EP1209431B1 - Process and apparatus for the production of nitrogen and oxygen - Google Patents

Process and apparatus for the production of nitrogen and oxygen Download PDF

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Publication number
EP1209431B1
EP1209431B1 EP01127958A EP01127958A EP1209431B1 EP 1209431 B1 EP1209431 B1 EP 1209431B1 EP 01127958 A EP01127958 A EP 01127958A EP 01127958 A EP01127958 A EP 01127958A EP 1209431 B1 EP1209431 B1 EP 1209431B1
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Prior art keywords
pressure column
low
nitrogen
liquid
oxygen
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EP01127958A
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German (de)
French (fr)
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EP1209431A1 (en
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Herbert Schoenecker
Jürgen Voit
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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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
    • F25J3/04224—Cores associated with a liquefaction or refrigeration cycle
    • 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
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
    • 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
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
    • 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
    • F25J2200/50—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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • 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
    • 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
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen

Definitions

  • the invention relates to a process for the production of oxygen and nitrogen Cryogenic air separation according to the preamble of patent claim 1.
  • the invention has for its object a method of the type mentioned and specify a corresponding device that is particularly economical work.
  • the cooling liquid is in contrast to the invention by a Liquid formed, the composition of the bottom liquid of the pressure column equivalent.
  • the composition of the cooling fluid can be so be chosen that the product yield, especially the oxygen yield is increased.
  • the intermediate liquid, which is used as cooling fluid in the top condenser, from an intermediate point is subtracted, for example 10 to 20 theoretical floors above the point is where the oxygen-containing liquid fraction from the pressure column in the Low pressure column is fed.
  • the process can use liquid nitrogen from or from the low pressure column Top condenser removed and discharged as a liquid nitrogen product.
  • the process preferably has a nitrogen cycle on.
  • cycle nitrogen becomes gaseous from the upper area of the pressure column withdrawn and compressed in a circuit compressor, a first partial flow of compressed cycle nitrogen is relieved of work and a second Partial stream of the compressed cycle nitrogen liquefied and into the rectification system fed back and / or taken as a further liquid nitrogen product.
  • On such a cycle can also be carried out without oxygen production, for example with Use of the bottom liquid from low pressure column or pressure column as cooling fluid in the top condenser of the low pressure column.
  • the liquefied circulating nitrogen can be one of the Columns of the rectification system are fed, preferably the pressure column. The the corresponding amount can then be a liquid nitrogen and / or oxygen product be withdrawn from the rectification system.
  • Top nitrogen from the pressure column is liquefied in a main condenser. That included generated condensate is at least partly, preferably largely, as Return to the pressure column abandoned. Another part of the condensate can be on top introduced into the low pressure column and / or immediately as a liquid nitrogen product subtracted from.
  • the circuit can be designed as a two or more turbine system by one third partial stream of compressed cycle nitrogen independent of the first Partial stream is relaxed while working.
  • the invention also relates to a device according to claim 8 or 9.
  • An oxygen-containing liquid fraction (8) from the bottom of the pressure column is in one Cooled subcooler 9 and via line 10 at an intermediate point in the , Low pressure column 5 initiated.
  • gaseous top nitrogen is converted into a first part 11 in Main condenser 6 at least partially, preferably completely liquefied.
  • the the condensate 12 produced thereby becomes a first part 13 as a return flow onto the head the pressure column 4 abandoned.
  • a second part 14 of the main capacitor 6 condensed nitrogen 11 is introduced into the low pressure column.
  • Liquid nitrogen 19 is drawn off at the top of the low-pressure column and after Separation of flash gas in a separator 20 via line 21 as a liquid Withdrawn nitrogen product and introduced a tank 22.
  • the flash gas 23 is the Residual gas 16 admixed.
  • the residual mixture 24 is in the subcoolers 25, 9 and Main heat exchanger 2 warmed up and finally via line 27 into the atmosphere blown off and / or as a regeneration gas for the device, not shown Purification of the feed air used.
  • a second partial stream of the compressed cycle nitrogen is passed through line 42 two series-connected post-compressors 43, 45, each of which has an after-cooler 44, 46 follows.
  • the second partial flow continues to the first circuit heat exchanger 37 (Line 47), is further cooled in the second circuit heat exchanger 40 and finally liquefied or - in the third circuit heat exchanger 48 supercritical pressure - pseudo-liquefied.
  • a third partial flow of the compressed cycle nitrogen is combined with the second partial flow through the post-compressors 43, 45 and the first and second Circuit heat exchanger 37, 40 out.
  • the third substream 56 becomes one cold turbine 57 led.
  • the work-relieved, relaxed third partial flow overflows Line 58 through the three circuit heat exchangers 48, 40, 37 to the entry of the Circuit compressor back.
  • the cold parts of the system are in an insulating housing (cold box) 64 arranged.

