EP1146301A1 - Process and apparatus for the production of high pressure nitrogen from air separation - Google Patents

Process and apparatus for the production of high pressure nitrogen from air separation Download PDF

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Publication number
EP1146301A1
EP1146301A1 EP01108734A EP01108734A EP1146301A1 EP 1146301 A1 EP1146301 A1 EP 1146301A1 EP 01108734 A EP01108734 A EP 01108734A EP 01108734 A EP01108734 A EP 01108734A EP 1146301 A1 EP1146301 A1 EP 1146301A1
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EP
European Patent Office
Prior art keywords
pressure column
low
liquid
nitrogen
low pressure
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EP01108734A
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German (de)
French (fr)
Inventor
Jürgen Dipl.-Phys. Voit
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Linde GmbH
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Linde GmbH
Linde Gas AG
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Publication of EP1146301A1 publication Critical patent/EP1146301A1/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
    • F25J3/04321—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 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
    • 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
    • F25J3/04006—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
    • F25J3/04084—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 nitrogen
    • 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
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen

Definitions

  • the invention relates to a process for the production of pressure nitrogen by Cryogenic separation of air in a rectification system using a pressure column and has a low pressure column, wherein in the process feed air in one Main heat exchanger system is cooled and introduced into the pressure column, one oxygen-containing liquid fraction removed from the pressure column and into the Low pressure column is fed, gaseous nitrogen from the low pressure column in the liquefaction chamber of a top condenser through indirect heat exchange with a liquid evaporating in the evaporation space of the top condenser is at least partially condensed and with the liquid nitrogen from Liquefaction room of the top condenser or from the low pressure column deducted, brought to a pressure in the liquid state, which is the pressure of the Low pressure column exceeds, then evaporated and as a gaseous Pressure nitrogen product is discharged.
  • the invention is therefore based on the object of a method of the beginning Specify the type and a corresponding device that is economical are particularly cheap, in particular due to particularly low equipment costs and / or through greater flexibility with regard to product printing.
  • the "main heat exchanger system” is in the simplest case in the invention realized a single heat exchanger block in which the feed air cooled and the gaseous product fractions are warmed up. But it can also go through a plurality of heat exchanger blocks connected in parallel and / or in series are formed, of which in at least one of the liquid pressurized nitrogen in indirect heat exchange occurs with at least part of the feed air and thereby is evaporated.
  • the nitrogen can also be obtained under supercritical pressure are so that "evaporate” can also mean “pseudo-evaporate”.
  • a supercritical product pressure leads the pressure increase from the liquid to the supercritical state.
  • a gaseous nitrogen stream can be taken from the pressure column and can be obtained as a further gaseous nitrogen product.
  • compressed and cleaned air 1 is cooled in a main heat exchanger 2 and fed to a pressure column 4 under a pressure of 8.4 bar (3).
  • the rectification system also has a low-pressure column 5, which is operated at a pressure of 4.3 bar and is in heat-exchanging connection with the pressure column via a common condenser-evaporator (main condenser) 6.
  • a portion 8 of the nitrogen removed at the top of the pressure column is liquefied in the main condenser 6 and fed via lines 9 and 10 as a return to the pressure column and via 160, 15, 161 to the low pressure column 5.
  • Bottom liquid 11 of the pressure column is at least partially throttled into the low-pressure column 5 after hypothermia 15 as an oxygen-rich liquid fraction (12).
  • the rest of the supercooled oxygen-rich liquid fraction is expanded via the valve 163 into the evaporation space of the top condenser 17 of the low pressure column 5.
  • the bottom liquid 13 of the low-pressure column 5 is expanded (16) and then introduced into the evaporation space of the top condenser 17 of the low-pressure column 5.
  • gaseous nitrogen 18 condenses from the top of the low-pressure column 5; a first part of the condensate 19 is returned to the low-pressure column and used there as a return.
  • FIG. 1 Another part 20 of the liquid nitrogen 19 from the top condenser 17 is either as shown in Figure 1 taken from the low pressure column or directly branched off from line 19. (Alternatively, some floors can be removed possible below the head of the low pressure column 5).
  • This liquid nitrogen 20 is brought to an increased pressure (in the example 9 bar) in the liquid state (Pump 21), via line 22 to the main heat exchanger 2 and there under the increased pressure evaporated and warmed.
  • the warm nitrogen gas will eventually dissipated as a printed product 29. It can be in a gaseous state if necessary further compressed and, if desired, with one removed directly from the pressure column Pressure nitrogen 27, 28 are mixed. In the example, approx. 60% of the total pressure nitrogen product (28 + 29) from the low pressure column 5.
  • Cold is obtained here by work-relieving residual gas by at least a portion 150 of the impure oxygen 31 from the overhead condenser 17 the low pressure column 5 in a relaxation machine 133 from one Intermediate temperature of the main heat exchanger 2 is relaxed from work.
  • the turbine exhaust gas 151 is warmed up again in the heat exchanger 2 and as residual gas 152 discharged or for the regeneration of a device for the Purification of the feed air used.
  • the one in the relaxation machine 133 Mechanical energy obtained can be given to a generator or used for Compaction of a process fraction can be used, preferably by direct mechanical coupling of the relaxation machine 133 with a not shown Compressor.
  • FIG. 2 differs from FIG. 1 in that the insert for the turbine 133 does not come from the top condenser of the low pressure column, but from the main condenser 6.
  • oxygen-containing gas 31 ' is drawn off directly above the bottom of the low-pressure column 5.
  • the two columns 4, 5 can also be arranged side by side.
  • the main capacitor would be arranged at the top of the pressure column 4 and via a Liquid and a steam line with the lower end of the low pressure column connected.

