EP1319912A1 - Device and process for obtaining gaseous oxygen under high pressure - Google Patents

Device and process for obtaining gaseous oxygen under high pressure Download PDF

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Publication number
EP1319912A1
EP1319912A1 EP02002634A EP02002634A EP1319912A1 EP 1319912 A1 EP1319912 A1 EP 1319912A1 EP 02002634 A EP02002634 A EP 02002634A EP 02002634 A EP02002634 A EP 02002634A EP 1319912 A1 EP1319912 A1 EP 1319912A1
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Prior art keywords
pressure column
high pressure
secondary condenser
line
column
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EP02002634A
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German (de)
French (fr)
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Augustin Rampp
Michael Lauter
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Linde GmbH
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Linde GmbH
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Priority to EP02027308A priority Critical patent/EP1319913A1/en
Publication of EP1319912A1 publication Critical patent/EP1319912A1/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
    • F25J3/04248—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
    • F25J3/0429—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 feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
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    • 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/04103—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression using solely hydrostatic liquid head
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    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
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    • F25J3/04236—Integration of different exchangers in a single core, so-called integrated cores
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    • 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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
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    • 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
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    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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    • 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
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    • 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
    • F25J3/04854—Safety aspects of operation
    • F25J3/0486—Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
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    • 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
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    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
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    • 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.
    • F25J3/04884—Arrangement of reboiler-condensers
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
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    • 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
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    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
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    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J2210/50—Oxygen
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    • F25J2250/50—One fluid being oxygen
    • 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
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    • Y10S62/00—Refrigeration
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Abstract

Device for producing gaseous oxygen under elevated pressure comprises distillation column system consisting of low pressure column arranged above high pressure column; condenser-evaporator having liquefying and evaporation chamber; process air line connected to high pressure column; transfer line for introducing fraction from high pressure into low pressure column; liquid line; and product line. <??>Device for producing gaseous oxygen under elevated pressure comprises a distillation column system consisting of a low pressure column (107) arranged above a high pressure column (106); a condenser-evaporator (102) having a liquefying chamber and an evaporation chamber and arranged below the sump of the low pressure column; a process air line (1-4) connected to the high pressure column; a transfer line (18, 19) for introducing a fraction from the high pressure column into the low pressure column; a liquid line (28) for removing a liquid oxygen fraction from the low pressure column; and a product line (29, 30) for gaseous oxygen under elevated pressure which is connected to the evaporation chamber of the condenser-evaporator. The condenser-evaporator is arranged below the high pressure column. <??>An Independent claim is also included for a process for producing gaseous oxygen under elevated pressure.

Description

Die Erfindung betrifft eine Vorrichtung zur Erzeugung gasförmigen Sauerstoffs unter erhöhtem Druck mit einem Destilliersäulen-System, das eine Hochdrucksäule und eine Niederdrucksäule aufweist, wobei die Niederdrucksäule oberhalb der Hochdrucksäule angeordnet ist, mit einem Nebenkondensator, der einen Verflüssigungsraum und einen Verdampfungsraum aufweist und unterhalb des Sumpfs der Niederdrucksäule angeordnet ist, mit einer Einsatzluft-Leitung, die mit der Hochdrucksäule verbunden ist, mit mindestens einer Übergangsleitung zur Einleitung einer Fraktion aus der Hochdrucksäule in die Niederdrucksäule, mit einer Flüssigkeitsleitung zum Entnehmen einer flüssigen Sauerstofffraktion aus der Niederdrucksäule, wobei die Flüssigkeitsleitung in den Verdampfungsraum des Nebenkondensators führt, und mit einer Produktleitung für gasförmigen Sauerstoff unter erhöhtem Druck, die mit dem Verdampfungsraum des Kondensator-Verdampfers verbunden ist.The invention relates to a device for generating gaseous oxygen under increased pressure with a distillation column system that includes a high pressure column and a Has low pressure column, the low pressure column above the high pressure column is arranged, with a secondary condenser, which has a liquefaction space and Has evaporation space and below the bottom of the low pressure column is arranged, with a feed air line which is connected to the high pressure column, with at least one transition line for the introduction of a fraction from the High pressure column in the low pressure column, with a liquid line for removal a liquid oxygen fraction from the low pressure column, the Liquid line leads into the evaporation chamber of the secondary condenser, and with a product line for gaseous oxygen under increased pressure, which with the Evaporation chamber of the condenser-evaporator is connected.

