EP1052465A1 - Process and device for cryogenic air separation - Google Patents

Process and device for cryogenic air separation Download PDF

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Publication number
EP1052465A1
EP1052465A1 EP99112289A EP99112289A EP1052465A1 EP 1052465 A1 EP1052465 A1 EP 1052465A1 EP 99112289 A EP99112289 A EP 99112289A EP 99112289 A EP99112289 A EP 99112289A EP 1052465 A1 EP1052465 A1 EP 1052465A1
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Prior art keywords
liquid
level
fraction
transfer fraction
column
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EP99112289A
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German (de)
French (fr)
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EP1052465B1 (en
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Thomas Dipl.-Ing. Nohlen
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Linde GmbH
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Linde GmbH
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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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • 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
    • F25J3/04666—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
    • F25J3/04642—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
    • F25J3/04703—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 being arranged in more than one vessel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
    • 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
    • F25J2235/06—Lifting of liquids by gas lift, e.g. "Mammutpumpe"
    • 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
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being 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

Definitions

  • the invention relates to a method for the low-temperature separation of air according to the Preamble of claim 1.
  • the invention particularly relates to two- or multi-column systems a pressure column and with a low pressure column arranged above the pressure column and / or an arranged or around a multi-column system with further separation columns for nitrogen-oxygen separation.
  • the pressure column represents the "first Rectification column "in the sense of the invention; rectification in the low pressure column and / or the evaporation in the top condenser of the crude argon column is the "further one Process step ".
  • The” transfer fraction is here by the bottom liquid or an intermediate liquid of the pressure column formed in the low pressure column or in the evaporation space of the top condenser of the crude argon column is introduced.
  • the invention relates in particular to double-column processes as shown in Figs. 4.21, 4.23, 4.26, 4.28 and 4.34 in Chapter 4.5 by Hausen / Linde.
  • the invention Mass transfer preferably in at least one separation column (e.g. low pressure and / or crude argon column) at least partially by packing or ordered Pack causes.
  • the transfer fraction collects in one within the first rectification column Reservoir through the sump of this column or a cup inside the column is formed.
  • the liquid level in this reservoir sets the "first level” h1 firmly in the sense of the invention.
  • the transfer fraction in passed a container in which a further process step is carried out, for example the low pressure column or the evaporation space of a condenser-evaporator (e.g. top condenser of the raw argon column).
  • a further process step for example the low pressure column or the evaporation space of a condenser-evaporator (e.g. top condenser of the raw argon column).
  • the place of feeding too this further process step defines the "second, higher level" in the sense of Invention.
  • Air separation plants in which packings in the low pressure part of a double column are used, for example, in EP 321163 A, WO 9319335, WO 9319336 or EP 628777 A.
  • a disadvantage of using packs is that the overall height noticeably increased compared to the bottom columns.
  • the claim cited inequality apply, that is, the pressure difference between pressure and Low pressure column or between the pressure column and the evaporation chamber of the Top condenser of the crude argon column is no longer sufficient to match the corresponding one to overcome hydrostatic pressure of a liquid column of the conduction fraction. While this situation also applies to normal operation under full load in some systems can occur, it often appears especially in special operating cases, especially when operating under underload, i.e. with a lower product and Amount used than in full load operation.
  • the invention has for its object the aforementioned method and appropriate device to further improve.
  • the expansion valve is at a suitable intermediate level between the first and the second level.
  • the specific definition of this intermediate level is different for each special embodiment of the invention, but can be easily determined with the aid of the calculation tools that are available to the person skilled in the art if the height of the intermediate level is specified as a degree of freedom.
  • the transfer fraction is subcooled before relaxing by indirect heat exchange. This will the formation of a two-phase mixture upstream of the relaxation entirely or partially avoided, so that the invention only when relaxing targeted vapor bubble formation occurs.
  • the hypothermia usually takes place nearby of the first level.
  • the transfer fraction is immediate upstream of relaxing completely or substantially completely in is in liquid form, but is no longer hypothermic.
  • the degree of supercooling of the conduction fraction becomes usually determined regardless of the liquid transport process and is of other criteria determines, for example the effort, relatively little flash gas to generate when feeding into the second container.
  • the relaxation process in particular the arrangement of the expansion valve, then becomes determines that the transition fraction immediately at the specified supercooling before relaxing just in the single-phase liquid state and neither a noticeable hypothermia still steam bubbles to a significant extent available.
  • the invention also relates to a device for the low-temperature separation of air according to claims 4 to 6.
  • cleaned air 1 is under a Pressure from 4 to 20 bar, preferably 5 to 12 bar in a heat exchanger 2 against Product flows cooled to about dew point and into the pressure column 3 a two-stage Rectifier fed.
  • the pressure column 3 stands over a common one Condenser-evaporator 4 in heat exchange relationship with a low pressure column 5.
  • the method of transferring a liquid according to the invention can also be applied the liquid nitrogen 7 from the top of the pressure column as a (further) "transfer fraction" be applied.
  • the "first level” is due to the liquid level formed inside the cup 16 in which the coming from the main capacitor 4 Liquid is collected.
  • the countercurrent 8 is supercooled supercooled nitrogen 17 flows to an expansion valve 18 which is on a Intermediate level hz 'is arranged and finally further to the feed point 19th ("second level" h2 ') at the head of the low pressure column.
  • the Invention also for the transport of a liquid transfer fraction in the Evaporation space of the top condenser of a crude argon column can be used.
  • the crude argon column is formed in the example by two sections 20a, 20b, their function in European patent EP 628777 B1 and in the corresponding U.S. Patent US 5,426,946 is described in detail.
  • the invention can be used by anyone known type of raw argon extraction are used, in which an argon-containing Oxygen fraction 21 introduced from the low pressure column 5 into a crude argon column is, with an oxygen-depleted in the upper area of the crude argon column Argon product 22a, 22b is obtained in the gaseous and / or liquid state.
  • the further transition fraction is in the example shown in the drawing through part 13a of the supercooled sump liquid 6 from the pressure column 5 educated. It is relaxed in an expansion valve 14a, which is on a Intermediate level is arranged. This intermediate level is in the example the same or approximately the same height as the intermediate level hz.
  • the in 14a relaxed transfer fraction 15a of sump 12 of the pressure column 3 is on a "second level" h2 "in the evaporation chamber 23 of the top condenser Raw argon column introduced.