Abstract

Production of compressed N2 by low temperature air separation in a rectification system involves contacting the compressed liquid N2 (22) in indirect heat exchange (2) with at least part of the inlet air (1) during evaporation. Production of compressed N2 by low temperature air separation in a rectification system comprises feeding cooled air from a main heat exchanger into a pressure column (4), passing at least part of the O2-containing liquid fraction to a low pressure column (5) while passing N2 gas into the liquefaction chamber of a head condenser (17) and at least partly condensing it by indirect heat exchange with an evaporating liquid (13), drawing the liquid N2 out of the condenser or the low-pressure column (5), compressing it at a pressure greater than that in the low-pressure column and then evaporating it and drawing it off as a compressed product, the novel feature being that the compressed liquid N2 is contacted in indirect heat exchange with at least part of the inlet air during evaporation. An Independent claim is also included for process apparatus comprising (a) an inlet system (1,3) feeding air through a main heat-exchanger system to a pressure column; (b) a pipe (11) feeding an O2-containing liquid fraction to a low-pressure column; (c) a head condenser (17) whose liquefaction chamber is connected to an upper part of the low-pressure column and which has a pipe (20,22) for liquid N2 connecting the liquefaction chamber to the low-pressure column via a compressor (21) to lead the liquid to the main heat exchanger; and (d) a compressed product pipe (29).

Description

Die Erfindung betrifft ein Verfahren zur Gewinnung von Druckstickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem, das eine Drucksäule und eine Niederdrucksäule aufweist, wobei bei dem Verfahren Einsatzluft in einem Hauptwärmetauschersystem abgekühlt und in die Drucksäule eingeleitet wird, eine sauerstoffhaltige flüssige Fraktion aus der Drucksäule entnommen und in die Niederdrucksäule eingespeist wird, gasförmiger Stickstoff aus der Niederdrucksäule im Verflüssigungsraum eines Kopfkondensators durch indirekten Wärmeaustausch mit einer im Verdampfungsraum des Kopfkondensators verdampfenden Flüssigkeit mindestens teilweise kondensiert wird und bei dem flüssiger Stickstoff vom Verflüssigungsraum des Kopfkondensators oder aus der Niederdrucksäule abgezogen, in flüssigem Zustand auf einen Druck gebracht wird, der den Druck der Niederdrucksäule übersteigt, anschließend verdampft und als gasförmiges Druckstickstoffprodukt abgeführt wird.The invention relates to a process for the production of pressure nitrogen by Cryogenic separation of air in a rectification system using a pressure column and has a low pressure column, wherein in the process feed air in one Main heat exchanger system is cooled and introduced into the pressure column, one oxygen-containing liquid fraction removed from the pressure column and into the Low pressure column is fed, gaseous nitrogen from the low pressure column in the liquefaction chamber of a top condenser through indirect heat exchange with a liquid evaporating in the evaporation space of the top condenser is at least partially condensed and with the liquid nitrogen from Liquefaction room of the top condenser or from the low pressure column deducted, brought to a pressure in the liquid state, which is the pressure of the Low pressure column exceeds, then evaporated and as a gaseous Pressure nitrogen product is discharged.