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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)
  • Catalysts (AREA)

Abstract

Oxygen and nitrogen are produced by using a low temperature air decomposition process in a rectification system having a high pressure column (4) and a low pressure column (5). Process air (1, 3) is fed into the high pressure column, an oxygen-containing liquid fraction (8, 10) is removed from the high pressure column and injected into the low pressure column, and gaseous nitrogen (17) from the low pressure column is partially condensed by indirect heat exchange with a vaporizing coolant. A nitrogen product stream (19) is removed from the high pressure column and the low pressure column and an oxygen product stream (61, 62, 63) is removed as liquid and gas from the low pressure column. The coolant for the head condenser (7) of the low pressure column is formed by an intermediate liquid (15) removed from an intermediate site of the low pressure column. An Independent claim is also included for a device for the low temperature air decomposition. Preferred Features: The intermediate liquid is removed from an intermediate site which lies above the site at which the oxygen-containing liquid fraction from the high pressure column is injected into the low pressure column. Liquid nitrogen is removed from the low pressure column or its head condenser as a liquid nitrogen product.

Description

Die Erfindung betrifft ein Verfahren zur Erzeugung von Sauerstoff und Stickstoff durch Tieftemperaturzerlegung von Luft gemäß dem Oberbegriff des Patentanspruchs 1.The invention relates to a process for the production of oxygen and nitrogen Cryogenic air separation according to the preamble of patent claim 1.

Verfahren mit Kopfkühlung der Niederdrucksäule sind aus EP 1022530 A1, EP 811816 A2 oder EP 955509 A1 bekannt. Prozesse der eingangs genannten Art sind in WO 9819122 und US 5137559 gezeigt.Methods with head cooling of the low pressure column are from EP 1022530 A1, EP 811816 A2 or EP 955509 A1 known. Processes of the type mentioned are in WO 9819122 and US 5137559 are shown.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art und eine entsprechende Vorrichtung anzugeben, die wirtschaftlich besonders günstig arbeiten.The invention has for its object a method of the type mentioned and specify a corresponding device that is particularly economical work.

Diese Aufgabe wird durch die Merkmale des Patentanspruch 1 gelöst.This object is solved by the features of claim 1.

Bei WO 9819122 wird die Kühlflüssigkeit im Gegensatz zur Erfindung durch eine Flüssigkeit gebildet, deren Zusammensetzung der Sumpfflüssigkeit der Drucksäule entspricht. Bei der Erfindung kann dagegen die Zusammensetzung des Kühlfluids so gewählt werden, dass die Produktausbeute, insbesondere die Sauerstoffausbeute erhöht wird.In WO 9819122 the cooling liquid is in contrast to the invention by a Liquid formed, the composition of the bottom liquid of the pressure column equivalent. In contrast, in the invention the composition of the cooling fluid can be so be chosen that the product yield, especially the oxygen yield is increased.

Zur Optimierung der Sauerstoffausbeute ist es günstig, wenn die Zwischenflüssigkeit, die als Kühlfluid im Kopfkondensator eingesetzt wird, von einer Zwischenstelle abgezogen wird, die beispielsweise 10 bis 20 theoretische Böden oberhalb der Stelle liegt, an der die sauerstoffhaltige flüssige Fraktion aus der Drucksäule in die Niederdrucksäule eingespeist wird.To optimize the oxygen yield, it is advantageous if the intermediate liquid, which is used as cooling fluid in the top condenser, from an intermediate point is subtracted, for example 10 to 20 theoretical floors above the point is where the oxygen-containing liquid fraction from the pressure column in the Low pressure column is fed.