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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

To maintain very low air temps., the intake air (1) is passed to an initial rectifying column (3). An overflow fraction (6,7 a given density (p) is taken in a liquid condition from a reservoir (24,16) within the first column (3), is relaxed (14,14a,18), transferred to a further process stage (5,23). The liquid level in the reservoir (24,16) is at a first level (h1) and an initial pressure (p1). The relaxed fraction is brought to a second and higher level (h2(h2 ≥ h1)) at the next stage (5,23) and is hel a second and lower pressure (p2 ≤ p1). The pressure difference DELTA p=p1 x p2 is lower than the hydrostatic pressure (phydr=p x g(h2+h1)) between the two levels, where g is the acceleration of the earth rotation. The relaxation is structured so that the developed gas bubbles reduce the density to give the pressure difference DELTA p to allow the fraction to pass to t next stage (5,23).

Description

Die Erfindung betrifft ein Verfahren zur Tieftemperaturzerlegung von Luft gemäß dem Oberbegriff von Patentanspruch 1.The invention relates to a method for the low-temperature separation of air according to the Preamble of claim 1.

Einschlägige Luftzerlegungsverfahren und -vorrichtungen sind zum Beispiel in Hausen/Linde, Tieftemperaturtechnik, 2. Auflage 1985, Kapitel 4 (Seiten 281 bis 337) beschreiben. Die Erfindung betrifft insbesondere Zwei- oder Mehrsäulensysteme mit einer Drucksäule und mit einer über der Drucksäule angeordneten Niederdrucksäule und/oder einer angeordneten oder um ein Mehrsäulensystem mit weiteren Trennsäulen zur Stickstoff-Sauerstoff-Trennung. Die Drucksäule stellt in diesem Fall die "erste Rektifiziersäule" im Sinne der Erfindung dar; die Rektifikation in der Niederdrucksäule und/oder die Verdampfung im Kopfkondensator der Rohargonsäule ist der "weitere Verfahrensschritt". Die "Überleitungsfraktion" wird hier durch die Sumpfflüssigkeit oder eine Zwischenflüssigkeit der Drucksäule gebildet, die in die Niederdrucksäule oder in den Verdampfungsraum des Kopfkondensators der Rohargonsäule eingeleitet wird.Relevant air separation processes and devices are, for example, in Hausen / Linde, low-temperature technology, 2nd edition 1985, chapter 4 (pages 281 to 337) describe. The invention particularly relates to two- or multi-column systems a pressure column and with a low pressure column arranged above the pressure column and / or an arranged or around a multi-column system with further separation columns for nitrogen-oxygen separation. In this case, the pressure column represents the "first Rectification column "in the sense of the invention; rectification in the low pressure column and / or the evaporation in the top condenser of the crude argon column is the "further one Process step ". The" transfer fraction "is here by the bottom liquid or an intermediate liquid of the pressure column formed in the low pressure column or in the evaporation space of the top condenser of the crude argon column is introduced.

