausch mit Produktströmen abgekühlt und in die Druckstufe 3 einer zweistufigen Rektifiziersäule 2 eingespeist. Die Druckstufe 3 (Betriebsdruck: 6 bis 20 bar, vorzugsweise 8 bis 17 bar) steht mit der Mitteldruckstufe 4 (Betriebsdruck: 1,5 bis 10 bar, vorzugsweise 2,0 bis 8,0 bar) über einen gemeinsamen Kondensator/Verdampfer 13 in wärmetauschender Verbindung. Die eingeführte Luft wird in der Druckstufe 3 in Stickstoff und in eine sauerstoffangereicherte Fraktion vorzerlegt. Die sauerstoffangereicherte Fraktion wird über Leitung 6 in flüssigem Zustand abgeführt, in Wärmetauscher 18 unterkühlt und in die Mitteldruckstufe 4 eingedrosselt. Stickstoff vom Kopf der Druckstufe 3 wird über Leitung 5 ebenfalls flüssig abgezogen, in Wärmetauscher 18 unterkühlt und zum einen Teil über Leitung 8 als flüssiges Produkt abgeführt. Der andere Teil des Stickstoffs aus der Druckstufe 3 wird über Leitung 9 als Rücklauf auf die Mitteldruckstufe 4 aufgegeben. Eine weitere flüssige Fraktion wird über Leitung 7 aus der Druckstufe 3 ab- und der Niederdruckstufe 4 zugeführt.Compressed and pre-cleaned air is introduced via line 1, cooled in a main heat exchanger 17 in indirect heat exchange with product streams and fed into pressure stage 3 of a two-stage rectification column 2. The pressure level 3 (operating pressure: 6 to 20 bar, preferably 8 to 17 bar) is with the medium pressure level 4 (operating pressure: 1.5 to 10 bar, preferably 2.0 to 8.0 bar) via a common condenser / evaporator 13 in heat exchanging connection. The introduced air is pre-divided in pressure stage 3 into nitrogen and into an oxygen-enriched fraction. The oxygen-enriched fraction is discharged in the liquid state via line 6, subcooled in heat exchanger 18 and throttled into the medium pressure stage 4. Nitrogen from the head of pressure stage 3 is also drawn off in liquid form via line 5, subcooled in heat exchanger 18 and partly discharged as a liquid product via line 8. The other part of the nitrogen from the pressure stage 3 is fed via line 9 as a return to the medium pressure stage 4. Another liquid fraction is discharged via line 7 from pressure stage 3 and fed to low pressure stage 4.
  • Als Produkte der Mitteldruckstufe 4 werden flüssiger Sauerstoff (Leitung 14), gasförmiger Reinstickstoff (Leitung 15) und unreiner Stickstoff (Leitung 16) entnommen und im Hauptwärmetauscher 17, die Stickstoffströme zusätzlich im Wärmetauscher 18, angewärmt.As products of medium pressure stage 4, liquid oxygen (line 14), gaseous pure nitrogen (line 15) and impure nitrogen (line 16) are removed and the nitrogen streams are additionally heated in the main heat exchanger 17, in the heat exchanger 18.
  • Vor der Einspeisung in die Druckstufe 3 kann ein Teil (Leitung 21) der Luft in Leitung 1 in Wärmetausch 20 mit Sauerstoff 14 aus dem Sumpf der Mitteldruckstufe 4 kondensiert werden. Die Flüssigkeit 14 aus dem Sumpf der Mitteldruckstufe 4 wird dazu mittels einer Pumpe 19 auf hohen Druck gebracht und bei dem Wärmeaustausch im Kondensator 20 teilweise verdampft. Die teilweise kondensierte Luft 22 wird oberhalb der ersten Einspeisestelle (Leitung 1) in die Druckstufe 3 eingeführt. Der verdampfte Anteil des Sauerstoffs wird über Leitung 23 abgeführt und angewärmt (17). Ein anderer Teil des Sauerstoffs wird über Leitung 42 als flüssiger Produktstrom abgezogen.Before feeding into pressure stage 3, part (line 21) of the air in line 1 can be condensed in heat exchange 20 with oxygen 14 from the bottom of medium pressure stage 4. The liquid 14 from the sump of the medium pressure stage 4 is brought to high pressure by means of a pump 19 and at which Heat exchange in the condenser 20 partially evaporates. The partially condensed air 22 is introduced into the pressure stage 3 above the first feed point (line 1). The vaporized portion of the oxygen is removed via line 23 and warmed (17). Another part of the oxygen is withdrawn via line 42 as a liquid product stream.