Das Destilliersäulen-System, beispielsweise eine Linde-Doppelsäulen-Anlage, dient zur Tieftemperatur-Zerlegung der Einsatzluft in Sauerstoff und Stickstoff. Die Grundlagen der Tieftemperatur-Zerlegung von Luft im Allgemeinen sowie der Aufbau von Doppelsäulen-Anlagen im Speziellen sind in der Monografie "Tieftemperaturtechnik" von Hausen/Linde (2. Auflage, 1985) und in einem Aufsatz von Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, Seite 35) beschrieben. Hochdrucksäule und Niederdrucksäule stehen im Regelfall über einen Hauptkondensator in Wärmeaustausch-Beziehung, in dem Kopfgas der Hochdrucksäule gegen verdampfende Sumpfflüssigkeit der Niederdrucksäule verflüssigt wird.The distillation column system, for example a Linde double column system, is used for the low-temperature decomposition of the feed air into oxygen and nitrogen. The Basics of the low-temperature decomposition of air in general as well as the structure of double column systems in particular are in the monograph "Low temperature technology" by Hausen / Linde (2nd edition, 1985) and in an article by Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, page 35). High-pressure column and low-pressure column are usually above one Main condenser in heat exchange relationship, in the top gas of the High pressure column against evaporating sump liquid of the low pressure column is liquefied.

Eine Vorrichtung der eingangs genannten Art ist aus DE 2323941 A, EP 384483 B1 und EP 1074805 A1 bekannt. Der Nebenkondensator dient zur Verdampfung. Er ist üblicherweise neben der Hochdrucksäule angeordnet.A device of the type mentioned at the outset is known from DE 2323941 A, EP 384483 B1 and EP 1074805 A1. The secondary condenser is used for evaporation. He is usually arranged next to the high pressure column.

Destilliersäulen-System und Nebenkondensator, meist auch ein Hauptwärmetauscher zur Abkühlung der Einsatzluft und gegebenenfalls ein Unterkühlungs-Gegenströmer müssen gegen den Eintrag von Wärme isoliert werden. Hierzu dient im Allgemeinen eine oder mehrere mit Pulver (Perlite) gefüllte Hüllen, so genannte Coldboxen.Distillation column system and secondary condenser, usually also a main heat exchanger for cooling the feed air and, if necessary, a subcooling counterflow must be insulated against the entry of heat. This is generally used one or more envelopes filled with powder (perlite), so-called cold boxes.

Als "Nebenkondensator" (side condenser) wird hier ein Kondensator-Verdampfer bezeichnet, der außerhalb der Niederdrucksäule angeordnet ist und dessen Verdampfungsseite während des Betriebs der Anlage ein unter einem höheren Druck als die Niederdrucksäule steht. Dort verdampfter Sauerstoff wird dann unter einem entsprechend erhöhten Druck als gasförmiges Produkt gewonnen. Die Druckerhöhung wird durch das geodätische Gefälle bewirkt (und gegebenenfalls zusätzlich durch eine Pumpe). Der Nebenkondensator ist vorzugsweise als Flüssigkeitsbadverdampfer (Umlaufverdampfer) ausgeführt: Ein Plattenwärmetauscherblock enthält Verdampfungs- und Verflüssigungspassagen. Er ist in einem Behälter angeordnet, der während des Betriebs teilweise mit zu verdampfender Flüssigkeit gefüllt ist. Die Flüssigkeit wird mittels des Thermosiphon-Effekt durch die Verdampfungspassagen des Plattenwärmetauscherblocks umgeworfen. Der Verdampfungsraum wird durch diese Verdampfungspassagen und durch den Außenraum zwischen Block und Behälterwand gebildet, der Verflüssigungsraum durch die Verflüssigungspassagen.A "condenser" is used here as a "side condenser" referred to, which is arranged outside the low pressure column and its Evaporation side during operation of the plant under a higher pressure than the low pressure column stands. Evaporated oxygen there is then under one correspondingly increased pressure obtained as a gaseous product. The pressure increase is caused by the geodetic gradient (and possibly also by a Pump). The secondary condenser is preferably a liquid bath evaporator (Circulation evaporator): One plate heat exchanger block contains Evaporation and liquefaction passages. It is placed in a container that is partially filled with liquid to be evaporated during operation. The Liquid is released through the evaporation passages by means of the thermosiphon effect of the plate heat exchanger block overturned. The evaporation space is through these evaporation passages and through the outside space between block and Container wall formed, the liquefaction room through the liquefaction passages.

Der Erfindung liegt die Aufgabe zugrunde, eine Vorrichtung der eingangs genannten Art besonders kostengünstig und insbesondere besonders kompakt zu gestalten.The invention has for its object a device of the aforementioned Art to make particularly inexpensive and especially particularly compact.

Zu diesem Zweck war es bisher üblich, alle Apparateteile, sogar die Kolonnen, nebeneinander anzuordnen (siehe zum Beispiel DE 19904526).For this purpose it has been customary up to now to have all parts of the apparatus, even the columns, to be arranged side by side (see for example DE 19904526).