Die Erfindung betrifft insbesondere Doppelsäulenverfahren, wie sie in den Bildern 4.21, 4.23, 4.26, 4.28 und 4.34 im Kapitel 4.5 von Hausen/Linde dargestellt sind. Abweichend von den Beispielen in Hausen/Linde wird bei der Erfindung der Stoffaustausch vorzugsweise in mindestens einer Trennsäule (z.B. Niederdruck und/oder Rohargonsäule) mindestens teilweise durch Füllkörper oder geordnete Packung bewirkt.The invention relates in particular to double-column processes as shown in Figs. 4.21, 4.23, 4.26, 4.28 and 4.34 in Chapter 4.5 by Hausen / Linde. Deviating from the examples in Hausen / Linde, the invention Mass transfer preferably in at least one separation column (e.g. low pressure and / or crude argon column) at least partially by packing or ordered Pack causes.

Die Überleitungsfraktion sammelt sich innerhalb der ersten Rektifiziersäule in einem Reservoir, das durch den Sumpf dieser Säule oder eine in der Säule befindliche Tasse gebildet wird. Der Flüssigkeitsspiegel in diesem Reservoir legt das "erste Niveau" h1 im Sinne der Erfindung fest. Aus diesem Reservoir wird die Überleitungsfraktion in einen Behälter geleitet, in dem ein weiterer Verfahrensschritt durchgeführt wird, beispielsweise die Niederdrucksäule oder der Verdampfungsraum eines Kondensator-Verdampfers (z.B. Kopfkondensator der Rohargonsäule). Die Stelle der Zuspeisung zu diesem weiteren Verfahrensschritt definiert das "zweite, höhere Niveau" im Sinne der Erfindung. The transfer fraction collects in one within the first rectification column Reservoir through the sump of this column or a cup inside the column is formed. The liquid level in this reservoir sets the "first level" h1 firmly in the sense of the invention. From this reservoir the transfer fraction in passed a container in which a further process step is carried out, for example the low pressure column or the evaporation space of a condenser-evaporator (e.g. top condenser of the raw argon column). The place of feeding too this further process step defines the "second, higher level" in the sense of Invention.

Seit einigen Jahre setzt sich der Einsatz von druckverlustarmen Einbauten in Luftzerlegersäulen immer mehr durch, da sie eine Reihe von Vorteilen aufweisen. Luftzerlegungsanlagen, bei denen Packungen im Niederdruckteil einer Doppelsäule eingesetzt werden, sind beispielsweise in EP 321163 A, WO 9319335, WO 9319336 oder EP 628777 A beschrieben.The use of low-pressure internals has been in use for several years Air separation columns more and more because they have a number of advantages. Air separation plants, in which packings in the low pressure part of a double column are used, for example, in EP 321163 A, WO 9319335, WO 9319336 or EP 628777 A.

Ein Nachteil der Verwendung von Packungen besteht darin, daß sich die Bauhöhe gegenüber Bodenkolonnen spürbar erhöht. In diesem Fall kann die im Patentanspruch angeführte Ungleichung gelten, das heißt, der Druckunterschied zwischen Druck- und Niederdrucksäule beziehungsweise zwischen Drucksäule und Verdampfungsraum des Kopfkondensators der Rohargonsäule reicht nicht mehr aus, um den entsprechenden hydrostatischen Druck einer Flüssigkeitssäule der Überleitungsfraktion zu überwinden. Während diese Situation bei einigen Anlagen auch im Normalbetrieb unter Vollast auftreten kann, erscheint es häufig insbesondere bei speziellen Betriebsfällen, insbesondere bei einem Betrieb unter Unterlast, also mit einer geringeren Produkt- und Einsatzmenge als beim Vollastbetrieb.A disadvantage of using packs is that the overall height noticeably increased compared to the bottom columns. In this case, the claim cited inequality apply, that is, the pressure difference between pressure and Low pressure column or between the pressure column and the evaporation chamber of the Top condenser of the crude argon column is no longer sufficient to match the corresponding one to overcome hydrostatic pressure of a liquid column of the conduction fraction. While this situation also applies to normal operation under full load in some systems can occur, it often appears especially in special operating cases, especially when operating under underload, i.e. with a lower product and Amount used than in full load operation.

Das Problem wurde bereits in EP 567360 A grundsätzlich erwähnt und durch die Einspeisung eines "Erleicherterungsgases" stromabwärts des Ventils gelöst.The problem has already been mentioned in principle in EP 567360 A and by Infeed of a "relief gas" released downstream of the valve.

Der Erfindung liegt die Aufgabe zugrunde, das vorgenannte Verfahren und die entsprechende Vorrichtung weiter zu verbessern.The invention has for its object the aforementioned method and appropriate device to further improve.

