EP0384213A2 - Air rectification process and apparatus - Google Patents

Air rectification process and apparatus Download PDF

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Publication number
EP0384213A2
EP0384213A2 EP90102355A EP90102355A EP0384213A2 EP 0384213 A2 EP0384213 A2 EP 0384213A2 EP 90102355 A EP90102355 A EP 90102355A EP 90102355 A EP90102355 A EP 90102355A EP 0384213 A2 EP0384213 A2 EP 0384213A2
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EP
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Prior art keywords
rectification
medium pressure
pressure stage
oxygen
crude argon
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Granted
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EP90102355A
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German (de)
French (fr)
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EP0384213A3 (en
EP0384213B1 (en
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Dietrich Dipl.-Ing. Rottmann
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Linde GmbH
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Linde GmbH
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Priority claimed from DE19893905521 external-priority patent/DE3905521A1/en
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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
    • 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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/0423—Subcooling of liquid process streams
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation 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
    • F25J3/04327—Generation 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
    • 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
    • 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
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes 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
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/52—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being oxygen enriched compared to air, e.g. "crude oxygen"
    • 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
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • Y—GENERAL 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/923—Inert gas
    • Y10S62/924—Argon

Definitions

  • the invention relates to a process for air separation by rectification, in which air is compressed, pre-cleaned, cooled and pre-separated into a nitrogen-rich fraction and an oxygen-rich liquid in the pressure stage of a two-stage rectification, 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 and in which an argon-containing oxygen stream is taken from the medium pressure stage and fed to crude argon rectification, and also a device for carrying out the method.
  • the crude argon rectification is carried out under the pressure under which the argon-containing oxygen fraction is removed from the medium pressure stage. Liquid oxygen is recycled from crude argon rectification to approximately the same point in the medium pressure stage.
  • Such a method is favorable if the medium pressure stage and thus the crude argon rectification are carried out essentially under atmospheric pressure.
  • oxygen and / or nitrogen, which are generated in the medium pressure stage are required under increased pressure, for example in coal gasification plants or for blowing nitrogen in during the extraction of oil or natural gas. It is economically more advantageous for the production of pressurized nitrogen and oxygen to operate the medium pressure stage under an increased pressure, approximately 2.0 to 8.0 bar, than to subsequently compress products obtained without pressure.
  • the object on which the invention is based is to improve the method and the device of the type mentioned at the outset in such a way that both the production of pressurized nitrogen and pressurized oxygen and the production of argon can be carried out economically.
  • This object is achieved in that the crude argon rectification is operated under a pressure which is lower than the pressure of the medium pressure stage.
  • the pressure conditions in the crude argon rectification are no longer tied to those of the medium pressure stage, so that an optimal value for the argon yield of 1.1 to 2.0 bar, preferably 1.3 to 1.5 bar can be maintained. Nevertheless, the medium pressure stage can still release oxygen and nitrogen under increased pressure.