Bei der Erfindung wird diese Aufgabe dadurch gelöst, dass der Nebenkondensator unterhalb der Hochdrucksäule angeordnet ist. Vorzugsweise sind Nebenkondensator. Hochdrucksäule und Niederdrucksäule in einer Linie untereinander angeordnet. Eine gemeinsame Coldbox, die alle drei Apparateteile umschließt kann dadurch besonders kompakt und damit kostengünstig ausgeführt werden. Ein weiterer Vorteil ergibt sich durch den größeren vertikalen Abstand zwischen Niederdrucksäule und Nebenkondensator. Entsprechend stärker ist die Druckerhöhung, die sich allein durch das Gefälle zwischen Niederdrucksäule und Nebenkondensator ergibt, also ohne Energiezufuhr von außen. Das gasförmige Sauerstoffprodukt kann also unter einem besonders hohen Druck gewonnen werden, beispielsweise 1,5 bis 3,5 bar, vorzugsweise 2 bis 2,8 bar. Dabei beträgt der Betriebsdruck der Säulen des Destilliersäulen-Systems (jeweils am Kopf) beispielsweise 5 bis 9 bar, vorzugsweise 6,0 bis 7,5 bar in der Hochdrucksäule und beispielsweise 1,3 bis 2,0 bar, vorzugsweise 1,5 bis 1,8 bar in der NiederdrucksäuleIn the invention, this object is achieved in that the secondary capacitor is arranged below the high pressure column. Secondary capacitors are preferred. High pressure column and low pressure column arranged in a line one below the other. A Common cold box, which encloses all three parts of the apparatus, can be special compact and therefore inexpensive. Another advantage arises due to the larger vertical distance between the low pressure column and Besides capacitor. The increase in pressure, which is reflected solely by the gradient between the low pressure column and the secondary condenser results, i.e. without External energy supply. The gaseous oxygen product can therefore be under one particularly high pressure can be obtained, for example 1.5 to 3.5 bar, preferably 2 to 2.8 bar. The operating pressure of the columns is Distillation column system (each at the head), for example 5 to 9 bar, preferably 6.0 to 7.5 bar in the high pressure column and for example 1.3 to 2.0 bar, preferably 1.5 to 1.8 bar in the low pressure column

Vorzugsweise wird die Einsatzluft-Leitung durch den Verflüssigungsraum des Nebenkondensators geführt. Die Einsatzluft dient damit als Heizmittel für die Verdampfung der flüssigen Sauerstofffraktion und kondensiert dabei teilweise oder vollständig.Preferably, the feed air line through the liquefaction room of the Secondary condenser performed. The feed air thus serves as a heating medium for the Evaporation of the liquid oxygen fraction and partially condenses or Completely.

Dabei ist es günstig, wenn die Einsatzluft-Leitung und der Nebenkondensator so ausgebildet sind, dass während des Betriebs der Vorrichtung die Einsatzluft in dem Nebenkondensator nur partiell kondensiert wird, beispielsweise zu 30 mol% oder weniger, vorzugsweise zu 25 bis 30 mol%. Damit kann einerseits die gesamte Einsatzluft (ggf. abzüglich einer Turbinenluftmenge) durch den Nebenkondensator geführt werden, und weitere Einsatzluft-Leitungen sind unnötig. Andererseits wird bei der nur teilweisen Kondensation eine höhere Verdampfungstemperatur bei gleichem Druck erreicht; umgekehrt reicht bei gleichem Sauerstoff-Produktdruck ein niedrigerer Luftdruck aus. Der Druck im Verflüssigungsraum des Nebenkondensators beträgt vorzugsweise 6 bis 8 bar. Die partiell kondensierte Einsatzluft aus dem Nebenkondensator kann in einen Abscheider (Phasentrenner) eingeleitet werden, der beispielsweise unmittelbar neben dem Nebenkondensator innerhalb der Coldbox angeordnet ist.It is advantageous if the feed air line and the secondary condenser are so are formed so that the feed air in the Auxiliary condenser is only partially condensed, for example 30 mol% or less, preferably 25 to 30 mol%. On the one hand, the entire Feed air (possibly less a turbine air quantity) through the secondary condenser out, and additional emergency air lines are unnecessary. On the other hand, at the only partial condensation a higher evaporation temperature at the same Pressure reached; conversely, a lower one is sufficient for the same oxygen product pressure Air pressure off. The pressure in the liquefaction chamber of the secondary condenser is preferably 6 to 8 bar. The partially condensed feed air from the Auxiliary capacitor can be introduced into a separator (phase separator) for example, right next to the secondary condenser inside the cold box is arranged.

Jede Luftzerlegungs-Anlage weist einen Hauptwärmetauscher zur Abkühlung von Einsatzluft gegen Produktströme auf. Bei der erfindungsgemäßen Vorrichtung ist es günstig, wenn dieser Hauptwärmetauscher unterhalb der Hochdrucksäule angeordnet ist, insbesondere zwischen Hochdrucksäule und Nebenkondensator. Dadurch kann auch der Hauptwärmetauscher von der gemeinsamen, kompakten Coldbox umschlossen werden. Eine separate Isolierung und eine voluminöse Gestaltung der Box können vermieden werden. Die zusätzliche Höhe des Hauptwärmetauschers bringt eine zusätzliche Druckerhöhung im Sauerstoffprodukt mit sich.Each air separation plant has a main heat exchanger for cooling Operating air against product flows. It is with the device according to the invention favorable if this main heat exchanger is arranged below the high pressure column is, especially between the high pressure column and secondary condenser. This can also the main heat exchanger from the common, compact cold box be enclosed. Separate insulation and a voluminous design of the Boxes can be avoided. The additional height of the main heat exchanger brings with it an additional pressure increase in the oxygen product.