Diese Aufgabe wird durch das kennzeichnende Merkmal des Patentanspruchs 1 gelöst.This object is achieved by the characterizing feature of patent claim 1 solved.

Im Rahmen der Erfindung hat es sich herausgestellt, daß es möglich ist das "Erleichterungsgas" im Sinne der EP 567360 A unmittelbar aus der Überleitungsfraktion selbst zu gewinnen. Die Nachteile der in EP 567360 A beschriebenen Methode werden dabei vermieden, insbesondere sind bei der Überleitung von sauerstoffangereicherter Flüssigkeit aus der Drucksäule weder ein Verbrauch von Druckluft als "Erleichterungsgas" noch aufwendige zusätzliche Schritte zur Erzeugung von "Erleichterungsgas" aus der Überleitungsfraktion notwendig; auch eine zusätzliche Regelung entfällt. In the context of the invention it has been found that it is possible "Lightening gas" in the sense of EP 567360 A directly from the Win transition fraction itself. The disadvantages of EP 567360 A described method are avoided, especially in the Transfer of oxygen-enriched liquid from the pressure column neither Consumption of compressed air as a "lightening gas" still requires additional steps necessary to produce "relief gas" from the transfer fraction; also there is no additional regulation.

Hierfür bedarf es einer Anordnung des Entspannungsventils auf einem geeigneten Zwischenniveau zwischen dem ersten und dem zweiten Niveau. Die konkrete Festlegung dieses Zwischenniveaus ist für jede spezielle Ausführung der Erfindung verschieden, kann aber mit Hilfe der Berechnungswerkzeuge, die dem Fachmann zur Verfügung stehen, ohne weiteres ermittelt werden, wenn man die Höhe des Zwischenniveaus als Freiheitsgrad vorgibt. In typischen Fällen wird das Entspannungsventil auf einem Zwischenniveau von hz = h1 + x · (h2 - h1), wobei x 30 bis 80 %, vorzugsweise 40 bis 70 %, beträgt.This requires an arrangement of the expansion valve at a suitable intermediate level between the first and the second level. The specific definition of this intermediate level is different for each special embodiment of the invention, but can be easily determined with the aid of the calculation tools that are available to the person skilled in the art if the height of the intermediate level is specified as a degree of freedom. In typical cases, the relief valve is at an intermediate level of hz = h1 + x · (h2 - h1), where x is 30 to 80%, preferably 40 to 70%.

Diese Auslegung muß für einen bestimmten Betriebsfall vorgenommen werden, zum Beispiel für das Anfahren der Anlage. In einem anderen Beispiel wird die Anordnung des Entspannungsventils für den Unterlastfall im stationären Betrieb der Anlage ausgelegt; dann müssen unter Umständen zusätzliche Mittel zum Transport der Überleitungsflüssigkeit zum "weiteren Verfahrensschritt" während des Anfahrens der Anlage vorgesehen sein; dabei können übliche Methoden zum Transport von Flüssigkeit (mechanische Pumpe, Eindüsen von externem Gas usw.) eingesetzt werden, alternativ oder zusätzlich kann das Druckniveau in der ersten Rektifiziersäule beim Anfahren erhöhte werden.This interpretation must be made for a specific operating case, for Example of starting up the system. In another example, the arrangement of the relief valve for underload in stationary operation of the system designed; then additional funds may be required to transport the Transfer liquid to the "further process step" during startup of the Plant be provided; usual methods for the transport of Liquid (mechanical pump, injection of external gas, etc.) is used , alternatively or additionally, the pressure level in the first rectification column be increased when starting.

Bei dem erfindungsgemäßen Verfahren ist es günstig, wenn die Überleitungsfraktion vor dem Entspannen durch indirekten Wärmeaustausch unterkühlt wird. Dadurch wird die Bildung eines Zweiphasengemischs stromaufwärts des Entspannens ganz oder teilweise vermieden werden, so daß erst beim Entspannen die erfindungsgemäße gezielte Dampfblasenbildung erfolgt. Die Unterkühlung erfolgt in der Regel in der Nähe des ersten Niveaus.In the method according to the invention, it is advantageous if the transfer fraction is subcooled before relaxing by indirect heat exchange. This will the formation of a two-phase mixture upstream of the relaxation entirely or partially avoided, so that the invention only when relaxing targeted vapor bubble formation occurs. The hypothermia usually takes place nearby of the first level.

Vorzugsweise wird gerade so stark unterkühlt, daß die Überleitungsfraktion unmittelbar stromaufwärts des Entspannens vollständig oder im wesentlichen vollständig in flüssiger Form vorliegt, aber nicht mehr unterkühlt ist. It is preferably just so strongly supercooled that the transfer fraction is immediate upstream of relaxing completely or substantially completely in is in liquid form, but is no longer hypothermic.