Bei dem Verfahren kann flüssiger Stickstoff aus der Niederdrucksäule oder aus deren Kopfkondensator abgezogen und als flüssiges Stickstoffprodukt abgeführt werden. Insbesondere in diesem Fall weist der Prozess vorzugsweise einen Stickstoff-Kreislauf auf. Dabei wird Kreislauf-Stickstoff gasförmig aus dem oberen Bereich der Drucksäule abgezogen und in einem Kreislauf-Verdichter verdichtet, wobei ein erster Teilstrom des verdichteten Kreislauf-Stickstoffs arbeitsleistend entspannt wird und ein zweiter Teilstrom des verdichteten Kreislauf-Stickstoffs verflüssigt und in das Rektifiziersystem zurückgespeist und/oder als weiteres flüssiges Stickstoffprodukt entnommen wird. Ein derartiger Kreislauf kann auch ohne Sauerstoffproduktion, beispielsweise mit Verwendung der Sumpfflüssigkeit von Niederdrucksäule oder Drucksäule als Kühlfluid im Kopfkondensator der Niederdrucksäule, eingesetzt werden.The process can use liquid nitrogen from or from the low pressure column Top condenser removed and discharged as a liquid nitrogen product. In this case in particular, the process preferably has a nitrogen cycle on. Here, cycle nitrogen becomes gaseous from the upper area of the pressure column withdrawn and compressed in a circuit compressor, a first partial flow of compressed cycle nitrogen is relieved of work and a second Partial stream of the compressed cycle nitrogen liquefied and into the rectification system fed back and / or taken as a further liquid nitrogen product. On such a cycle can also be carried out without oxygen production, for example with Use of the bottom liquid from low pressure column or pressure column as cooling fluid in the top condenser of the low pressure column.

Durch die arbeitsleistende Entspannung des ersten Teilstroms des Kreislauf-Stickstoffs wird Kälte erzeugt, die über den verflüssigten zweiten Teilstrom weitertransportiert und zur Erhöhung der Flüssigproduktion eingesetzt werden kann. Die Flüssigkeit aus dem Kreislauf kann beispielsweise direkt als flüssiges Stickstoff-Produkt abgezogen werden. Altemativ oder zusätzlich kann der verflüssigte Kreislauf-Stickstoff einer der Säulen des Rektifiziersystems zugespeist werden, vorzugsweise der Drucksäule. Die entsprechende Menge kann dann als flüssiges Stickstoff- und/oder Sauerstoff-Produkt aus dem Rektifiziersystem abgezogen werden.Due to the relaxation of the first partial stream of circulating nitrogen refrigeration is generated, which is transported further via the liquefied second partial stream and can be used to increase liquid production. The liquid from the The cycle can be drawn off directly as a liquid nitrogen product, for example become. Alternatively or additionally, the liquefied circulating nitrogen can be one of the Columns of the rectification system are fed, preferably the pressure column. The the corresponding amount can then be a liquid nitrogen and / or oxygen product be withdrawn from the rectification system.

Kopfstickstoff der Drucksäule wird in einem Hauptkondensator verflüssigt. Das dabei erzeugte Kondensat wird mindestens zum Teil, vorzugsweise zum größten Teil, als Rücklauf auf die Drucksäule aufgegeben. Ein weiterer Teil des Kondensats kann oben in die Niederdrucksäule eingeleitet und/oder unmittelbar als flüssiges Stickstoffprodukt abgezogen werden. Top nitrogen from the pressure column is liquefied in a main condenser. That included generated condensate is at least partly, preferably largely, as Return to the pressure column abandoned. Another part of the condensate can be on top introduced into the low pressure column and / or immediately as a liquid nitrogen product subtracted from.

Der Kreislauf kann als Zwei- oder Mehr-Turbinen-System ausgeführt sein, indem ein dritter Teilstrom des verdichteten Kreislauf-Stickstoffs unabhängig vom ersten Teilstrom arbeitsleistend entspannt wird.The circuit can be designed as a two or more turbine system by one third partial stream of compressed cycle nitrogen independent of the first Partial stream is relaxed while working.

Die Erfindung betrifft außerdem eine Vorrichtung gemäß Patentanspruch 8 beziehungsweise 9.The invention also relates to a device according to claim 8 or 9.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand eines in der Zeichnung dargestellten Ausführungsbeispiels näher erläutert.The invention and further details of the invention are described below of an embodiment shown in the drawing.