  • the argon-containing oxygen stream is expanded while performing work before being introduced into the crude argon rectification.
  • the energy recovered during expansion can be used to compress other process streams.
  • a lot of cold is generated during relaxation work, which is required for air separation. In this way, the supply of externally generated cold can be dispensed with at least in part.
  • the generally liquid residual fraction of crude argon rectification consists essentially of oxygen. Since it would be uneconomical to discard this fraction, it is proposed according to a further feature of the invention to return the liquid fraction from the crude argon rectification to the medium pressure stage and to pump it to the pressure of the medium pressure stage before introduction into the medium pressure stage.
  • the resulting vaporized oxygen-rich fraction is advantageously returned to the medium pressure stage.
  • the vaporized oxygen-rich fraction must be compressed in the medium pressure stage before being introduced.
  • the work obtained in the work-relieving expansion of the argon-containing oxygen stream is used at least in part to compress the vaporized oxygen-rich fraction.
  • the invention further relates to a device for carrying out the method according to claims 10 to 12.
  • Compressed and pre-cleaned air is supplied via line 1, cooled in a heat exchanger 36 in indirect heat exchange with product streams and fed into the 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 32 and in part throttled via line 10 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 32 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.
  • liquid oxygen (line 14), gaseous pure nitrogen (line 15) and impure nitrogen (line 16) are removed and the nitrogen streams in the heat exchanger 32 are additionally heated.
  • an argon-containing oxygen stream is also removed from line 17 via line 17, heated in heat exchanger 36 and introduced into crude argon rectification 20, which is under a pressure of 1.1 bar to 2.0 bar, preferably 1.3 to 1.5 bar is operated.
  • the residual fraction obtained in the bottom of the crude argon rectification 20 is discharged via line 22 and brought according to the invention by pump 23 to the pressure required for feeding back into the medium pressure stage 4.
  • the argon-rich oxygen stream 17 is expanded prior to introduction into the crude argon rectification 20 in an expansion turbine 18 in order to bring it to the lower pressure prevailing in the crude argon rectification 20 on the one hand and to produce process cold on the other.
  • the gaseous crude argon obtained at the top of the crude argon rectification 20 is introduced via line 33 into a condenser 35, partly liquefied and partly returned via line 34 as a return to the crude argon rectification 20, partly discharged via line 21 as an intermediate product and heated in the heat exchanger 36 .
  • the condenser 35 is cooled by a portion of the oxygen-rich fraction 6 from the pressure stage, which is brought in via line 11, subcooled in a heat exchanger 24 and passed to the condenser 35 via line 25.
  • the portion evaporated during the indirect heat exchange with the top gas of the crude argon rectification 20 is discharged via line 26 and heated in the heat exchangers 24 and 36.
  • the oxygen-rich stream is compressed in two compressor stages 27 and 29 and then each cooled (water coolers 28 and 30).
  • the oxygen-rich stream is then passed via line 31 through the heat exchanger 36, cooled there again and then fed into the medium pressure stage 4. It is advantageous to use the work obtained in the expansion of the argon-rich oxygen fraction 17 to drive the compression 29.
  • part of the air in line 1 can be condensed in heat exchange with oxygen from the sump of medium pressure stage 4.
  • the liquid from the sump of the medium pressure stage can be brought to high pressure by means of a pump and partially evaporates during the heat exchange.
  • the partially condensed air is then introduced into the pressure stage 3 above the first feed point (line 1) shown in the drawing. This part of the process is not shown in the drawing, but can be economically advantageous at the indicated rectification pressures.