Häufig werden die Einsatzflüssigkeit(en) für die Niederdrucksäule gegen das oder die Gasprodukte der Niederdrucksäule durch indirekten Wärmeaustausch in einem Unterkühlungs-Gegenströmer unterkühlt. Im Rahmend er Erfindung ist es günstig, wenn dieser weitere Wärmetauscher ebenfalls zwischen der Hochdrucksäule und dem Nebenkondensator angeordnet ist. Er kann damit ebenfalls von der gemeinsamen, kompakten Coldbox umschlossen werden. Eine separate Isolierung und eine voluminöse Gestaltung der Box können vermieden werden. Die zusätzliche Höhe des Hauptwärmetauschers bringt eine zusätzliche Druckerhöhung im Sauerstoffprodukt mit sich.Often, the feed liquid (s) for the low pressure column against the or Low pressure column gas products through indirect heat exchange in one Supercooling countercurrent supercooled. In the context of the invention, it is favorable if this additional heat exchanger also between the high pressure column and the Auxiliary capacitor is arranged. He can also use the common compact cold box. Separate insulation and one voluminous design of the box can be avoided. The additional amount of The main heat exchanger brings an additional pressure increase in the oxygen product yourself.

Vorzugsweise sind die Apparateteile in folgender Reihenfolge jeweils unmittelbar übereinander angeordnet: Nebenkondensator (ggf. mit Abscheider)- Unterkühlungs-Gegenströmer - Hauptwärmetauscher - Hochdrucksäule -Niederdrucksäule.The parts of the apparatus are preferably each direct in the following order arranged one above the other: secondary condenser (possibly with separator) - subcooling counterflow - Main heat exchanger - high pressure column - low pressure column.

Die Erfindung betrifft außerdem ein Verfahren zur Erzeugung gasförmigen Sauerstoffs unter erhöhtem Druck gemäß den Patentansprüchen 6 bis 10The invention also relates to a method for producing gaseous oxygen under increased pressure according to claims 6 to 10

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand von in den Zeichnungen schematisch dargestellten Ausführungsbeispielen näher erläutert. Hierbei zeigen:

Figur 1
ein beispielhafte räumliche Anordnung der verschiedenen Apparateteile,
Figuren 2 und 3
zwei Ausführungsformen der Erfindung mit Details zur Abfolge der Verfahrensschritte, mit Kälteerzeugung durch Turbine (Figur 2) beziehungsweise mit Kältezufuhr von außen (Figur 3).
The invention and further details of the invention are explained in more detail below on the basis of exemplary embodiments schematically illustrated in the drawings. Here show:
Figure 1
an exemplary spatial arrangement of the various parts of the apparatus,
Figures 2 and 3
two embodiments of the invention with details on the sequence of the process steps, with cooling by means of a turbine (FIG. 2) or with cooling from outside (FIG. 3).

Einander entsprechende Bauteile beziehungsweise Verfahrensschritte tragen in allen Zeichnungen dieselben Bezugszeichen.Corresponding components or process steps bear in all Drawings the same reference numerals.

In Figur 1 ist der räumliche Aufbau einer erfindungsgemäßen Vorrichtung schematisch dargestellt. Details wie Rohrleitungen, Ventile, Mess- und Stelleinrichtungen werden nicht gezeigt.In Figure 1 , the spatial structure of a device according to the invention is shown schematically. Details such as pipes, valves, measuring and actuating devices are not shown.

Innerhalb einer quader- oder zylinderförmigen Coldbox 101 sind übereinander sämtliche Apparateteile untergebracht, die einer Wärmeisolierung bedürfen. Als Unterstes stehen ein Nebenkondensator 102 und der zugehörige Abscheider 103 auf dem Boden. Darüber sind nacheinander der Unterkühlungs-Gegenströmer 104, der Hauptwärmetauscher 105, die Hochdrucksäule 106 und die Niederdrucksäule 107 angeordnet. Der Zwischenraum 108 zwischen den Apparaten und der Coldbox-Wand ist mit isolierendem Pulver (Perlite) gefüllt.Within a cuboid or cylindrical cold box 101 are one above the other all parts of the apparatus housed that require thermal insulation. As At the bottom are a secondary capacitor 102 and the associated separator 103 the floor. Above this are the supercooling counterflow 104, the Main heat exchanger 105, the high pressure column 106 and the low pressure column 107 arranged. The space 108 between the apparatus and the cold box wall is filled with insulating powder (perlite).

Unterkühlungs-Gegenströmer 104 und Hauptwärmetauscher 105 können auch als gemeinsamer, integrierten Wärmeaustauscher-Block ausgebildet sein (in Figur 1 nicht dargestellt).Subcooling counterflow 104 and main heat exchanger 105 can also be used as common, integrated heat exchanger block can be formed (not in Figure 1 ) Shown.