Bei der Auslegung einer Anlage wird dies praktisch so durchgeführt, daß zunächst die Unterkühlung festgelegt wird. Das Maß der Unterkühlung der Überleitungsfraktion wird in der Regel unabhängig vom Flüssigkeitstransportvorgang bestimmt und ist von anderen Kriterien bestimmt, beispielsweise dem Bestreben, relativ wenig Flashgas beim Einspeisen in den zweiten Behälter zu erzeugen. Der Entspannungsvorgang, insbesondere die Anordnung des Entspannungsventils, wird anschließend so bestimmt, daß bei der vorgegebenen Unterkühlung die Überleitungsfraktion unmittelbar vor dem Entspannen gerade noch im einphasigen flüssigen Zustand vorliegt und weder eine nennenswerte Unterkühlung noch Dampfblasen in nennenswertem Umfang vorliegen.When designing a system, this is practically carried out so that the Hypothermia is set. The degree of supercooling of the conduction fraction becomes usually determined regardless of the liquid transport process and is of other criteria determines, for example the effort, relatively little flash gas to generate when feeding into the second container. The relaxation process, in particular the arrangement of the expansion valve, then becomes determines that the transition fraction immediately at the specified supercooling before relaxing just in the single-phase liquid state and neither a noticeable hypothermia still steam bubbles to a significant extent available.

Die Erfindung betrifft außerdem eine Vorrichtung zur Tieftemperaturzerlegung von Luft gemäß den Patentansprüchen 4 bis 6.The invention also relates to a device for the low-temperature separation of air according to claims 4 to 6.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im folgenden anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispiel näher erläutert. In dem Ausführungsbeispiel ist sowohl die Überleitung von Drucksäulen-Sumpfflüssigkeit und Drucksäulen-Stickstoff in die Niederdrucksäule als auch die Argongewinnung mit Überführung der Drucksäulen-Sumpfflüssigkeit in den Kopfkondensator einer Rohargonsäule gezeigt.The invention and further details of the invention are described below of an embodiment schematically illustrated in the drawing. In the exemplary embodiment, both the transfer of pressure column sump liquid and pressure column nitrogen into the low pressure column as well Argon extraction with transfer of the pressure column sump liquid into the Top condenser of a crude argon column shown.

Bei dem in dem Schema dargestellten Verfahren wird gereinigte Luft 1 unter einem Druck von 4 bis 20 bar, vorzugsweise 5 bis 12 bar in einem Wärmetauscher 2 gegen Produktströme auf etwa Taupunkt abgekühlt und in die Drucksäule 3 einer zweistufigen Rektifiziereinrichtung eingespeist. Die Drucksäule 3 steht über einen gemeinsamen Kondensator-Verdampfer 4 in Wärmeaustauschbeziehung mit einer Niederdrucksäule 5.In the method shown in the diagram, cleaned air 1 is under a Pressure from 4 to 20 bar, preferably 5 to 12 bar in a heat exchanger 2 against Product flows cooled to about dew point and into the pressure column 3 a two-stage Rectifier fed. The pressure column 3 stands over a common one Condenser-evaporator 4 in heat exchange relationship with a low pressure column 5.

Sumpfflüssigkeit 6 und Stickstoff 7 werden aus der Drucksäule 3 abgezogen, in einem Gegenströmer 8 unterkühlt und mindestens teilweise in die Niederdrucksäule 5 eingedrosselt. Aus der Niederdrucksäule werden Sauerstoff 9, Stickstoff 10 und unreiner Stickstoff 11 gasförmig entnommen. Die Produkte können auch mindestens teilweise flüssig entnommen werden (Sauerstoff 9a, Stickstoff 10a). Bottom liquid 6 and nitrogen 7 are withdrawn from the pressure column 3 in one Countercurrent 8 subcooled and at least partially into the low pressure column 5 throttled. Oxygen 9, nitrogen 10 and impure nitrogen 11 taken in gaseous form. The products can also at least partially removed in liquid form (oxygen 9a, nitrogen 10a).