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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 process and apparatus for air rectification with subsequent recovery of crude argon are described. The crude argon rectification (20) is operated at a lower pressure than the medium-pressure stage (4) of the two-stage air rectification (2). <IMAGE>

Description

Gegenstand der Erfindung sind 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 und bei dem der Mitteldruckstufe ein argonhaltiger Sauerstoffstrom entnommen und einer Rohargonrektifikation zugeleitet wird, und ferner eine Vorrichtung zur Durchführung des Verfahrens.The invention relates to a process for air separation by rectification, in which air is compressed, pre-cleaned, cooled and pre-separated into a nitrogen-rich fraction and an oxygen-rich liquid in the pressure stage of a two-stage rectification, 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 and in which an argon-containing oxygen stream is taken from the medium pressure stage and fed to crude argon rectification, and also a device for carrying out the method.

Ein derartiges Verfahren, bei dem im Anschluß an eine Luftzerle­gung Rohargon gewonnen wird, ist aus der DE-OS 34 36 897 be­kannt.Such a method, in which crude argon is obtained after air separation, is known from DE-OS 34 36 897.

Wie bei den bislang angewandten Verfahren üblich, wird bei dem vorveröffentlichten Verfahren die Rohargonrektifikation unter demjenigen Druck durchgeführt, unter dem die argonhaltige Sauer­stofffraktion aus der Mitteldruckstufe entnommen wird. Flüssiger Sauerstoff wird aus der Rohargonrektifikation an ungefähr die gleiche Stelle der Mitteldruckstufe zurückgeführt.As is customary in the previously used processes, in the previously published process the crude argon rectification is carried out under the pressure under which the argon-containing oxygen fraction is removed from the medium pressure stage. Liquid oxygen is recycled from crude argon rectification to approximately the same point in the medium pressure stage.

Solch ein Verfahren ist günstig, falls die Mitteldruckstufe und damit auch die Rohargonrektifikation im wesentlichen unter Atmosphärendruck durchgeführt. In vielen Fällen werden jedoch Sauerstoff und/oder Stickstoff, die in der Mitteldruckstufe erzeugt werden, unter erhöhtem Druck benötigt, beispielsweise in Kohlevergasungsanlagen oder zur Einblasung von Stickstoff bei der Erdöl- oder Erdgasgewinnung. Dabei ist es für die Druck­stickstoff- und -sauerstoffgewinnung wirtschaftlich vorteilhaf­ter, die Mitteldruckstufe unter einem erhöhten Druck, etwa 2,0 bis 8,0 bar, zu betreiben, als drucklos gewonnene Produkte anschließend zu verdichten.Such a method is favorable if the medium pressure stage and thus the crude argon rectification are carried out essentially under atmospheric pressure. In many cases, however, oxygen and / or nitrogen, which are generated in the medium pressure stage, are required under increased pressure, for example in coal gasification plants or for blowing nitrogen in during the extraction of oil or natural gas. It is economically more advantageous for the production of pressurized nitrogen and oxygen to operate the medium pressure stage under an increased pressure, approximately 2.0 to 8.0 bar, than to subsequently compress products obtained without pressure.

Da jedoch bei den bekannten Verfahren auch die Rohargonrektifi­kation unter dem erhöhten Druck betrieben werden muß, ergeben sich auch Nachteile, da unter dieser Voraussetzung nur eine relativ geringe Argonausbeute zu erreichen ist.However, since in the known methods the crude argon rectification must also be carried out under the increased pressure, there are also disadvantages, since under this condition only a relatively low argon yield can be achieved.

Die Aufgabe, welche der Erfindung zugrunde liegt, besteht darin, das Verfahren und die Vorrichtung der eingangs genannten Art dahingehend zu verbessern, daß sowohl die Druckstickstoff- und Drucksauerstofferzeugung, als auch die Argongewinnung wirt­schaftlich günstig durchgeführt werden können.The object on which the invention is based is to improve the method and the device of the type mentioned at the outset in such a way that both the production of pressurized nitrogen and pressurized oxygen and the production of argon can be carried out economically.

Diese Aufgabe wird dadurch gelöst, daß die Rohargonrektifikation unter einem Druck betrieben wird, der niedriger als der Druck der Mitteldruckstufe ist.This object is achieved in that the crude argon rectification is operated under a pressure which is lower than the pressure of the medium pressure stage.

Damit sind die Druckverhältnisse bei der Rohargonrektifikation nicht mehr an diejenigen der Mitteldruckstufe gebunden, so daß ein für die Argonausbeute optimaler Wert von 1,1 bis 2,0 bar, vorzugsweise 1,3 bis 1,5 bar eingehalten werden kann. Trotzdem kann die Mitteldruckstufe weiterhin Sauerstoff und Stickstoff unter erhöhtem Druck abgeben.Thus, the pressure conditions in the crude argon rectification are no longer tied to those of the medium pressure stage, so that an optimal value for the argon yield of 1.1 to 2.0 bar, preferably 1.3 to 1.5 bar can be maintained. Nevertheless, the medium pressure stage can still release oxygen and nitrogen under increased pressure.