Verdichtete und gereinigte Einsatzluft strömt über Leitung 1 in einen Hauptwärmetauscher 2 und wird dort auf etwa Taupunkt abgekühlt. Über Leitung 3 wird die kalte Luft der Drucksäule 4 des Rektifiziersystems zugeführt, das aus der Drucksäule 4, der Niederdrucksäule 5, dem Hauptkondensator 6 und dem Kopfkondensator 7 besteht.Compressed and cleaned feed air flows into a via line 1 Main heat exchanger 2 and is cooled there to about dew point. Via line 3 the cold air is fed to the pressure column 4 of the rectification system, which from the Pressure column 4, the low pressure column 5, the main condenser 6 and the Head capacitor 7 exists.

Eine sauerstoffhaltige flüssige Fraktion (8) vom Sumpf der Drucksäule wird in einem Unterkühler 9 abgekühlt und über Leitung 10 an einer Zwischenstelle in die ,Niederdrucksäule 5 eingeleitet.An oxygen-containing liquid fraction (8) from the bottom of the pressure column is in one Cooled subcooler 9 and via line 10 at an intermediate point in the , Low pressure column 5 initiated.

Am Kopf der Drucksäule 4 wird gasförmiger Kopfstickstoff zu einem ersten Teil 11 im Hauptkondensator 6 mindestens teilweise, vorzugsweise vollständig verflüssigt. Das dabei erzeugte Kondensat 12 wird zu einem ersten Teil 13 als Rücklauf auf den Kopf der Drucksäule 4 aufgegeben. Ein zweiter Teil 14 des im Hauptkondensator 6 kondensierten Stickstoffs 11 wird in die Niederdrucksäule eingeleitet.At the top of the pressure column 4, gaseous top nitrogen is converted into a first part 11 in Main condenser 6 at least partially, preferably completely liquefied. The the condensate 12 produced thereby becomes a first part 13 as a return flow onto the head the pressure column 4 abandoned. A second part 14 of the main capacitor 6 condensed nitrogen 11 is introduced into the low pressure column.

Vom Sumpf der Niederdrucksäule, der gleichzeitig den Verdampfungsraum des Hauptkondensators 6 darstellt, wird ein flüssiger Sauerstoff-Produktstrom 61 abgezogen. Eine Restmenge 62 Sauerstoffs wird dem unteren Teil der Niederdrucksäule gasförmig entnommen, im Hauptwärmetauscher 2 angewärmt und schließlich über Leitung 63 in Richtung des Verbrauchers abgegeben. In dem Beispiel erfolgt der Produkt-Abzug aus der Säule hauptsächlich in Flüssigform; alternativ oder zusätzlich könnte der Sauerstoff-Produktstrom gasförmig aus der Säule herausgeführt werden. Bei Flüssigabzug ist anschließend ist eine Nutzung als Flüssigprodukt - gegebenenfalls nach Unterkühlung - und/oder eine Verdampfung - beispielsweise unter erhöhtem Druck - möglich. Eine derartige Verdampfung kann durch indirekten (Nebenkondensator oder Innenverdichtung) oder direkten Wärmeaustausch (Mischsäule) durchgeführt werden.From the sump of the low pressure column, which also the evaporation chamber of the Represents main condenser 6, becomes a liquid oxygen product stream 61 deducted. A residual amount of 62 oxygen is added to the lower part of the Low pressure column removed in gaseous form, warmed in the main heat exchanger 2 and finally delivered via line 63 towards the consumer. In the example the product is withdrawn from the column mainly in liquid form; alternatively or in addition, the oxygen product stream could be led out of the column in gaseous form become. In the case of liquid discharge, use as a liquid product is then - optionally after hypothermia - and / or evaporation - for example under increased pressure - possible. Such evaporation can be done by indirect (Secondary condenser or internal compression) or direct heat exchange (Mixing column).