  • Erfindungsgemäß wird ein Teil des unreinen Stickstoffs in Leitung 16 auf einer mittleren Temperatur von etwa 110 bis 210 K, vorzugsweise 135 bis 185 K, über Leitung 30 aus dem Hauptwärmetauscher 17 abgezogen und in einer Entspannungsturbine 31 arbeitsleistend auf einen Druck von 2,6 bis 1,4 bar, vorzugsweise etwa 2,0 bar entspannt. Der entspannte Stickstoff wird über Leitung 32 erneut zum kalten Ende des Hauptwärmetauschers 17 geführt und auf etwa Umgebungstemperatur angewärmt. Er gibt dabei die beim Entspannen gewonnene Kälte an zu zerlegende Luft in Leitung 1 ab.According to the invention, part of the impure nitrogen in line 16 is drawn off from the main heat exchanger 17 via line 30 at an average temperature of approximately 110 to 210 K, preferably 135 to 185 K, and in a pressure-reducing turbine 31 to perform a pressure of 2.6 to 1 , 4 bar, preferably about 2.0 bar relaxed. The expanded nitrogen is again conducted via line 32 to the cold end of the main heat exchanger 17 and warmed to approximately ambient temperature. He releases the cold obtained during relaxation to air to be separated in line 1.
  • Um den entspannten Teil des Stickstoffs gemeinsam mit dem nicht entspannten Anteil (Leitung 39) abziehen zu können, wird dieser in zwei Stufen 33, 36 wieder verdichtet, wobei jeweils die Kompressionswärme anschließend entfernt wird (Kühler 35, 37). Die zweite Verdichtungsstufe 36 ist mit der Entspannungsturbine 31 gekoppelt, so daß die bei der Entspannung gewonnene Arbeit für das Verfahren zurückgewonnen wird. Um das Gas wieder auf seinen Anfangsdruck (in Leitung 30 bzw. 39) zu bringen ist jedoch eine weitere Verdichtungsstufe 33 erforderlich, die mit von außen eingebrachter Energie betrieben wird. Diese zusätzlich aufgewandte Energie wird jedoch durch die erfindungsgemäße Verfahrensweise außerordentlich effektiv in Verfahrenskälte umgesetzt.In order to be able to draw off the relaxed part of the nitrogen together with the non-relaxed portion (line 39), this is compressed again in two stages 33, 36, the compression heat then being removed in each case (cooler 35, 37). The second compression stage 36 is coupled to the expansion turbine 31, so that the work gained in the expansion is recovered for the process. In order to bring the gas back to its initial pressure (in line 30 or 39), however, a further compression stage 33 is required, which is operated with energy introduced from outside. However, this additional energy is converted extremely effectively into process cold by the procedure according to the invention.
  • Falls der Reinstickstoff unter einem höheren Druck als dem Mitteldruckstufe 4 benötigt wird, kann er nach seiner Erwärmung verdichtet werden. Dies geschieht im allgemeinen in mehreren Verdichterstufen 40, 41. Dabei wird in der Regel hinter jeder Stufe 40, 41 die Verdichtungswärme durch (in der Zeichnung nicht dargestellte) Wasserkühler abgeführt.If the pure nitrogen is required under a pressure higher than medium pressure level 4, it can be compressed after it has been heated. This is generally done in several compressor stages 40, 41. As a rule, each is behind Stage 40, 41 the heat of compression removed (not shown in the drawing) water cooler.
  • Besonders in diesem Fall ist es günstig, einen Verstärkungskreislauf zur Erhöhung von Umsatz und Produktreinheiten der Mitteldruckstufe vorzusehen. Dazu ist die in der Zeichnung gestrichelt dargestellte Leitung notwendig. Über Leitung 43 wird mindestens ein Teil des Reinstickstoffs aus Leitung 15 auf dem Druckniveau der Drucksäule (im Falle des Ausführungsbeispiel zwischen den Verdichterstufen 40 und 41) abgezweigt, im Hauptwärmetauscher 17 abgekühlt und weiter über Leitung 43 in die Druckstufe 3 eingespeist.In this case in particular, it is expedient to provide a reinforcement circuit for increasing the sales and product purities of the medium pressure stage. This requires the line shown in dashed lines in the drawing. At least part of the pure nitrogen from line 15 is branched off via line 43 at the pressure level of the pressure column (in the case of the exemplary embodiment between the compressor stages 40 and 41), cooled in the main heat exchanger 17 and further fed via line 43 into the pressure stage 3.