Ein derartiges Verfahren ist aus WO 9819122 bekannt. Hier wird insbesondere am Kopf der Niederdrucksäule gewonnener Stickstoff flüssig auf Druck gebracht, verdampft und als gasförmiges Druckstickstoffprodukt gewonnen. Die Verdampfung wird in einem Produktverdampfer durchgeführt, der mit Gas aus einer der Säulen beheizt wird. Dieser Prozeß ist an sich sehr günstig, erfordert aber einen separaten Wärmetauscher als Produktverdampfer; außerdem liegt der Produktdruck durch den Betriebsdruck der Säulen des Rektifiziersystems fest.Such a method is known from WO 9819122. Here in particular on The pressure from the top of the low-pressure column is brought under pressure, evaporated and obtained as a gaseous pressure nitrogen product. The evaporation is carried out in a product evaporator using gas from one of the columns is heated. This process is very cheap in itself, but requires a separate one Heat exchangers as product evaporators; in addition, the product pressure is due to the Operating pressure of the rectification system columns.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art und eine entsprechende Vorrichtung anzugeben, die wirtschaftlich besonders günstig sind, insbesondere durch besonders geringe Apparatekosten und/oder durch eine höhere Flexibilität hinsichtlich des Produktdrucks. The invention is therefore based on the object of a method of the beginning Specify the type and a corresponding device that is economical are particularly cheap, in particular due to particularly low equipment costs and / or through greater flexibility with regard to product printing.

Diese Aufgabe wird dadurch gelöst, daß der flüssig auf Druck gebrachte Stickstoff beim Verdampfen in indirekten Wärmeaustausch mit mindestens einem Teil der Einsatzluft tritt.This object is achieved in that the liquid pressurized nitrogen when evaporating in indirect heat exchange with at least part of the Air enters.

Mindestens ein Teil der Einsatzluft muß dabei selbstverständlich auf einen entsprechend hohen Druck verdichtet werden, wie es bei Innenverdichtungsverfahren üblich ist. Im Gegensatz zu bekannten Verfahren mit Innenverdichtung von Stickstoff (siehe z.B. EP 716280 A2) wird der flüssige Stickstoff jedoch nicht der Drucksäule, sondern der Niederdrucksäule (beziehungsweise deren Kopfkondensator) entnommen, was demgegenüber eine verbesserte Ausbeute an Druckstickstoff ermöglicht.Of course, at least a part of the input air must be on one correspondingly high pressure, as is the case with internal compression processes is common. In contrast to known processes with internal compression of nitrogen (see e.g. EP 716280 A2) the liquid nitrogen is not used in the pressure column, but the low pressure column (or its top condenser) taken, which in contrast an improved yield of pressurized nitrogen enables.

Das "Hauptwärmetauschersystem" ist bei der Erfindung im einfachsten Fall durch einen einzelnen Wärmetauscherblock realisiert, in dem die Einsatzluft abgekühlt und die gasförmigen Produktfraktionen angewärmt werden. Es kann aber auch durch mehrere parallel und/oder seriell verbundene Wärmetauscherblöcke gebildet werden, von denen in mindestens einem der flüssig auf Druck gebrachte Stickstoff in indirektem Wärmeaustausch mit mindestens einem Teil der Einsatzluft tritt und dabei verdampft wird.The "main heat exchanger system" is in the simplest case in the invention realized a single heat exchanger block in which the feed air cooled and the gaseous product fractions are warmed up. But it can also go through a plurality of heat exchanger blocks connected in parallel and / or in series are formed, of which in at least one of the liquid pressurized nitrogen in indirect heat exchange occurs with at least part of the feed air and thereby is evaporated.