Beim erfindungsgemäßen Verfahren erweist es sich als vorteil­haft, wenn der argonhaltige Sauerstoffstrom vor der Einleitung in die Rohargonrektifikation arbeitsleistend entspannt wird. Die bei der Entspannung zurückgewonnene Energie kann zur Verdichtung anderer Prozeßströme eingesetzt werden. Außerdem wird bei der arbeitsleistenden Entspannung besonders viel Kälte erzeugt, die bei der Luftzerlegung benötigt wird. Auf diese Weise kann mindestens teilweise auf die Zufuhr von extern erzeugter Kälte verzichtet werden.In the method according to the invention, it proves to be advantageous if the argon-containing oxygen stream is expanded while performing work before being introduced into the crude argon rectification. The energy recovered during expansion can be used to compress other process streams. In addition, a lot of cold is generated during relaxation work, which is required for air separation. In this way, the supply of externally generated cold can be dispensed with at least in part.

Dabei ist es günstig, den argonhaltigen Sauerstoffstrom vor der arbeitsleistenden Entspannung zu erwärmen. Dies kann im Wärme­austausch mit anderen Verfahrensströmen, vorzugsweise mit zu zerlegender Luft erfolgen.It is advantageous to heat the argon-containing oxygen stream before the work-related relaxation. This can take place in the heat exchange with other process streams, preferably with air to be separated.

Die im allgemeinen flüssig anfallende Restfraktion der Rohargon­rektifikation besteht im wesentlichen aus Sauerstoff. Da es unwirtschaftlich wäre, diese Fraktion zu verwerfen, wird gemäß einem weiteren Merkmal der Erfindung vorgeschlagen, die flüssige Fraktion aus der Rohargonrektifikation zur Mitteldruckstufe zurückzuleiten und vor der Einführung in die Mitteldruckstufe auf den Druck der Mitteldruckstufe zu pumpen.The generally liquid residual fraction of crude argon rectification consists essentially of oxygen. Since it would be uneconomical to discard this fraction, it is proposed according to a further feature of the invention to return the liquid fraction from the crude argon rectification to the medium pressure stage and to pump it to the pressure of the medium pressure stage before introduction into the medium pressure stage.

Es erweist sich als vorteilhaft, wenn eine gasförmige Fraktion vom Kopf der Rohargonrektifikation in indirektem Wärmetausch mit verdampfender sauerstoffreicher Flüssigkeit aus der Druckstufe kondensiert wird. Auf diese Weise kann im Verfahren vorhandene Kälte zur Bildung von Rücklauf für die Rohargonrektifikation ausgenützt und auf den Einsatz externer Kälte in diesem Bereich verzichtet werden.It proves to be advantageous if a gaseous fraction is condensed from the top of the crude argon rectification in indirect heat exchange with evaporating oxygen-rich liquid from the pressure stage. In this way, the cold that is present in the process can be used to form reflux for crude argon rectification and the use of external cold in this area can be dispensed with.

Die dabei entstehende verdampfte sauerstoffreiche Fraktion wird günstigerweise zur Mitteldruckstufe zurückgeführt.The resulting vaporized oxygen-rich fraction is advantageously returned to the medium pressure stage.

Die verdampfte sauerstoffreiche Fraktion muß vor der Einführung in der Mitteldruckstufe verdichtet werden. Zu diesem Zweck wird gemäß einer weiteren Ausgestaltung des erfindungsgemäßen Verfah­rens die bei der arbeitsleistenden Entspannung des argonhaltigen Sauerstoffstroms gewonnene Arbeit wenigstens teilweise zur Verdichtung der verdampften sauerstoffreichen Fraktion einge­setzt.The vaporized oxygen-rich fraction must be compressed in the medium pressure stage before being introduced. For this purpose, according to a further embodiment of the method according to the invention, the work obtained in the work-relieving expansion of the argon-containing oxygen stream is used at least in part to compress the vaporized oxygen-rich fraction.

Hierzu ist es vorteilhaft, die verdampfte sauerstoffreiche Fraktion nach der Verdichtung abzukühlen.For this purpose, it is advantageous to cool the evaporated oxygen-rich fraction after the compression.