In den Figuren 2 und 3 ist die räumliche Anordnung der Apparateteile nicht vollständig dargestellt. Es gilt hierfür die in Figur 1 dargestellte Konstruktion.In Figures 2 and 3, the spatial arrangement of the parts of the apparatus is not complete shown. The construction shown in FIG. 1 applies here.

Bei dem Ausführungsbeispiel von Figur 2 wird verdichtete und gereinigte Luft 1 unter einem Druck von beispielsweise 8,2 bar herangeführt und tritt am warmen Ende in einen Hauptwärmetauscher 105 ein. Der Hauptteil der Luft wird über Leitung 2 am kalten Ende des Hauptwärmetauschers 105 entnommen und dem Verflüssigungsraum eines Nebenkondensators 102 zugeführt. Dort kondensiert die Luft partiell. Über Leitung 3 tritt ein Zwei-Phasen-Gemisch aus dem Nebenkondensator 102 aus, das etwa 26 mol% Flüssigkeit enthält. Es wird in einen Abscheider 103 eingeleitet. Der gasförmig verbliebene Luftanteil 4 wird auf etwa 6 bar abgedrosselt (5) und in die Hochdrucksäule 106 eines Destilliersäulen-Systems eingespeist, das außerdem ein Niederdrucksäule 107 aufweist. (Die Leitungen 1, 2, 3 und 4 stellen in dem Ausführungsbeispiel die "Einsatzluft-Leitung" dar.) Die Flüssigkeit 6 wird nach Durchgang durch ein andere Drosselventil 7 unter etwa 1,5 bar in die Niederdrucksäule 107 eingeführt.In the embodiment of FIG. 2 , compressed and cleaned air 1 is brought in under a pressure of, for example, 8.2 bar and enters a main heat exchanger 105 at the warm end. The main part of the air is removed via line 2 at the cold end of the main heat exchanger 105 and fed to the liquefaction space of a secondary condenser 102. The air condenses there partially. A two-phase mixture emerges from the secondary condenser 102 via line 3 and contains approximately 26 mol% of liquid. It is introduced into a separator 103. The gaseous air fraction 4 is throttled to about 6 bar (FIG. 5) and fed into the high pressure column 106 of a distillation column system, which also has a low pressure column 107. (Lines 1, 2, 3 and 4 represent the "feed air line" in the exemplary embodiment.) After passing through another throttle valve 7, the liquid 6 is introduced into the low-pressure column 107 under approximately 1.5 bar.

Gasförmiger Kopfstickstoff 8 der Hochdrucksäule 106 wird mindestens zu einem Teil 9 in einem Hauptkondensator gegen verdampfende Sumpfflüssigkeit der Niederdrucksäule 107 kondensiert. Der dabei gebildete flüssige Stickstoff 11 wird zu einem ersten Teil 12 als Rücklauf in die Hochdrucksäule 106 zurückgeleitet. Ein zweiter Teil 14 wird in einem Unterkühlungs-Gegenströmer 104 unterkühlt und über Leitung 15 und Ventil 16 auf den Kopf der Niederdrucksäule 107 aufgegeben. (Der Unterkühlungs-Gegenströmer 104 und der Hauptwärmetauscher sind bei dem Ausführungsbeispiel als integrierter Wärmeaustauscher-Block ausgebildet.) Der Flüssigstickstoff 15 dient hauptsächlich als Rücklauf in der Niederdrucksäule 107; er kann aber auch zu einem Teil 17 als druckloses Flüssigprodukt (LIN) entnommen werden. Ein weiterer Teil 13 des flüssigen Stickstoffs 11 aus dem Hauptkondensator 10 kann als Druck-Flüssigprodukt (PLIN) abgezogen werden.Gaseous top nitrogen 8 of the high pressure column 106 becomes at least part 9 in a main condenser against evaporating sump liquid Low pressure column 107 condensed. The liquid nitrogen 11 thus formed becomes a first part 12 is returned to the high-pressure column 106 as a return. On second part 14 is subcooled in a supercooling counterflow 104 and over Line 15 and valve 16 abandoned on the top of the low pressure column 107. (The Supercooling counterflow 104 and the main heat exchanger are in the Embodiment designed as an integrated heat exchanger block.) The Liquid nitrogen 15 serves mainly as a return in the low pressure column 107; he can also be taken to a part 17 as an unpressurized liquid product (LIN) become. Another part 13 of the liquid nitrogen 11 from the main condenser 10 can be deducted as a liquid pressure product (PLIN).

Die Sumpfflüssigkeit 18 der Hochdrucksäule 106 wird über den Unterkühlungs-Gegenströmer 104, Leitung 19 und Ventil 20 in die Niederdrucksäule übergeführt ("Übergangsleitung").The bottom liquid 18 of the high pressure column 106 is over the supercooling counterflow 104, line 19 and valve 20 transferred to the low pressure column ( "Transition line").