In der Drucksäule bildet der Sumpf ein Reservoir 24 für die vom untersten Stoffaustauschabschnitt ablaufende Kolonnenflüssigkeit. Die Sumpfflüssigkeit, die sich in diesem Reservoir sammelt bildet die Überleitungsfraktion im Sinne der Erfindung. Das "erste Niveau" h1 ist durch den Flüssigkeitsspiegel im Sumpf der Drucksäule bestimmt. Die Überleitungsfraktion 6 wird in dem Gegenströmer 8 unterkühlt. Die unterkühlte Überleitungsfraktion strömt zu einem ersten Teil 13 einem Entspannungsventil 14 zu, das auf dem Niveau hz angeordnet ist. Beim Entspannen 14 wird soviel Dampf erzeugt, daß der verbleibende Druckunterschied ausreicht, um die Überleitungsfraktion als Zweiphasengemisch 15 in die Niederdrucksäule zu drücken, und zwar auf dem "zweiten Niveau" h2. In einem konkreten Zahlenbeispiel gilt:

  • h1 = 3100 mm
  • h2 = 22100 mm
  • hz = 46100 mm
    • In the pressure column, the sump forms a reservoir 24 for the column liquid draining from the lowest mass transfer section. The bottom liquid which collects in this reservoir forms the transfer fraction in the sense of the invention. The "first level" h1 is determined by the liquid level in the sump of the pressure column. The conduction fraction 6 is subcooled in the counterflow 8. The supercooled conduction fraction flows to a first part 13 of an expansion valve 14 which is arranged at the level hz. During the expansion 14 so much steam is generated that the remaining pressure difference is sufficient to press the transfer fraction as a two-phase mixture 15 into the low pressure column, namely at the "second level" h2. In a concrete numerical example:
  • h1 = 3100 mm
  • h2 = 22100 mm
  • hz = 46100 mm

    • Die erfindungsgemäß Methode der Überführung einer Flüssigkeit kann genauso auf den flüssigen Stickstoff 7 vom Kopf der Drucksäule als (weitere) "Überleitungsfraktion" angewandt werden. Das "erste Niveau" wird dabei durch den Flüssigkeitsspiegel innerhalb der Tasse 16 gebildet, in der die von Hauptkondensator 4 kommende Flüssigkeit aufgefangen wird. Unterkühlt wird wiederum im Gegenströmer 8. Der unterkühlte Stickstoff 17 fließt zu einem Entspannungsventil 18, das auf einem Zwischenniveau hz' angeordnet ist und schließlich weiter zu der Einspeisestelle 19 ("zweites Niveau" h2') am Kopf der Niederdrucksäule.The method of transferring a liquid according to the invention can also be applied the liquid nitrogen 7 from the top of the pressure column as a (further) "transfer fraction" be applied. The "first level" is due to the liquid level formed inside the cup 16 in which the coming from the main capacitor 4 Liquid is collected. Again, the countercurrent 8 is supercooled supercooled nitrogen 17 flows to an expansion valve 18 which is on a Intermediate level hz 'is arranged and finally further to the feed point 19th ("second level" h2 ') at the head of the low pressure column.

    Wird zusätzlich Argon gewonnen, wie es in der Zeichnung dargestellt ist, kann die Erfindung auch auf den Transport einer flüssigen Überleitungsfraktion in den Verdampfungsraum des Kopfkondensators einer Rohargonsäule angewandt werden. Die Rohargonsäule wird in dem Beispiel durch zwei Abschnitte 20a, 20b gebildet, deren Funktion im europäischen Patent EP 628777 B1 und in dem korrespondierenden US-Patent US 5426946 ausführlich beschrieben ist. Die Erfindung kann bei jeder bekannten Art der Rohargongewinnung eingesetzt werden, bei der eine argonhaltige Sauerstofffraktion 21 aus der Niederdrucksäule 5 in eine Rohargonsäule eingeleitet wird, wobei im oberen Bereich der Rohargonsäule ein an Sauerstoff abgereichertes Argonprodukt 22a, 22b in gasförmigem und/oder flüssigem Zustand anfällt. If argon is also obtained, as shown in the drawing, the Invention also for the transport of a liquid transfer fraction in the Evaporation space of the top condenser of a crude argon column can be used. The crude argon column is formed in the example by two sections 20a, 20b, their function in European patent EP 628777 B1 and in the corresponding U.S. Patent US 5,426,946 is described in detail. The invention can be used by anyone known type of raw argon extraction are used, in which an argon-containing Oxygen fraction 21 introduced from the low pressure column 5 into a crude argon column is, with an oxygen-depleted in the upper area of the crude argon column Argon product 22a, 22b is obtained in the gaseous and / or liquid state.