Die Erfindung betrifft ferner eine Vorrichtung zur Durchführung des Verfahrens gemäß den Patentansprüchen 10 bis 12.The invention further relates to a device for carrying out the method according to claims 10 to 12.

Anhand der Zeichnung, in welcher eine Auführungsform 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 Wärmetauscher 36 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 32 unterkühlt und zu einem Teil über Leitung 10 in die Mitteldruckstufe 4 eingedrosselt. Stickstoff vom Kopf der Druckstufe 3 wird über Leitung 5 ebenfalls flüssig abgezogen, in Wärmetauscher 32 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.Compressed and pre-cleaned air is supplied via line 1, cooled in a heat exchanger 36 in indirect heat exchange with product streams and fed into the 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 32 and in part throttled via line 10 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 32 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.

Als Produkte der Mitteldruckstufe 4 werden flüssiger Sauerstoff (Leitung 14), gasförmiger Reinstickstoff (Leitung 15) und unreiner Stickstoff (Leitung 16) entnommen und im Wärmetauscher 36, die Stickstoffströme zusätzlich im Wärmetauscher 32, 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 in the heat exchanger 32 are additionally heated.

Über die bisher genannten Strome hinaus wird der Mitteldruck­stufe 4 außerdem ein argonhaltiger Sauerstoffstrom über Leitung 17 entnommen, im Wärmetauscher 36 angewärmt und in eine Rohar­gonrektifikation 20 eingeleitet, die unter einem Druck von 1,1 bar bis 2,0 bar, vorzugsweise 1,3 bis 1,5 bar betrieben wird. Die im Sumpf der Rohargonrektifikation 20 anfallende Restfraktion wird über Leitung 22 abgeführt und erfindungsgemäß durch Pumpe 23 auf den für die Zurückspeisung in die Mittel­druckstufe 4 erforderlichen Druck gebracht. Außerdem wird der argonreiche Sauerstoffstrom 17 vor der Einleitung in die Rohar­gonrektifikation 20 in einer Entspannungsturbine 18 arbeitslei­stend entspannt, um ihn einerseits auf den in der Rohargonrekti­fikation 20 herrschenden niedrigeren Druck zu bringen und andererseits Verfahrenskälte zu erzeugen.In addition to the currents mentioned so far, an argon-containing oxygen stream is also removed from line 17 via line 17, heated in heat exchanger 36 and introduced into crude argon rectification 20, which is under a pressure of 1.1 bar to 2.0 bar, preferably 1.3 to 1.5 bar is operated. The residual fraction obtained in the bottom of the crude argon rectification 20 is discharged via line 22 and brought according to the invention by pump 23 to the pressure required for feeding back into the medium pressure stage 4. In addition, the argon-rich oxygen stream 17 is expanded prior to introduction into the crude argon rectification 20 in an expansion turbine 18 in order to bring it to the lower pressure prevailing in the crude argon rectification 20 on the one hand and to produce process cold on the other.

Das am Kopf der Rohargonrektifikation 20 anfallende gasförmige Rohargon wird über Leitung 33 in einen Kondensator 35 einge­führt, teilweise verflüssigt und zum einen Teil über Leitung 34 als Rücklauf in die Rohargonrektifikation 20 zurückgeführt, zum anderen Teil über Leitung 21 als Zwischenprodukt abgeführt und im Wärmetauscher 36 angewärmt.The gaseous crude argon obtained at the top of the crude argon rectification 20 is introduced via line 33 into a condenser 35, partly liquefied and partly returned via line 34 as a return to the crude argon rectification 20, partly discharged via line 21 as an intermediate product and heated in the heat exchanger 36 .