Als gasförmige Produkte der Niederdrucksäule 107 werden reiner und unreiner Stickstoff über die Produktleitung 21/22 beziehungsweise über die Restgasleitung 23/24/25 durch den Unterkühlungs-Gegenströmer 104 und den Hauptwärmetauscher 105 geführt und schließlich als Produkt (GAN) abgezogen beziehungsweise in die Atmosphäre abgeblasen beziehungsweise als Regeneriergas in einer Molekularsieb-Anlage zur Reinigung der Luft (nicht dargestellt) eingesetzt. Auch direkt aus der Hochdrucksäule kann ein Produkt gewonnen werden. Hierzu wird ein Teil 26 des Kopfstickstoffs 8 im Hauptwärmetauscher 105 angewärmt und als gasförmiges Druckstickstoff-Produkt 27 (PGAN) gewonnen.The gaseous products of the low pressure column 107 become cleaner and more impure Nitrogen via the product line 21/22 or via the residual gas line 23/24/25 through the supercooling counterflow 104 and the main heat exchanger 105 led and finally deducted as a product (GAN) or in the Blow off atmosphere or as a regeneration gas in a molecular sieve system used to purify the air (not shown). Also directly from the A high pressure column can be used to obtain a product. For this purpose, part 26 of the Head nitrogen 8 warmed in the main heat exchanger 105 and as a gaseous Compressed nitrogen product 27 (PGAN) won.

Vom Sumpf der Niederdrucksäule 107 wird eine flüssige Sauerstofffraktion 28 abgezogen, erfährt eine hydrostatische Druckerhöhung und wird in den Verdampfungsraum des Nebenkondensators 102 eingeleitet und dort wird teilweise verdampft. Der dabei gebildete gasförmige Sauerstoff 29 wird zum Hauptwärmetauscher geführt und schließlich über Leitung 30 als Druckgasprodukt (GOX) zu einem Verbraucher geführt. Der flüssig verbliebene Sauerstoff wird als Spülflüssigkeit 31 aus dem Verdampfungsraum des Nebenkondensators 102 abgezogen und entweder verworfen oder (wie in Figur 2 dargestellt) als Flüssigprodukt (LOX) gewonnen; alternativ oder zusätzlich ist eine Eindüsung in Leitung 30 möglich.A liquid oxygen fraction 28 becomes from the bottom of the low-pressure column 107 subtracted, experiences a hydrostatic pressure increase and is in the Evaporation space of the secondary condenser 102 is introduced and there is partial evaporated. The gaseous oxygen 29 thus formed becomes Main heat exchanger performed and finally via line 30 as a compressed gas product (GOX) led to a consumer. The remaining liquid oxygen is called Flushing liquid 31 from the evaporation space of the secondary condenser 102 withdrawn and either discarded or (as shown in Figure 2) as a liquid product (LOX) won; alternatively or additionally, injection into line 30 is possible.

Die für den Augleich der Isolationsverluste und für die Produktverflüssigung benötigte Kälte wird bei dem Ausführungsbeispiel von Figur 2 durch arbeitsleistende Entspannung eines Prozessstroms erzeugt. Hierzu wird ein Teilstrom 32 der Einsatzluft 1 bei einer Zwischentemperatur aus dem Hauptwärmetauscher 105 abgezogen, einer Entspannungsmaschine (beispielsweise Turbine) 33 zugeführt, dort auf etwa den Betriebsdruck der Niederdrucksäule 107 entspannt und über die Leitungen 34 und 35 in die Niederdrucksäule 107 eingeleitet. Insbesondere bei relativ großer Flüssigproduktion kann ein Teil 36 Turbinenluft 34 dem Restgas 23 zugemischt und gemeinsam mit diesem aus dem Verfahren entfernt werden.The one required for the equalization of the insulation losses and for the product liquefaction Cold is in the embodiment of Figure 2 by work Relaxation of a process stream generated. For this purpose, a partial flow 32 of the feed air 1 at an intermediate temperature from the main heat exchanger 105, one Relaxation machine (for example turbine) 33 supplied, there to about Operating pressure of the low pressure column 107 relaxed and via lines 34 and 35 introduced into the low pressure column 107. Especially with relatively large ones Liquid production can be mixed with a portion 36 of turbine air 34 and the residual gas 23 be removed from the process together with this.