    Die weitere Überleitungsfraktion wird in dem in der Zeichnung dargestellten Beispiel durch einen Teil 13a der unterkühlten Sumpfflüssigkeit 6 aus der Drucksäule 5 gebildet. Sie wird in einem Entspannungsventil 14a entspannt, das auf einem Zwischenniveau angeordnet ist. Dieses Zwischenniveau liegt in dem Beispiel auf derselben oder etwa derselben Höhe wie das Zwischenniveau hz. Die in 14a entspannte Überleitungsfraktion 15a von Sumpf 12 der Drucksäule 3 wird auf einem "zweiten Niveau" h2" in den Verdampfungsraum 23 des Kopfkondensators der Rohargonsäule eingeführt.The further transition fraction is in the example shown in the drawing through part 13a of the supercooled sump liquid 6 from the pressure column 5 educated. It is relaxed in an expansion valve 14a, which is on a Intermediate level is arranged. This intermediate level is in the example the same or approximately the same height as the intermediate level hz. The in 14a relaxed transfer fraction 15a of sump 12 of the pressure column 3 is on a "second level" h2 "in the evaporation chamber 23 of the top condenser Raw argon column introduced.

    Claims (6)

    Verfahren zur Tieftemperaturzerlegung von Luft, bei dem Einsatzluft (1) in eine erste Rektifiziersäule (3) eingeleitet wird und eine Überleitungsfraktion (6, 7) der Dichte ρ in flüssigem Zustand aus einem Reservoir (24, 16) innerhalb der ersten Rektifiziersäule (3) entnommen, entspannt (14, 14a, 18) und einem weiteren Verfahrensschritt (5, 23) zugeleitet wird, wobei sich der Flüssigkeitsspiegel in dem Reservoir (24, 16) auf einem ersten Niveau h1 befindet und unter einem ersten Druck p1 steht, die entspannte Überleitungsfraktion dem weiteren Verfahrensschritt (5, 23) auf einem zweiten, höheren Niveau h2 (h2 > h1) und unter einem zweiten, niedrigeren Druck (p2 < p1) zugeführt wird, die Differenz der beiden Drücke Δp = p1 - p2 kleiner ist als der durch eine Flüssigkeitssäule der Überleitungsfraktion zwischen dem ersten und dem zweiten Niveau erzeugten hydrostatischen Druck (phydr = ρ · g · [h2-h1]) Δp = p1 - p2 < ρ · g · [h2 - h1]   (g: Erdbeschleunigung), dadurch gekennzeichnet, daß die Entspannung (14, 14a, 18) so durchgeführt wird, daß die beim Entspannen entstehenden Gasblasen die Dichte der Überleitungsfraktion soweit verringern, daß die Druckdifferenz Δp ausreicht, um die Überleitungsfraktion dem weiteren Verfahrensschritt (5, 23) zuzuführen. Method for the low-temperature decomposition of air, in which feed air (1) is introduced into a first rectification column (3) and a transfer fraction (6, 7) of density ρ in the liquid state from a reservoir (24, 16) within the first rectification column (3) removed, relaxed (14, 14a, 18) and a further process step (5, 23) is fed, wherein the liquid level in the reservoir (24, 16) is at a first level h1 and is under a first pressure p1, the relaxed transfer fraction is fed to the further process step (5, 23) at a second, higher level h2 (h2> h1) and under a second, lower pressure (p2 <p1), the difference between the two pressures Δp = p1 - p2 is smaller than the hydrostatic pressure generated by a liquid column of the transfer fraction between the first and the second level (p hydr = ρ · g · [h2-h1]) Δp = p1 - p2 <ρ · g · [h2 - h1] (g: gravitational acceleration), characterized in that the expansion (14, 14a, 18) is carried out in such a way that the gas bubbles formed during the expansion reduce the density of the transfer fraction to such an extent that the pressure difference Δp is sufficient to supply the transfer fraction to the further process step (5, 23). Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Überleitungsfraktion (6, 7) vor dem Entspannen (14, 14a, 18) durch indirekten Wärmeaustausch (8) unterkühlt wird.Method according to claim 1, characterized in that the transfer fraction (6, 7) is subcooled by indirect heat exchange (8) before the expansion (14, 14a, 18). Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die Unterkühlung (8) so durchgeführt wird, daß die Überleitungsfraktion (13, 13a, 17) unmittelbar stromaufwärts des Entspannens (14, 14a, 18) vollständig oder im wesentlichen vollständig in flüssiger Form vorliegt.Method according to Claim 2, characterized in that the supercooling (8) is carried out in such a way that the transfer fraction (13, 13a, 17) is completely or substantially completely in liquid form immediately upstream of the expansion (14, 14a, 18). Vorrichtung zur Tieftemperaturzerlegung von Luft, die für mindestens einen Betriebsfall ausgelegt ist und eine erste Rektifiziersäule (3) mit einem Reservoir (24, 16) für eine flüssige Überleitungsfraktion und eine Flüssigkeitsleitung (6 - 13 - 15, 6 - 13a - 15a, 7 - 17 - 19) aufweist, die auf mit dem Reservoir (24, 16) in der ersten Rektifiziersäule (3) und mit einem weiteren Behälter (5, 23) verbunden ist und zwischen diesen Verbindungen ein Entspannungsventil (14, 14a, 18) aufweist, wobei in dem Betriebsfall sich der Flüssigkeitsspiegel in dem Reservoir (24, 16) auf einem ersten Niveau h1 befindet und unter einem ersten Druck p1 steht, in dem weiteren Behälter (5, 23) an der die Stelle der Verbindung zwischen Flüssigkeitsleitung (15, 15a, 19) und weiterem Behälter (5, 23) in dem Betriebsfall ein zweiter Druck (p2) herrscht, die Stelle der Verbindung zwischen Flüssigkeitsleitung (15, 15a, 19) und weiterem Behälter (5, 23) auf einem zweiten, höheren Niveau h2 (h2 > h1) angeordnet ist, die Differenz der beiden Drücke Δp = p1 - p2 in dem Betriebsfall kleiner ist als der durch eine Flüssigkeitssäule der Überleitungsfraktion zwischen dem ersten und dem zweiten Niveau erzeugten hydrostatischen Druck (phydr = ρ·g·[h2-h1]) ist: Δp = p1 - p2 < ρ·g·[h2-h1]   g: Erdbeschleunigung. dadurch gekennzeichnet, daß das Entspannungsventil (14, 14a, 18) so angeordnet ist, daß in dem Betriebsfall die beim Entspannen entstehenden Gasblasen den beim Entspannen die Dichte der Überleitungsfraktion soweit verringern, daß die Druckdifferenz Δp ausreicht, um die Überleitungsfraktion in dem weiteren Behälter (5, 23) zuzuführen. Device for the low-temperature separation of air, which is designed for at least one operating case and a first rectification column (3) with a reservoir (24, 16) for a liquid transfer fraction and a liquid line (6 - 13 - 15, 6 - 13a - 15a, 7 - 17 - 19), which is connected to the reservoir (24, 16) in the first rectification column (3) and to a further container (5, 23) and has an expansion valve (14, 14a, 18) between these connections, in which in the operating case, the liquid level in the reservoir (24, 16) is at a first level h1 and is under a first pressure p1, in the further container (5, 23) at which the point of connection between the liquid line (15, 15a, 19) and the further container (5, 23) there is a second pressure (p2) in the operating case, the location of the connection between the liquid line (15, 15a, 19) and the further container (5, 23) is arranged at a second, higher level h2 (h2> h1), the difference between the two pressures Δp = p1 - p2 in the operating case is smaller than the hydrostatic pressure generated by a liquid column of the transfer fraction between the first and the second level (p hydr = ρ · g · [h2-h1]): Δp = p1 - p2 <ρ · g · [h2-h1] g: gravitational acceleration. characterized in that the expansion valve (14, 14a, 18) is arranged in such a way that in the operating case the gas bubbles formed during the expansion reduce the density of the transfer fraction during expansion so that the pressure difference Δp is sufficient to reduce the transfer fraction in the further container ( 5, 23). Vorrichtung nach Anspruch 4, gekennzeichnet durch einen Wärmetauscher (8) zur Abkühlung der Überleitungsfraktion durch indirekten Wärmeaustausch, der in der Flüssigkeitsleitung (6 - 13 - 15, 6 - 13a - 15a, 7 - 17 - 19) stromaufwärts des Entspannungsventils (14, 14a, 18) angeordnet ist.Apparatus according to claim 4, characterized by a heat exchanger (8) for cooling the transfer fraction by indirect heat exchange, which in the liquid line (6 - 13 - 15, 6 - 13a - 15a, 7 - 17 - 19) upstream of the expansion valve (14, 14a , 18) is arranged. Vorrichtung nach Anspruch 5, dadurch gekennzeichnet, daß der Wärmetauscher (8) so angeordnet ist, daß in dem Betriebsfall die Überleitungsfraktion unmittelbar stromaufwärts des Entspannungsventils (14, 14a, 18) vollständig oder im wesentlichen vollständig in flüssiger Form vorliegt.Apparatus according to claim 5, characterized in that the heat exchanger (8) is arranged in such a way that in the operating case the transfer fraction is completely or essentially completely in liquid form immediately upstream of the expansion valve (14, 14a, 18).
    EP99112289A 1999-05-12 1999-06-25 Process and device for cryogenic air separation Expired - Lifetime EP1052465B1 (en)

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    FR2853405A1 (en) * 2003-04-01 2004-10-08 Air Liquide Cryogenic distillation air separation procedure and plant uses lightening gas formed at least partly from purging gas drawn from vaporizer-condenser

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