Der Kondensator 35 wird durch einen Teil der sauerstoffreichen Fraktion 6 aus der Druckstufe gekühlt, der über Leitung 11 herangeführt, in einem Wärmetauscher 24 unterkühlt und über Leitung 25 zum Kondensator 35 geleitet wird. Der beim indirekten Wärmeaustausch mit dem Kopfgas der Rohargonrektifikation 20 verdampfte Anteil wird über Leitung 26 abgeführt und in den Wärmetauschern 24 und 36 erwärmt.The condenser 35 is cooled by a portion of the oxygen-rich fraction 6 from the pressure stage, which is brought in via line 11, subcooled in a heat exchanger 24 and passed to the condenser 35 via line 25. The portion evaporated during the indirect heat exchange with the top gas of the crude argon rectification 20 is discharged via line 26 and heated in the heat exchangers 24 and 36.

Da es wirtschaftlich ungünstig wäre, den in diesem Strom enthal­tenen Sauerstoff zu verwerfen, wird er im Verfahren des Ausfüh­rungsbeispiels zur Mitteldruckstufe 4 zurückgeführt. Um den dafür notwendigen Druck zu erreichen, wird der sauerstoffreiche Strom in zwei Verdichterstufen 27 und 29 komprimiert und jeweils anschließend abgekühlt (Wasserkühler 28 und 30). Anschließend wird der sauerstoffreiche Strom über Leitung 31 durch den Wärmetauscher 36 geführt, dort wieder abgekühlt und anschließend in die Mitteldruckstufe 4 eingespeist. Dabei ist es günstig, die bei der Entspannung der argonreichen Sauerstofffraktion 17 gewonnene Arbeit zum Antrieb des Verdichtes 29 zu verwenden.Since it would be economically unfavorable to discard the oxygen contained in this stream, it is returned to the medium pressure stage 4 in the process of the exemplary embodiment. In order to achieve the pressure required for this, the oxygen-rich stream is compressed in two compressor stages 27 and 29 and then each cooled (water coolers 28 and 30). The oxygen-rich stream is then passed via line 31 through the heat exchanger 36, cooled there again and then fed into the medium pressure stage 4. It is advantageous to use the work obtained in the expansion of the argon-rich oxygen fraction 17 to drive the compression 29.

Vor der Einspeisung in die Druckstufe 3 kann ein Teil der Luft in Leitung 1 in Wärmetausch mit Sauerstoff aus dem Sumpf der Mitteldruckstufe 4 kondensiert werden. Die Flüssigkeit aus dem Sumpf der Mitteldruckstufe kann dazu mittels einer Pumpe auf hohen Druck gebracht werden und verdampft bei dem Wärmeaustausch teilweise. Die partiell kondensierte Luft wird dann oberhalb der in der Zeichnung gezeigten ersten Einspeisestelle (Leitung 1) in die Druckstufe 3 eingeführt. Dieser Verfahrensteil ist in der Zeichnung nicht dargestellt, kann aber bei den angegebenen Rektifizierdrücken wirtschaftlich günstig sein.Before feeding into pressure stage 3, part of the air in line 1 can be condensed in heat exchange with oxygen from the sump of medium pressure stage 4. The liquid from the sump of the medium pressure stage can be brought to high pressure by means of a pump and partially evaporates during the heat exchange. The partially condensed air is then introduced into the pressure stage 3 above the first feed point (line 1) shown in the drawing. This part of the process is not shown in the drawing, but can be economically advantageous at the indicated rectification pressures.

Für eine wirtschaftliche Argonausbeute ist es notwendig, den Produktsauerstoff (Leitung 14) mit einer Reinheit von mindestens 99,5 % herzustellen, um in dem argonreichen Sauerstoffstrom (Leitung 17) genügend Argon anzureichern. Bei 5 bar Druck in der Mitteldruckstufe 4 ist dazu bei einem konventionellen Verfahren ein Luftfaktor von 5,86 notwendig. Bei dem erfindungsgemäßen Verfahren reduziert sich der Luftfaktor auf 5,45. Damit wird eine Energieeinsparung von 7,0 erzielt.For an economical argon yield, it is necessary to produce the product oxygen (line 14) with a purity of at least 99.5% in order to accumulate sufficient argon in the argon-rich oxygen stream (line 17). At 5 bar pressure in medium pressure level 4, an air factor of 5.86 is necessary for this in a conventional process. In the method according to the invention, the air factor is reduced to 5.45. This results in an energy saving of 7.0.