Von einer Zwischenstelle der Niederdrucksäule 5, die in dem Beispiel zwölf praktische oder neun theoretische Böden oberhalb der Zuspeisung der Drucksäulen-Sumpfflüssigkeit 10 liegt, wird ein Kühlfluid 15 in flüssiger Form abgezogen, unterkühlt (25) und in den Verdampfungsraum des Kopfkondensators 7 der Niederdrucksäule geführt. Dort verdampft es bis auf eine kleine Spülmenge 60 vollständig und wird schließlich über Leitung 16 als Restgas abgezogen. Im Verflüssigungsraum des Kopfkondensators 7 wird gasförmiger Stickstoff 17 vom Kopf der Niederdrucksäule mindestens teilweise, vorzugsweise vollständig verflüssigt und über Leitung 18 in die Niederdrucksäule 5 zurückgespeist.From an intermediate point of the low pressure column 5, which is practical in the example twelve or nine theoretical plates above the supply of the pressure column bottom liquid 10, a cooling fluid 15 is drawn off in liquid form, supercooled (25) and in the evaporation space of the top condenser 7 of the low pressure column guided. There it evaporates completely except for a small flush volume 60 and becomes finally withdrawn via line 16 as residual gas. In the liquefaction room of the Top condenser 7 becomes gaseous nitrogen 17 from the top of the low pressure column at least partially, preferably completely liquefied and via line 18 in the Low pressure column 5 fed back.

Am Kopf der Niederdrucksäule wird flüssiger Stickstoff 19 abgezogen und nach Abtrennung von Flashgas in einem Abscheider 20 über Leitung 21 als flüssiges Stickstoffprodukt abgezogen und einen Tank 22 eingeleitet. Das Flashgas 23 wird dem Restgas 16 zugemischt. Das Restgemisch 24 wird in den Unterkühlem 25, 9 und im Hauptwärmetauscher 2 angewärmt und schließlich über Leitung 27 in die Atmosphäre abgeblasen und/oder als Regeneriergas für die nicht dargestellte Vorrichtung zur Reinigung der Einsatzluft verwendet.Liquid nitrogen 19 is drawn off at the top of the low-pressure column and after Separation of flash gas in a separator 20 via line 21 as a liquid Withdrawn nitrogen product and introduced a tank 22. The flash gas 23 is the Residual gas 16 admixed. The residual mixture 24 is in the subcoolers 25, 9 and Main heat exchanger 2 warmed up and finally via line 27 into the atmosphere blown off and / or as a regeneration gas for the device, not shown Purification of the feed air used.

Vom Kopf der Drucksäule wird über Leitung 28 Kreislauf-Stickstoff entnommen, zum Hauptwärmetauscher 2 geführt (29), dort auf etwa Umgebungstemperatur angewärmt und über die Leitungen 30, 31, 32 zum Eintritt eines Kreislauf-Verdichters 33 geführt. (Dieser Drucksäulen-Stickstoff 28 stellt vorzugsweise die einzige Zufuhr zum Stickstoff-Kreislauf dar; auf einen Feedgas-Verdichter zum Einführen von Niederdruck-Stickstoff in den Kreislauf kann somit verzichtet werden.) Stromabwärts eines Nachkühlers 34 wird ein erster Teilstrom 36 des verdichteten Kreislauf-Stickstoffs 35 abgetrennt, in einem ersten Kreislauf-Wärmetauscher 37 auf eine erste Zwischentemperatur abgekühlt und in einer warmen Turbine 38 arbeitsleistend entspannt. Das Abgas 39 der warmen Turbine 38 wird in einem zweiten Kreislauf-Wärmetauscher 40 und im ersten Kreislauf-Wärmetauscher 37 wieder angewärmt und zum Kreislaufverdichter 33 zurückgeführt (Leitungen 41, 32). From the top of the pressure column 28 cycle nitrogen is removed via line Main heat exchanger 2 out (29), warmed up to about ambient temperature and led via the lines 30, 31, 32 to the entry of a circuit compressor 33. (This pressure column nitrogen 28 is preferably the only supply to the nitrogen cycle group; to a feed gas compressor for introducing low pressure nitrogen the circuit can therefore be dispensed with.) Downstream of an aftercooler 34 a first partial stream 36 of the compressed cycle nitrogen 35 is separated, in a first circuit heat exchanger 37 to a first intermediate temperature cooled and relaxed in a warm turbine 38 to perform work. The exhaust 39 the warm turbine 38 is in a second circuit heat exchanger 40 and the first circuit heat exchanger 37 warmed up again and to the circuit compressor 33 returned (lines 41, 32).

