EP1209431A1 - 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
EP1209431A1
EP1209431A1 EP01127958A EP01127958A EP1209431A1 EP 1209431 A1 EP1209431 A1 EP 1209431A1 EP 01127958 A EP01127958 A EP 01127958A EP 01127958 A EP01127958 A EP 01127958A EP 1209431 A1 EP1209431 A1 EP 1209431A1
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European Patent Office
Prior art keywords
pressure column
low pressure
nitrogen
oxygen
liquid
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EP01127958A
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German (de)
French (fr)
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EP1209431B1 (en
Inventor
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 in a rectification system that includes a pressure column and has a low pressure column, with the process feed air into the pressure column initiated, an oxygen-containing liquid fraction removed from the pressure column and is fed into the low pressure column, gaseous nitrogen from the Low pressure column in a top condenser by indirect heat exchange with an evaporating cooling fluid is at least partially condensed Low pressure column and / or a nitrogen product stream removed from the pressure column and an oxygen product stream is discharged from the low pressure column.
  • EP 1022530 A1 Methods with head cooling of the low pressure column are known from EP 1022530 A1, WO 9819122 or EP 811816 A2 known.
  • a process of the type mentioned at the outset is shown in EP 955509 A1.
  • the invention has for its object a method of the type mentioned and specify a corresponding device that is particularly economical work.
  • cooling fluid for the top condenser Low pressure column is formed by an intermediate liquid, which is from a Intermediate point of the low pressure column is withdrawn.
  • this cooling liquid is caused by the bottom liquid Pressure column formed.
  • the invention has two advantages.
  • the composition of the cooling fluid can be chosen so that the Product yield, in particular the oxygen yield is increased.
  • the cooling fluid has a lower pressure so that it is before it is introduced into the Head capacitor only has to be throttled relatively slightly; corresponding the flash gas losses are lower.
  • the intermediate liquid, which is used as cooling fluid in the top condenser, from an intermediate point is subtracted, which is above the point at which the oxygen-containing liquid Fraction from the pressure column is fed into the low pressure column. Between there are, for example, 10 to 20 theoretical floors.
  • 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.
  • 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 partially, 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 and on 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 Circuit compressor back.
  • the cold parts of the system are in an insulating housing (cold box) 64 arranged.
  • the bottom liquid 8, 10 from the pressure column 4th also be introduced into the low pressure column 5 directly above the sump, the simultaneously represents the evaporation space of the main condenser 6.
  • the cooling fluid 15 for the top condenser 7 either from the bottom of the Low pressure column withdrawn or directly from the pressure column sump liquid 10 are branched off.

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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 in einem Rektifiziersystem, das eine Drucksäule und eine Niederdrucksäule aufweist, wobei bei dem Verfahren Einsatzluft in die Drucksäule eingeleitet, eine sauerstoffhaltige flüssige Fraktion aus der Drucksäule entnommen und in die Niederdrucksäule eingespeist wird, gasförmiger Stickstoff aus der Niederdrucksäule in einem Kopfkondensator durch indirekten Wärmeaustausch mit einem verdampfenden Kühlfluid mindestens teilweise kondensiert wird, der Niederdrucksäule und/oder der Drucksäule ein Stickstoff-Produktstrom entnommen und aus der Niederdrucksäule ein Sauerstoff-Produktstrom abgeführt wird.The invention relates to a process for the production of oxygen and nitrogen Cryogenic air separation in a rectification system that includes a pressure column and has a low pressure column, with the process feed air into the pressure column initiated, an oxygen-containing liquid fraction removed from the pressure column and is fed into the low pressure column, gaseous nitrogen from the Low pressure column in a top condenser by indirect heat exchange with an evaporating cooling fluid is at least partially condensed Low pressure column and / or a nitrogen product stream removed from the pressure column and an oxygen product stream is discharged from the low pressure column.

Verfahren mit Kopfkühlung der Niederdrucksäule sind aus EP 1022530 A1,
WO 9819122 oder EP 811816 A2 bekannt. Ein Prozess der eingangs genannten Art ist in EP 955509 A1 gezeigt.Methods with head cooling of the low pressure column are known from EP 1022530 A1,
WO 9819122 or EP 811816 A2 known. A process of the type mentioned at the outset is shown in EP 955509 A1.

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 dadurch gelöst, dass das Kühlfluid für den Kopfkondensator der Niederdrucksäule durch eine Zwischenflüssigkeit gebildet wird, die von einer Zwischenstelle der Niederdrucksäule abgezogen wird.This object is achieved in that the cooling fluid for the top condenser Low pressure column is formed by an intermediate liquid, which is from a Intermediate point of the low pressure column is withdrawn.