Claims (13)

1. Verfahren zur Luftzerlegung durch Rektifikation, bei dem Luft (1) verdichtet, vorgereinigt, abgekühlt (36) und in der Druckstufe (3) einer zweistufigen Rektifikation (2) in eine stickstoffreiche Fraktion (5) und in eine sauerstoffreiche Flüssigkeit (6) vorzerlegt wird und die beiden Fraktionen (5, 6) mindestens teilweise der Mitteldruckstufe (4) der Rektifikation (2) zugeführt und in Sauerstoff und Stickstoff zerlegt werden und bei dem der Mitteldruckstufe (4) ein argonhaltiger Sauerstoffstrom (17) entnommen und einer Roh­argonrektifikation (20) zugeleitet wird, dadurch gekenn­zeichnet, daß die Rohargonrektifikation (20) unter einem Druck betrieben wird, der niedriger als der Druck der Mitteldruckstufe (4) ist.1. A process for air separation by rectification, in which air (1) is compressed, pre-cleaned, cooled (36) and in the pressure stage (3) a two-stage rectification (2) into a nitrogen-rich fraction (5) and an oxygen-rich liquid (6) is preassembled and the two fractions (5, 6) are at least partially fed to the medium pressure stage (4) of the rectification (2) and decomposed into oxygen and nitrogen and from which an argon-containing oxygen stream (17) is removed from the medium pressure stage (4) and a crude argon rectification ( 20) is fed in, characterized in that the crude argon rectification (20) is operated under a pressure which is lower than the pressure of the medium pressure stage (4). 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der argonhaltige Sauerstoffstrom (17) vor der Einleitung in die Rohargonrektifikation (20) arbeitsleistend entspannt wird (18).2. The method according to claim 1, characterized in that the argon-containing oxygen stream (17) before the introduction into the crude argon rectification (20) is relaxed while working (18). 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß der argonhaltige Sauerstoffstrom (17) vor der arbeitsleistenden Entspannung (18) erwärmt wird.3. The method according to claim 2, characterized in that the argon-containing oxygen stream (17) is heated before the work-relieving relaxation (18). 4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekenn­zeichnet, daß eine flüssige Fraktion (22) aus der Rohargon­rektifikation (20) zur Mitteldruckstufe (4) zurückgeleitet und vor der Einführung in die Mitteldruckstufe (4) auf den Druck der Mitteldruckstufe (4) gepumpt wird (23).4. The method according to any one of claims 1 to 3, characterized in that a liquid fraction (22) from the crude argon rectification (20) is returned to the medium pressure stage (4) and is pumped (23) to the pressure of the medium pressure stage (4) before being introduced into the medium pressure stage (4). 5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekenn­zeichnet, daß eine gasförmige Fraktion (33) vom Kopf der Rohargonrektifikation (20) in indirektem Wärmetausch (35) mit verdampfender sauerstoffreicher Flüssigkeit (25) aus der Druckstufe (3) kondensiert wird.5. The method according to any one of claims 1 to 4, characterized in that a gaseous fraction (33) from the top of the crude argon rectification (20) in indirect heat exchange (35) with evaporating oxygen-rich liquid (25) from the pressure stage (3) is condensed. 6. Verfahren nach Anspruch 5, dadurch gekennzeichnet, daß die verdampfte sauerstoffreiche Fraktion (26) zur Mitteldruck­stufe (4) zurückgeführt wird.6. The method according to claim 5, characterized in that the evaporated oxygen-rich fraction (26) is returned to the medium pressure stage (4). 7. Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die verdampfte sauerstoffreiche Fraktion (26) vor der Einführung in der Mitteldruckstufe (4) verdichtet (27, 29) wird.7. The method according to claim 6, characterized in that the vaporized oxygen-rich fraction (26) is compressed (27, 29) before introduction into the medium pressure stage (4). 