Bei dem Verfahren kann der Stickstoff auch unter überkritischem Druck gewonnen werden, so daß "verdampfen" auch "pseudo-verdampfen" bedeuten kann. Im Falle eines überkritischen Produktdrucks führt die Druckerhöhung also vom flüssigen in den überkritischen Zustand.In the process, the nitrogen can also be obtained under supercritical pressure are so that "evaporate" can also mean "pseudo-evaporate". In the event of A supercritical product pressure leads the pressure increase from the liquid to the supercritical state.

Falls gewünscht, kann der Drucksäule ein gasförmiger Stickstoffstrom entnommen und als weiteres gasförmiges Stickstoffprodukt gewonnen werden.If desired, a gaseous nitrogen stream can be taken from the pressure column and can be obtained as a further gaseous nitrogen product.

Es ist günstig, wenn bei dem Verfahren ein sauerstoffhaltiger Strom aus dem Verdampfungsraum des Kopfkondensators und/oder aus einem unteren Bereich der Niederdrucksäule arbeitsleistend entspannt wird. Dadurch kann die Kälte gewonnen werden, die für den Ausgleich von Austausch- und Isolationsverlusten und gegebenenfalls für die Produktverflüssigung benötigt wird. It is advantageous if an oxygen-containing stream from the Evaporation space of the top condenser and / or from a lower area of the Low pressure column is relaxed while working. This can win the cold be used for the compensation of exchange and insulation losses and may be required for product liquefaction.

Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von Druckstickstoff gemäß Patentanspruch 5.Die Erfindung sowie weitere Einzelheiten der Erfindung werden im folgenden anhand von in den Zeichnungen dargestellten Ausführungsbeispielen näher erläutert. Hierbei zeigen:

Figur 1
ein erstes Ausführungsbeispiel des erfindungsgemäßen Verfahrens und einer entsprechenden Vorrichtung mit arbeitsleistender Entspannung von Restgas aus dem Kopfkondensator der Niederdrucksäule und
Figur 2
ein abgewandeltes Ausführungsbeispiel mit arbeitsleistender Entspannung von Gas aus dem unteren Bereich der Niederdrucksäule.
The invention also relates to a device for producing pressurized nitrogen according to claim 5. The invention and further details of the invention are explained in more detail below with reference to exemplary embodiments illustrated in the drawings. Here show:
Figure 1
a first embodiment of the method according to the invention and a corresponding device with work-related relaxation of residual gas from the top condenser of the low pressure column and
Figure 2
a modified embodiment with work-relieving relaxation of gas from the lower region of the low pressure column.