Bei EP 955509 A1 wird diese Kühlflüssigkeit dagegen durch die Sumpfflüssigkeit der Drucksäule gebildet. Im Vergleich hierzu weist die Erfindung zwei Vorteile auf. Zum einen kann die Zusammensetzung des Kühlfluids so gewählt werden, dass die Produktausbeute, insbesondere die Sauerstoffausbeute erhöht wird. Zum anderen weist das Kühlfluid einen niedrigeren Druck auf, sodass es vor seiner Einleitung in den Kopfkondensator nur relativ geringfügig abgedrosselt werden muss; entsprechend geringer sind die Flashgas-Verluste. In EP 955509 A1, on the other hand, this cooling liquid is caused by the bottom liquid Pressure column formed. In comparison, the invention has two advantages. To the On the one hand, the composition of the cooling fluid can be chosen so that the Product yield, in particular the oxygen yield is increased. On the other hand the cooling fluid has a lower pressure so that it is before it is introduced into the Head capacitor only has to be throttled relatively slightly; corresponding the flash gas losses are lower.

Zur Optimierung der Sauerstoffausbeute ist es günstig, wenn die Zwischenflüssigkeit, die als Kühlfluid im Kopfkondensator eingesetzt wird, von einer Zwischenstelle abgezogen wird, die oberhalb der Stelle liegt, an der die sauerstoffhaltige flüssige Fraktion aus der Drucksäule in die Niederdrucksäule eingespeist wird. Dazwischen liegen beispielsweise 10 bis 20 theoretische Böden.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, which is above the point at which the oxygen-containing liquid Fraction from the pressure column is fed into the low pressure column. Between there are, for example, 10 to 20 theoretical floors.

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 flow of circulating nitrogen refrigeration is generated, which is transported via the liquefied second partial flow 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 partially, 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 extraction, 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 feed of the pressure column sump 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 Unterkühlern 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.At the top of the low pressure column, liquid nitrogen 19 is drawn off and on 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 to 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 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.

Bei dem Ausführungsbeispiel sind verschiedene Abwandlungen denkbar. Falls kein Sauerstoffprodukt gewünscht ist, kann die Sumpfflüssigkeit 8, 10 von der Drucksäule 4 auch unmittelbar über dem Sumpf in die Niederdrucksäule 5 eingeleitet werden, der gleichzeitig den Verdampfungsraum des Hauptkondensators 6 darstellt. In diesem Fall würde das Kühlfluid 15 für den Kopfkondensator 7 entweder aus dem Sumpf der Niederdrucksäule abgezogen oder unmittelbar aus der Drucksäulen-Sumpfflüssigkeit 10 abgezweigt werden.Various modifications are conceivable in the exemplary embodiment. If not Oxygen product is desired, the bottom liquid 8, 10 from the pressure column 4th also be introduced into the low pressure column 5 directly above the sump, the simultaneously represents the evaporation space of the main condenser 6. In this case would the cooling fluid 15 for the top condenser 7 either from the bottom of the Low pressure column withdrawn or directly from the pressure column sump liquid 10 are branched off.

Claims (9)