8. Verfahren nach Anspruch 2 und 7, dadurch gekennzeichnet, daß die bei der arbeitsleistenden Entspannung (18) des argonhal­tigen Sauerstoffstroms (17) gewonnene Arbeit wenigstens teilweise zur Verdichtung (29) der verdampften sauerstoff­reichen Fraktion (26) eingesetzt wird.8. The method according to claim 2 and 7, characterized in that the work obtained in the relaxation work (18) of the argon-containing oxygen stream (17) work at least partially for the compression (29) of the vaporized oxygen-rich fraction (26) is used. 9. Verfahren nach Anspruch 7 oder 8, dadurch gekennzeichnet, daß die verdampfte sauerstoffreiche Fraktion (31) nach der Verdichtung (27, 29) abgekühlt (36) wird.9. The method according to claim 7 or 8, characterized in that the evaporated oxygen-rich fraction (31) after the compression (27, 29) is cooled (36). 10. Vorrichtung zur Durchführung des Verfahrens nach einem der Ansprüche 1 bis 9 mit einer Doppelrektifiziersäule (2) bestehend aus Drucksäule (3) und Mitteldrucksäule (4) und mit einer Rohargonrektifiziersäule (20) und einer ersten (17, 19) und einer zweiten (22) Verbindungsleitung zwischen Mitteldrucksäule (4) und Rohargonrektifiziersäule (20), dadurch gekennzeichnet, daß in der ersten Verbindungsleitung (17, 19) eine Entspannungseinrichtung (18) eingebaut ist.10. Apparatus for carrying out the method according to one of claims 1 to 9 with a double rectification column (2) consisting of a pressure column (3) and a medium pressure column (4) and with a crude argon rectification column (20) and a first (17, 19) and a second ( 22) connecting line between the medium pressure column (4) and crude argon rectifying column (20), characterized in that a relaxation device (18) is installed in the first connecting line (17, 19). 11. Vorrichtung nach Anspruch 10, gekennzeichnet, daß in der zweiten Verbindungsleitung (22) eine Pumpe (23) eingebaut ist.11. The device according to claim 10, characterized in that a pump (23) is installed in the second connecting line (22). 12. Vorrichtung nach Anspruch 10 oder 11, gekennzeichnet durch einen Wärmetauscher (35), der über eine erste Gasleitung (33) und über eine erste Flüssigkeitsleitung (34) mit der Rohargonrektifiziersäule (20) und über eine zweite Flüssig­keitsleitung (25) mit der Drucksäule (3) verbunden ist, durch eine zweite Gasleitung (26, 31), welche den Wärmetau­scher (35) mit der Mitteldrucksäule (4) verbindet, und durch einen Verdichter (27, 29) in der zweiten Gasleitung (26, 31).12. The apparatus of claim 10 or 11, characterized by a heat exchanger (35) via a first gas line (33) and a first liquid line (34) with the crude argon rectification column (20) and via a second liquid line (25) with the pressure column (3) is connected by a second gas line (26, 31) which connects the heat exchanger (35) to the medium pressure column (4) and by a compressor (27, 29) in the second gas line (26, 31). 13. Vorrichtung nach Anspruche 12, dadurch gekennzeichnet, daß eine Expansionsturbine als Entspannungseinrichtung (18) verwendet wird und diese mechanisch an den Verdichter (29) in der zweiten Gasleitung gekoppelt ist.13. The apparatus according to claim 12, characterized in that an expansion turbine is used as the expansion device (18) and this is mechanically coupled to the compressor (29) in the second gas line.
EP90102355A 1989-02-23 1990-02-07 Air rectification process and apparatus Expired - Lifetime EP0384213B1 (en)

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EP0384213B1 (en) 1992-12-02
JPH02247485A (en) 1990-10-03

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