Bei dem Verfahren der Figur 1 wird verdichtete und gereinigte Luft 1 in einem Hauptwärmetauscher 2 abgekühlt und einer Drucksäule 4 unter einem Druck von 8,4 bar zugeleitet (3). Das Rektifiziersystem weist außerdem eine Niederdrucksäule 5 auf, die mit einem Druck von 4,3 bar betrieben wird und mit der Drucksäule über einen gemeinsamen Kondensator-Verdampfer (Hauptkondensator) 6 in wärmetauschender Verbindung steht. Ein Teil 8 des am Kopf der Drucksäule entnommenen Stickstoffs wird im Hauptkondensator 6 verflüssigt und über die Leitungen 9 und 10 als Rücklauf auf die Drucksäule und über 160, 15, 161 auf die Niederdrucksäule 5 aufgegeben. Sumpfflüssigkeit 11 der Drucksäule wird nach Unterkühlung 15 als sauerstoffreiche flüssige Fraktion mindestens teilweise in die Niederdrucksäule 5 eingedrosselt (12). Der Rest der unterkühlten sauerstoffreichen flüssigen Fraktion wird über das Ventil 163 in den Verdampfungsraum des Kopfkondensators 17 der Niederdrucksäule 5 entspannt. Die Sumpfflüssigkeit 13 der Niederdrucksäule 5 wird entspannt (16) und anschließend in den Verdampfungsraum des Kopfkondensators 17 der Niederdrucksäule 5 eingeführt. In dessen Verflüssigungsraum kondensiert gasförmiger Stickstoff 18 vom Kopf der Niederdrucksäule 5; das Kondensat 19 wird zu einem ersten Teil in die Niederdrucksäule zurückgeleitet und dort als Rücklauf verwendet.In the method of FIG. 1 , compressed and cleaned air 1 is cooled in a main heat exchanger 2 and fed to a pressure column 4 under a pressure of 8.4 bar (3). The rectification system also has a low-pressure column 5, which is operated at a pressure of 4.3 bar and is in heat-exchanging connection with the pressure column via a common condenser-evaporator (main condenser) 6. A portion 8 of the nitrogen removed at the top of the pressure column is liquefied in the main condenser 6 and fed via lines 9 and 10 as a return to the pressure column and via 160, 15, 161 to the low pressure column 5. Bottom liquid 11 of the pressure column is at least partially throttled into the low-pressure column 5 after hypothermia 15 as an oxygen-rich liquid fraction (12). The rest of the supercooled oxygen-rich liquid fraction is expanded via the valve 163 into the evaporation space of the top condenser 17 of the low pressure column 5. The bottom liquid 13 of the low-pressure column 5 is expanded (16) and then introduced into the evaporation space of the top condenser 17 of the low-pressure column 5. In its liquefaction space, gaseous nitrogen 18 condenses from the top of the low-pressure column 5; a first part of the condensate 19 is returned to the low-pressure column and used there as a return.

Ein anderer Teil 20 des flüssigen Stickstoffs 19 aus dem Kopfkondensator 17 wird entweder wie in Figur 1 dargestellt aus der Niederdrucksäule entnommen oder direkt aus der Leitung 19 abgezweigt. (Alternativ ist auch eine Entnahme einige Böden unterhalb des Kopfs der Niederdrucksäule 5 möglich). Dieser flüssige Stickstoff 20 wird in flüssigem Zustand auf einen erhöhten Druck (im Beispiel 9 bar) gebracht (Pumpe 21), über Leitung 22 zum Hauptwärmetauscher 2 geführt und dort unter dem erhöhten Druck verdampft und angewärmt. Das warme Stickstoffgas wird schließlich als Druckprodukt 29 abgeführt. Es kann gegebenenfalls in gasförmigem Zustand weiter verdichtet und falls gewünscht mit direkt aus der Drucksäule abgezogenem Druckstickstoff 27, 28 vermischt werden. In dem Beispiel stammen ca. 60 % des gesamten Druckstickstoffprodukts (28+29) aus der Niederdrucksäule 5.Another part 20 of the liquid nitrogen 19 from the top condenser 17 is either as shown in Figure 1 taken from the low pressure column or directly branched off from line 19. (Alternatively, some floors can be removed possible below the head of the low pressure column 5). This liquid nitrogen 20 is brought to an increased pressure (in the example 9 bar) in the liquid state (Pump 21), via line 22 to the main heat exchanger 2 and there under the increased pressure evaporated and warmed. The warm nitrogen gas will eventually dissipated as a printed product 29. It can be in a gaseous state if necessary further compressed and, if desired, with one removed directly from the pressure column Pressure nitrogen 27, 28 are mixed. In the example, approx. 60% of the total pressure nitrogen product (28 + 29) from the low pressure column 5.