Figur 3 unterscheidet sich von Figur 2 durch die abweichende Form der Kältezufuhr. Hier wird auf eine Turbine verzichtet. Der Kältebedarf wird stattdessen durch Flüssigzufuhr von außen (liquid assist) gedeckt. Hierzu wird flüssiger Sauerstoff 337 aus einem Flüssigtank in den unteren Bereich der Niederdrucksäule 107 eingeleitet. Alternativ oder ergänzend ist die Zufuhr von tiefkalter Flüssigkeit aus einem Stickstoff-Flüssigtank. Der flüssige Stickstoff kann über Leitung 338 in den oberen Bereich der Niederdrucksäule 107 eingeführt werden und/oder über Leitung 339 in den oberen Bereich der Hochdrucksäule 106. Ebenso kann verflüssigte Luft oder jedes andere flüssige Gemisch aus Luftkomponenten zur Deckung des Kältebedarfs eingesetzt werden. Figure 3 differs from Figure 2 in the different form of cold supply. There is no turbine here. The cooling requirement is instead covered by liquid supply from outside (liquid assist). For this purpose, liquid oxygen 337 is introduced from a liquid tank into the lower area of the low pressure column 107. Alternatively or additionally, the supply of cryogenic liquid from a nitrogen liquid tank. The liquid nitrogen can be introduced via line 338 into the upper region of the low-pressure column 107 and / or via line 339 into the upper region of the high-pressure column 106. Liquefied air or any other liquid mixture of air components can also be used to cover the cooling requirement.

Claims (10)