Verfahren zur Erzeugung von Sauerstoff und Stickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem, das eine Drucksäule (4) und eine Niederdrucksäule (5) aufweist, wobei bei dem Verfahren Einsatzluft (1, 3) in die Drucksäule (4) eingeleitet, eine sauerstoffhaltige flüssige Fraktion (8, 10) aus der Drucksäule (4) entnommen und in die Niederdrucksäule (5) eingespeist wird, gasförmiger Stickstoff (17) aus der Niederdrucksäule (5) in einem Kopfkondensator (7) durch indirekten Wärmeaustausch mit einem verdampfenden Kühlfluid (15) mindestens teilweise kondensiert wird, der Niederdrucksäule (5) und/oder der Drucksäule (4) ein Stickstoff-Produktstrom (19) entnommen und aus der Niederdrucksäule (5) ein Sauerstoff-Produktstrom (61, 62, 63) flüssig und/oder gasförmig abgeführt wird, dadurch gekennzeichnet, dass das Kühlfluid für den Kopfkondensator (7) der Niederdrucksäule (5) durch eine Zwischenflüssigkeit (15) gebildet wird, die von einer Zwischenstelle der Niederdrucksäule (5) abgezogen wird.Process for the production of oxygen and 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 using feed air (1, 3) 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) in a top condenser (7) by indirect heat exchange with an evaporating cooling fluid (15) is condensed at least partially, a nitrogen product stream (19) is removed from the low pressure column (5) and / or the pressure column (4) and an oxygen product stream (61, 62, 63) is discharged in liquid and / or gaseous form from the low pressure column (5) is characterized in that the cooling fluid for the top condenser (7) of the low pressure column (5) is formed by an intermediate liquid (15) which is provided by an intermediate point the low pressure column (5) is withdrawn. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Zwischenflüssigkeit (15) von einer Zwischenstelle abgezogen wird, die oberhalb der Stelle liegt, an der die sauerstoffhaltige flüssige Fraktion (8, 10) aus der Drucksäule (4) in die Niederdrucksäule (5) eingespeist wird.A method according to claim 1, characterized in that the intermediate liquid (15) is withdrawn from an intermediate point which is above the point at which the oxygen-containing liquid fraction (8, 10) from the pressure column (4) is fed into the low pressure column (5) becomes. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass flüssiger Stickstoff (19) aus der Niederdrucksäule (5) oder aus deren Kopfkondensator (7) abgezogen und als flüssiges Stickstoffprodukt (22) abgeführt wird.A method according to claim 1 or 2, characterized in that liquid nitrogen (19) is withdrawn from the low pressure column (5) or from its top condenser (7) and discharged as a liquid nitrogen product (22). Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass Kreislauf-Stickstoff (28, 29, 30, 31, 32) gasförmig aus dem oberen Bereich der Drucksäule (4) abgezogen und in einem Kreislauf-Verdichter (33) verdichtet wird, wobei ein erster Teilstrom (36) des verdichteten Kreislauf-Stickstoffs (35) arbeitsleistend (38) entspannt wird und ein zweiter Teilstrom (42, 47, 50) des verdichteten Kreislauf-Stickstoffs (35) verflüssigt und in das Rektifiziersystem zurückgespeist (52) und/oder als weiteres flüssiges Stickstoffprodukt entnommen wird. Method according to one of claims 1 to 3, characterized in that cycle nitrogen (28, 29, 30, 31, 32) is withdrawn in gaseous form from the upper region of the pressure column (4) and compressed in a cycle compressor (33), wherein a first partial stream (36) of the compressed cycle nitrogen (35) is expanded while performing work (38) and a second partial stream (42, 47, 50) of the compressed cycle nitrogen (35) is liquefied and fed back into the rectification system (52) and / or is taken as a further liquid nitrogen product. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass Kopfstickstoff (11) aus der Drucksäule (4) in einem Hauptkondensator (6) verflüssigt wird.Method according to one of claims 1 to 4, characterized in that top nitrogen (11) from the pressure column (4) is liquefied in a main condenser (6). Verfahren nach Anspruch 5, dadurch gekennzeichnet, dass das im Hauptkondensator gebildete Kondensat (12) mindestens zum Teil (14) in die Niederdrucksäule eingeleitet wird.A method according to claim 5, characterized in that the condensate (12) formed in the main condenser is introduced at least in part (14) into the low pressure column. Verfahren nach Anspruch 5 oder 6, dadurch gekennzeichnet, dass das im Hauptkondensator gebildete Kondensat (12) mindestens zum Teil als flüssiges Stickstoffprodukt (22) abgezogen wird.A method according to claim 5 or 6, characterized in that the condensate (12) formed in the main condenser is withdrawn at least in part as a liquid nitrogen product (22). Vorrichtung zur Erzeugung von Sauerstoff und Stickstoff durch Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das eine Drucksäule (4) und eine Niederdrucksäule (5) aufweist, mit einer Einsatzleitung (1, 3) zum Einleiten von Einsatzluft in die Drucksäule (4), mit einer Flüssigkeitsleitung (8, 10) zum Überleiten einer sauerstoffhaltigen flüssigen Fraktion aus der Drucksäule (4) in die Niederdrucksäule (5), einem Kopfkondensator (7), dessen Verflüssigungsraum mit dem oberen Bereich der Niederdrucksäule (5) verbunden (17, 18) ist und dessen Verdampfungsraum mit einer Kühlmittelleitung (15) zum Einleiten eines Kühlfluids verbunden ist, mit einer Stickstoff-Produktleitung (19), die mit der Niederdrucksäule (5) und/oder mit der Drucksäule (4) verbunden ist und mit einer Sauerstoff-Produktleitung (61, 62, 63), die mit der Niederdrucksäule (5) verbunden ist, dadurch gekennzeichnet, dass die Kühlmittelleitung (15) mit einer Zwischenstelle der Niederdrucksäule (5) verbunden ist.Device for generating oxygen and nitrogen by low-temperature separation of air with a rectification system, which has a pressure column (4) and a low-pressure column (5), with an insert line (1, 3) for introducing feed air into the pressure column (4), with 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 to the upper region of the low pressure column (5) and (17, 18) whose evaporation chamber is connected to a coolant line (15) for introducing a cooling fluid, a nitrogen product line (19) which is connected to the low pressure column (5) and / or to the pressure column (4) and an oxygen product line (61 , 62, 63), which is connected to the low pressure column (5), characterized in that the coolant line (15) with an intermediate point of the low pressure column (5) v is connected. Vorrichtung nach Anspruch 8, dadurch gekennzeichnet, dass die Zwischenstelle, an der die Kühlmittelleitung (15) mit der Niederdrucksäule (5) verbunden ist, oberhalb der Stelle liegt, an der die Flüssigkeitsleitung (8, 10) zum Überleiten einer sauerstoffhaltigen flüssigen Fraktion aus der Drucksäule (4) in die Niederdrucksäule (5) einmündet.Apparatus according to claim 8, characterized in that the intermediate point at which the coolant line (15) is connected to the low pressure column (5) is above the point at which the liquid line (8, 10) for transferring an oxygen-containing liquid fraction from the Pressure column (4) opens into 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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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
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
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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