  • Der zusätzliche Stickstoff kondensiert an deren Kopf und verdampft dabei Flüssigkeit im Sumpf der Mitteldruckstufe 4. In flüssiger Form wird er zusätzlich über Leitung 5 entnommen und als Rücklauf auf die Mitteldrucksäule aufgegeben. Eine entsprechend erhöhte Stickstoffmenge wird dann auch über Leitung 15 abgezogen, angewärmt (18, 17) und in der Verdichterstufe 40 komprimiert, so daß sich der Verstärkungskreislauf schließt und die Bilanzen der Wärmetauscher 18 und 17 ausgeglichen sind.The additional nitrogen condenses at the top and thereby evaporates liquid in the bottom of the medium pressure stage 4. In liquid form, it is additionally removed via line 5 and fed as a return to the medium pressure column. A correspondingly increased amount of nitrogen is then drawn off via line 15, warmed (18, 17) and compressed in the compressor stage 40, so that the amplification circuit closes and the balances of the heat exchangers 18 and 17 are balanced.

Claims (7)

1. A process for the separation of air by rectification, wherein air (1) is compressed, pre-purified, cooled (17) and pre-separated in the pressure stage (3) of a two-stage rectification column (2) into a nitrogen-rich fraction (5) and an oxygen-rich liquid (6), and the two fractions (5, 6) are at least partially supplied to the medium pressure stage (4) of the rectification column (2) and separated into oxygen and nitrogen, wherein at least one gaseous nitrogen fraction is withdrawn (16) from the medium pressure stage (4), heated (17), and at least partially (32) compressed (33, 36), characterised in that prior to the compression (33, 36), the nitrogen is expanded (31), with production of work, and is re-heated (17), where the cold acquired by the expansion is fed to one or more other process stream (1, 43), and at least a part of the work obtained by the expansion (31) is used for the compression (36) of the nitrogen.
2. A process as claimed in Claim 1, characterised in that a part of the power for the compression (33) is applied by means of energy imported from outside of the process.
3. A process as claimed in Claim 1 or 2, characterised in that the nitrogen (32) which is expanded with production of work is compressed to a pressure (33, 36) which is substantially equal to the pressure prior to the work-producing expansion (31).
4. A process as claimed in Claim 3, characterised in that the expanded and re-compressed part (38) of the gaseous nitrogen fraction is returned to the non-expanded part (39) of the gaseous nitrogen fraction (16).
5. A process as claimed in one of Claims 1 to 4, characterised in that a further nitrogen fraction (15) is withdrawn from the head of the medium pressure stage (4), is heated (18, 17), compressed (40), then cooled again (17) and introduced (43) into the pressure stage (3).
6. A device for the execution of the process claimed in one of Claims 1 to 5, comprising a main heat exchanger (17) which contains passages for air (1) and for nitrogen (16, 39), and comprising a double rectifier column (2) composed of a pressure column (3) and a medium pressure column (4), where the passage for air (1) is connected to the pressure column (3) and the passage for nitrogen (16, 39) is connected to the med¡um pressure column (4), characterised by a line (30) which leads out from the central zone of the main heat exchanger (17) and is connected to the nitrogen passage (16) and to the input of an expansion turbine (31), and by a further line (32) which connects the output of the expansion turbine (31) to the input of a compressor (33, 36) and extends in the form of a passage through the main heat exchanger (17).
7. A device as claimed in Claim 6, characterised in that the output of the compressor (33, 36) is connected to the output of the nitrogen passage (39) of the main heat exchanger (17).
EP90103572A 1989-02-23 1990-02-23 Air rectification process and apparatus Expired - Lifetime EP0384483B1 (en)

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DE59000211D1 (en) 1992-08-27
JPH02245201A (en) 1990-10-01
EP0384483A2 (en) 1990-08-29
AU618659B2 (en) 1992-01-02
EP0383994A3 (en) 1990-11-07
EP0383994A2 (en) 1990-08-29
CN1025068C (en) 1994-06-15
CN1045173A (en) 1990-09-05
AU4996090A (en) 1990-08-30
US5036672A (en) 1991-08-06

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