Vorrichtung zur Erzeugung gasförmigen Sauerstoffs unter erhöhtem Druck mit einem Destilliersäulen-System, das eine Hochdrucksäule (106) und eine Niederdrucksäule (107) aufweist, wobei die Niederdrucksäule (107) oberhalb der Hochdrucksäule (106) angeordnet ist, mit einem Nebenkondensator (102), der einen Verflüssigungsraum und einen Verdampfungsraum aufweist und unterhalb des Sumpfs der Niederdrucksäule (107) angeordnet ist, mit einer Einsatzluft-Leitung (1, 2, 3, 4), die mit der Hochdrucksäule (106) verbunden ist, mit mindestens einer Übergangsleitung (18-19; 11-14-15) zur Einleitung einer Fraktion aus der Hochdrucksäule (106) in die Niederdrucksäule (107), mit einer Flüssigkeitsleitung (28) zum Entnehmen einer flüssigen Sauerstofffraktion aus der Niederdrucksäule (107), wobei die Flüssigkeitsleitung (28) in den Verdampfungsraum des Nebenkondensators (102) führt, und mit einer Produktleitung (29, 30) für gasförmigen Sauerstoff unter erhöhtem Druck, die mit dem Verdampfungsraum des Kondensator-Verdampfers (102) verbunden ist, dadurch gekennzeichnet, dass der Nebenkondensator (102) unterhalb der Hochdrucksäule (106) angeordnet ist.Device for generating gaseous oxygen under increased pressure with a distillation column system which has a high-pressure column (106) and a low-pressure column (107), the low-pressure column (107) being arranged above the high-pressure column (106), with a secondary condenser (102), which has a liquefaction space and an evaporation space and is arranged below the bottom of the low-pressure column (107), with a feed air line (1, 2, 3, 4) which is connected to the high pressure column (106), with at least one transition line (18-19; 11-14-15) for introducing a fraction from the high pressure column (106) into the low pressure column (107), with a liquid line (28) for withdrawing a liquid oxygen fraction from the low pressure column (107), the liquid line (28) leading into the evaporation space of the secondary condenser (102), and with a product line (29, 30) for gaseous oxygen under increased pressure, which is connected to the evaporation space of the condenser-evaporator (102), characterized in that the secondary condenser (102) is arranged below the high pressure column (106). Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass die Einsatzluft-Leitung (1, 2, 3, 4) durch den Verflüssigungsraum des Nebenkondensators (102) führt.Apparatus according to claim 1, characterized in that the feed air line (1, 2, 3, 4) leads through the liquefaction space of the secondary condenser (102). Vorrichtung nach Anspruch 2, dadurch gekennzeichnet, dass die Einsatzluft-Leitung (1, 2, 3, 4) und der Nebenkondensator (102) so ausgebildet sind, dass während des Betriebs der Vorrichtung die Einsatzluft in dem Nebenkondensator (102) nur partiell kondensiert wird.Apparatus according to claim 2, characterized in that the feed air line (1, 2, 3, 4) and the secondary condenser (102) are designed such that the feed air in the secondary condenser (102) is only partially condensed during operation of the apparatus , Vorrichtung nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Einsatzluft-Leitung (1, 2, 3, 4) durch einen Hauptwärmetauscher (105) zur Abkühlung der Einsatzluft gegen Produktströme führt und der Hauptwärmetauscher (105) unterhalb der Hochdrucksäule (106) angeordnet ist, insbesondere zwischen Hochdrucksäule (106) und Nebenkondensator (102).Device according to one of claims 1 to 3, characterized in that the feed air line (1, 2, 3, 4) leads through a main heat exchanger (105) to cool the feed air against product flows and the main heat exchanger (105) below the high pressure column (106 ) is arranged, in particular between the high pressure column (106) and secondary condenser (102). Vorrichtung nach einem der Ansprüche 1 bis 4, gekennzeichnet durch eine Gasprodukt-Leitung (21-22, 23-24-25) zum Abführen eines gasförmigen Produkts aus der Niederdrucksäule (107), wobei die Gasprodukt-Leitung (21-22, 23-24-25) mit einem Unterkühlungs-Gegenströmer (104) verbunden ist, durch den außerdem die Übergangsleitung (18-19; 11-14-15) führt, und wobei der Unterkühlungs-Gegenströmer (104) zwischen der Hochdrucksäule (106) und dem Nebenkondensator (102) angeordnet ist.Device according to one of claims 1 to 4, characterized by a gas product line (21-22, 23-24-25) for discharging a gaseous product from the low pressure column (107), the gas product line (21-22, 23- 24-25) is connected to a subcooling counterflow (104), through which the transition line (18-19; 11-14-15) also leads, and wherein the subcooling counterflow (104) between the high pressure column (106) and the Auxiliary capacitor (102) is arranged. Verfahren zur Erzeugung gasförmigen Sauerstoffs unter erhöhtem Druck in einem Destilliersäulen-System, das eine Hochdrucksäule (106) und eine Niederdrucksäule (107) aufweist, wobei die Niederdrucksäule (107) oberhalb der Hochdrucksäule (106) angeordnet ist, wobei bei dem Verfahren ein Einsatzluftstrom (1, 2, 3, 4) in die Hochdrucksäule (106) eingeleitet wird, mindestens eine Fraktion (18-19; 11-14-15) aus der Hochdrucksäule (106) in die Niederdrucksäule (107) geführt wird, eine flüssige Sauerstofffraktion der Niederdrucksäule (107) in den Verdampfungsraum des Nebenkondensators (102) eingeführt wird, der einen Verflüssigungsraum und einen Verdampfungsraum aufweist und unterhalb des Sumpfs der Niederdrucksäule (107) angeordnet ist, und gasförmiger Sauerstoff (29, 30) aus dem Verdampfungsraum des Kondensator-Verdampfers (102) abgezogen wird, dadurch gekennzeichnet, dass der Nebenkondensator (102) unterhalb der Hochdrucksäule (106) angeordnet ist.A method of generating gaseous oxygen under elevated pressure in a distillation column system having a high pressure column (106) and a low pressure column (107), the low pressure column (107) being located above the high pressure column (106), the method a feed air stream (1, 2, 3, 4) is introduced into the high pressure column (106), at least one fraction (18-19; 11-14-15) is led from the high pressure column (106) into the low pressure column (107), a liquid oxygen fraction of the low pressure column (107) is introduced into the evaporation space of the secondary condenser (102), which has a liquefaction space and an evaporation space and is arranged below the sump of the low pressure column (107), and gaseous oxygen (29, 30) is withdrawn from the evaporation space of the condenser-evaporator (102), characterized in that the secondary condenser (102) is arranged below the high pressure column (106). Verfahren nach Anspruch 6, dadurch gekennzeichnet, dass mindestens ein Teil der Einsatzluft (1, 2, 4) durch den Verflüssigungsraum des Nebenkondensators (102) geführt wird.A method according to claim 6, characterized in that at least part of the feed air (1, 2, 4) is passed through the liquefaction space of the secondary condenser (102). Verfahren nach Anspruch 7, dadurch gekennzeichnet, dass die Einsatzluft in dem Nebenkondensator (102) nur partiell kondensiert wird. A method according to claim 7, characterized in that the feed air in the secondary condenser (102) is only partially condensed. Verfahren nach einem der Ansprüche 6 bis 8, dadurch gekennzeichnet, dass die Einsatzluft (1) in einem Hauptwärmetauscher (105) gegen Produktströme (21, 23, 26) abgekühlt wird und der Hauptwärmetauscher (105) unterhalb der Hochdrucksäule (106) angeordnet ist, insbesondere zwischen Hochdrucksäule (106) und Nebenkondensator (102).Method according to one of claims 6 to 8, characterized in that the feed air (1) is cooled in a main heat exchanger (105) against product flows (21, 23, 26) and the main heat exchanger (105) is arranged below the high pressure column (106), in particular between high pressure column (106) and secondary condenser (102). Verfahren nach einem der Ansprüche 6 bis 9, dadurch gekennzeichnet, dass mindestens ein gasförmiger Produktstrom (21, 23) aus der Niederdrucksäule (107) abgezogen und in einem Unterkühlungs-Gegenströmer (104) gegen die Fraktion (18-19; 11-14-15) aus der Hochdrucksäule (106) angewärmt wird, wobei der Unterkühlungs-Gegenströmer (104) zwischen der Hochdrucksäule (106) und dem Nebenkondensator (102) angeordnet ist.Method according to one of claims 6 to 9, characterized in that at least one gaseous product stream (21, 23) is withdrawn from the low pressure column (107) and in a supercooling counterflow (104) against the fraction (18-19; 11-14- 15) is heated from the high-pressure column (106), the supercooling countercurrent (104) being arranged between the high-pressure column (106) and the secondary condenser (102).
EP02002634A 2001-12-14 2002-02-05 Device and process for obtaining gaseous oxygen under high pressure Withdrawn EP1319912A1 (en)

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