Kälte wird hier durch arbeitsleistende Entspannung von Restgas gewonnen, indem mindestens ein Teil 150 des unreinen Sauerstoffs 31 aus dem Kopfkondensator 17 der Niederdrucksäule 5 in einer Entspannungsmaschine 133 von einer Zwischentemperatur des Hauptwärmetauschers 2 aus arbeitsleistend entspannt wird. Das Turbinenabgas 151 wird wieder im Wärmetauscher 2 angewärmt und als Restgas 152 abgeführt beziehungsweise zur Regenerierung einer Vorrichtung für die Reinigung der Einsatzluft verwendet. Die in der Entspannungsmaschine 133 gewonnene mechanische Energie kann an einen Generator abgegeben oder zur Verdichtung einer Prozeßfraktion verwendet werden, vorzugsweise durch direkte mechanische Kopplung der Entspannungsmaschine 133 mit einem nicht dargestellten Verdichter.Cold is obtained here by work-relieving residual gas by at least a portion 150 of the impure oxygen 31 from the overhead condenser 17 the low pressure column 5 in a relaxation machine 133 from one Intermediate temperature of the main heat exchanger 2 is relaxed from work. The turbine exhaust gas 151 is warmed up again in the heat exchanger 2 and as residual gas 152 discharged or for the regeneration of a device for the Purification of the feed air used. The one in the relaxation machine 133 Mechanical energy obtained can be given to a generator or used for Compaction of a process fraction can be used, preferably by direct mechanical coupling of the relaxation machine 133 with a not shown Compressor.

Figur 2 unterscheidet sich dadurch von Figur 1, daß der Einsatz für die Turbine 133 nicht vom Kopfkondensator der Niederdrucksäule, sondern vom Hauptkondensator 6 stammt. Dazu wird sauerstoffhaltiges Gas 31' unmittelbar über dem Sumpf der Niederdrucksäule 5 abgezogen. FIG. 2 differs from FIG. 1 in that the insert for the turbine 133 does not come from the top condenser of the low pressure column, but from the main condenser 6. For this purpose, oxygen-containing gas 31 'is drawn off directly above the bottom of the low-pressure column 5.

Die beiden Säulen 4, 5 können auch nebeneinander angeordnet sein. In diesem Fall würde der Hauptkondensator am Kopf der Drucksäule 4 angeordnet und über eine Flüssig- und eine Dampfleitung mit dem unteren Ende der Niederdrucksäule verbunden.The two columns 4, 5 can also be arranged side by side. In this case the main capacitor would be arranged at the top of the pressure column 4 and via a Liquid and a steam line with the lower end of the low pressure column connected.

Claims (5)