Über Leitung 42 wird ein zweiter Teilstrom des verdichteten Kreislauf-Stickstoffs durch zwei seriell geschaltete Nachverdichter 43, 45 geführt, denen jeweils ein Nachkühler 44, 46 folgt. Der zweite Teilstrom fließt weiter zum ersten Kreislauf-Wärmetauscher 37 (Leitung 47), wird im zweiten Kreislauf-Wärmetauscher 40 weiter abgekühlt und schließlich im dritten Kreislauf-Wärmetauscher 48 verflüssigt beziehungsweise - bei überkritischem Druck - pseudo-verflüssigt. Nach Entspannung auf etwa Drucksäulen-Druck in einem Drosselventil 49 wird der verflüssigte zweite Teilstrom 50, 52 - nach Abtrennung gasförmiger Bestandteile in einem Abscheider 51 - in die Drucksäule 4 eingeführt (52). Flashgas 53 aus dem Abscheider 51 wird über die Leitungen 54 und/oder 55 zum Kreislauf-Verdichter 33 zurückgeführt.A second partial stream of the compressed cycle nitrogen is passed through line 42 two series-connected post-compressors 43, 45, each of which has an after-cooler 44, 46 follows. The second partial flow continues to the first circuit heat exchanger 37 (Line 47), is further cooled in the second circuit heat exchanger 40 and finally liquefied or - in the third circuit heat exchanger 48 supercritical pressure - pseudo-liquefied. After relaxation to pressure column pressure in a throttle valve 49, the liquefied second partial flow 50, 52 - after Separation of gaseous components in a separator 51 - into the pressure column 4 introduced (52). Flash gas 53 from the separator 51 is sent via the lines 54 and / or 55 returned to the circuit compressor 33.

Ein dritter Teilstrom des verdichteten Kreislauf-Stickstoffs wird gemeinsam mit dem zweiten Teilstrom durch die Nachverdichter 43, 45 und den ersten und zweiten Kreislauf-Wärmetauscher 37, 40 geführt. Bei einer zweiten Zwischentemperatur, die niedriger als die erste Zwischentemperatur ist, wird der dritte Teilstrom 56 zu einer kalten Turbine 57 geführt. Der arbeitsleistend entspannte dritte Teilstrom strömt über Leitung 58 durch die drei Kreislauf-Wärmetauscher 48, 40, 37 zum Eintritt des Kreislauf-Verdichters zurück.A third partial flow of the compressed cycle nitrogen is combined with the second partial flow through the post-compressors 43, 45 and the first and second Circuit heat exchanger 37, 40 out. At a second intermediate temperature, the is lower than the first intermediate temperature, the third substream 56 becomes one cold turbine 57 led. The work-relieved, relaxed third partial flow overflows Line 58 through the three circuit heat exchangers 48, 40, 37 to the entry of the Circuit compressor back.

Die kalten Teile der Anlage sind in einem isolierenden Gehäuse (Coldbox) 64 angeordnet.The cold parts of the system are in an insulating housing (cold box) 64 arranged.

Claims (7)