Verfahren zur Gewinnung von Druckstickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem, das eine Drucksäule (4) und eine Niederdrucksäule (5) aufweist, wobei bei dem Verfahren Einsatzluft (1, 3) in einem Hauptwärmetauschersystem (2) abgekühlt und in die Drucksäule (4) eingeleitet wird, eine sauerstoffhaltige flüssige Fraktion (11) aus der Drucksäule (4) entnommen und mindestens zu einem Teil in die Niederdrucksäule (5) eingespeist wird, gasförmiger Stickstoff (18) aus der Niederdrucksäule (5) im Verflüssigungsraum eines Kopfkondensators (17) durch indirekten Wärmeaustausch mit einer im Verdampfungsraum des Kopfkondensators (17) verdampfenden Flüssigkeit (13) mindestens teilweise kondensiert wird und bei dem flüssiger Stickstoff (20) aus dem Verflüssigungsraum des Kopfkondensators (17) oder aus der Niederdrucksäule (5) abgezogen, in flüssigem Zustand auf einen Druck gebracht (21) wird, der den Druck der Niederdrucksäule (5) übersteigt, anschließend verdampft und als gasförmiges Druckstickstoffprodukt (29) abgeführt wird, dadurch gekennzeichnet, daß der flüssig auf Druck gebrachte Stickstoff (22) beim Verdampfen in indirekten Wärmeaustausch (2) mit mindestens einem Teil der Einsatzluft (1) tritt.Process for the production of pressurized nitrogen by low-temperature separation of air in a rectification system, which has a pressure column (4) and a low-pressure column (5), the process cooling feed air (1, 3) in a main heat exchanger system (2) and into the pressure column (4 ) is introduced, an oxygen-containing liquid fraction (11) is removed from the pressure column (4) and at least part of it is fed into the low pressure column (5), gaseous nitrogen (18) from the low pressure column (5) in the liquefaction chamber of a top condenser (17) is condensed at least partially by indirect heat exchange with a liquid (13) evaporating in the evaporation space of the top condenser (17) and in which liquid nitrogen (20) is drawn off from the liquefaction space of the top condenser (17) or from the low pressure column (5) a pressure is brought (21), which exceeds the pressure of the low pressure column (5), then end vaporized and removed as gaseous pressurized nitrogen product (29), characterized in that the liquid brought to pressure nitrogen (22) occurs upon evaporation in indirect heat exchange (2) with at least a portion of the feed air (1). Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß aus der Drucksäule (4) ein gasförmiger Stickstoffstrom (27) entnommen und als weiteres gasförmiges Stickstoffprodukt (28) gewonnen wird.Method according to claim 1, characterized in that a gaseous nitrogen stream (27) is removed from the pressure column (4) and is obtained as a further gaseous nitrogen product (28). Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß ein sauerstoffhaltiger Strom (31, 31') aus dem Verdampfungsraum des Kopfkondensators (17) und/oder aus einem unteren Bereich der Niederdrucksäule (5) arbeitsleistend entspannt (133) wird.Method according to Claim 1 or 2, characterized in that an oxygen-containing stream (31, 31 ') from the evaporation space of the top condenser (17) and / or from a lower region of the low-pressure column (5) is expanded (133) while performing work. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß ein weiterer Teil der sauerstoffhaltigen flüssigen Fraktion (11, 163) aus der Drucksäule (4) und/oder eine flüssige Fraktion (13) aus der Niederdrucksäule (5) in den Verdampfungsraum des Kopfkondensators (17) wird. Method according to one of claims 1 to 3, characterized in that a further part of the oxygen-containing liquid fraction (11, 163) from the pressure column (4) and / or a liquid fraction (13) from the low pressure column (5) into the evaporation chamber of the Head capacitor (17). Vorrichtung zur Gewinnung von Druckstickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem, das eine Drucksäule (4) und eine Niederdrucksäule (5) aufweist, mit einer Einsatzluftleitung (1, 3), die durch einen Hauptwärmetauschersystem (2) in die Drucksäule (4) führt, mit einer Leitung (11) für eine sauerstoffhaltige flüssige Fraktion, die von der Drucksäule (4) in die Niederdrucksäule (5) führt, mit einem Kopfkondensator (17), dessen Verflüssigungsraum mit einem oberen Bereich der Niederdrucksäule (5) verbunden (18) ist, mit einer Flüssigstickstoffleitung (20, 22), die vom Verflüssigungsraum des Kopfkondensators (17) der Niederdrucksäule (5) oder von einem oberen Bereich der Niederdrucksäule (5) über Mittel (21) zur Druckerhöhung einer Flüssigkeit zum Hauptwärmetauschersystem (2) führt und in Strömungsverbindung mit einer Druckproduktleitung (29) steht.Device for the production of pressurized nitrogen by cryogenic decomposition of air in a rectification system comprising a pressure column (4) and a Low pressure column (5), with a feed air line (1, 3) through a Main heat exchanger system (2) in the pressure column (4) leads with a line (11) for an oxygen-containing liquid fraction, which from the pressure column (4) in the Low pressure column (5) leads, with a top condenser (17), the Liquefaction room with an upper area of the low pressure column (5) is connected (18), with a liquid nitrogen line (20, 22) which from Liquefaction space of the top condenser (17) of the low pressure column (5) or from an upper region of the low pressure column (5) via means (21) for Pressure increase of a liquid leads to the main heat exchanger system (2) and in Flow connection with a pressure product line (29) is.
EP01108734A 2000-04-12 2001-04-06 Process and apparatus for the production of high pressure nitrogen from air separation Withdrawn EP1146301A1 (en)

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