  1. Process for producing oxygen and nitrogen by low-temperature fractionation of air in a rectification system which has a pressure column (4) and a low-pressure column (5), in which process feed air (1, 3) is introduced into the pressure column (4), an oxygen-containing liquid fraction (8, 10) is removed from the pressure column (4) and fed into the low-pressure column (5), gaseous nitrogen (17) from the low-pressure column (5) is at least partially condensed in a top condenser (7) by indirect heat exchange with an evaporating cooling fluid (15), a nitrogen product stream (19) is removed from the low-pressure column (5) and an oxygen product stream (61, 62, 63) is discharged in liquid and/or gas form from the low-pressure column (5), the cooling fluid for the top condenser (7) of the low-pressure column (5) being formed by an intermediate liquid (15) which is extracted from an intermediate location in the low-pressure column (5), characterized in that the intermediate liquid (15) is extracted from an intermediate location which is located above the location at which the oxygen-containing liquid fraction (8, 10) from the pressure column (4) is fed into the low-pressure column (5) and below the location at which the nitrogen product stream (19) is removed.
  2. Process according to Claim 1, characterized in that liquid nitrogen (19) is extracted from the low-pressure column (5) or from its top condenser (7) and is discharged as liquid nitrogen product (22).
  3. Process according to Claim 1 or 2, characterized in that cycle nitrogen (28, 29, 30, 31, 32) is extracted in gas form from the upper region of the pressure column (4) and is compressed in a cycle compressor (33), a first part-stream (36) of the compressed cycle nitrogen (35) being expanded in a work-performing manner (38), and a second part-stream (42, 47, 50) of the compressed cycle nitrogen (35) being liquefied and fed back (52) into the rectification system and/or removed as further liquid nitrogen product.
  4. Process according to any of Claims 1 to 3, characterized in that top nitrogen (11) from the pressure column (4) is liquefied in a main condenser (6).
  5. Process according to Claim 4, characterized in that the condensate (12) which is formed in the main condenser is at least in part (14) introduced into the low-pressure column.
  6. Process according to Claim 4 or 5, characterized in that the condensate (12) formed in the main condenser is at least in part extracted as liquid nitrogen product (22).
  7. Apparatus for producing oxygen and nitrogen by low-temperature fractionation of air, having a rectification system which includes a pressure column (4) and a low-pressure column (5), having a feed line (1, 3) for introducing feed air into the pressure column (4), having a liquid line (8, 10) for transferring an oxygen-containing liquid fraction from the pressure column (4) into the low-pressure column (5), a top condenser (7), the liquefaction space of which is connected (17, 18) to the upper region of the low-pressure column (5) and the evaporation space of which is connected to a coolant line (15) for introducing a cooling fluid, having a nitrogen product line (19), which is connected to the low-pressure column (5), and having an oxygen product line (61, 62, 63), which is connected to the low-pressure column (5), the coolant line (15) being connected to an intermediate location of the low-pressure column (5), characterized in that the intermediate location at which the coolant line (15) is connected to the low-pressure column (5) is located above the location at which the liquid line (8, 10) for transferring an oxygen-containing liquid fraction out of the pressure column (4) opens out into the low-pressure column (5) and below the location at which the nitrogen product line (19) is connected to the low-pressure column (5).
EP01127958A 2000-11-24 2001-11-23 Process and apparatus for the production of nitrogen and oxygen Expired - Lifetime EP1209431B1 (en)

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DE10058332A DE10058332A1 (en) 2000-11-24 2000-11-24 Method and device for generating oxygen and nitrogen
DE10058332 2000-11-24

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US20150168057A1 (en) * 2013-12-17 2015-06-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for producing liquid nitrogen
US20150168058A1 (en) * 2013-12-17 2015-06-18 L'air Liquide, Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Apparatus for producing liquid nitrogen
CN109676367A (en) * 2018-12-28 2019-04-26 乔治洛德方法研究和开发液化空气有限公司 A kind of method of heat exchanger assemblies and the assembly heat exchanger assemblies

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US4439220A (en) * 1982-12-02 1984-03-27 Union Carbide Corporation Dual column high pressure nitrogen process
US4832719A (en) 1987-06-02 1989-05-23 Erickson Donald C Enhanced argon recovery from intermediate linboil
US5006139A (en) * 1990-03-09 1991-04-09 Air Products And Chemicals, Inc. Cryogenic air separation process for the production of nitrogen
US5137559A (en) * 1990-08-06 1992-08-11 Air Products And Chemicals, Inc. Production of nitrogen free of light impurities
US5697229A (en) * 1996-08-07 1997-12-16 Air Products And Chemicals, Inc. Process to produce nitrogen using a double column plus an auxiliary low pressure separation zone
US5682762A (en) * 1996-10-01 1997-11-04 Air Products And Chemicals, Inc. Process to produce high pressure nitrogen using a high pressure column and one or more lower pressure columns
DE19735154A1 (en) * 1996-10-30 1998-05-07 Linde Ag Producing compressed nitrogen@ by low temperature distillation of air in rectifier system
EP0955509B1 (en) * 1998-04-30 2004-12-22 Linde Aktiengesellschaft Process and apparatus to produce high purity nitrogen
DE19902255A1 (en) 1999-01-21 2000-07-27 Linde Tech Gase Gmbh Process and device for the production of pressurized nitrogen

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ATE268893T1 (en) 2004-06-15
EP1209431A1 (en) 2002-05-29
DE50102525D1 (en) 2004-07-15
US20020062658A1 (en) 2002-05-30
US6490884B2 (en) 2002-12-10

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