EP1031804A1 - Air separation process with nitrogen recycling - Google Patents

Air separation process with nitrogen recycling Download PDF

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Publication number
EP1031804A1
EP1031804A1 EP00102977A EP00102977A EP1031804A1 EP 1031804 A1 EP1031804 A1 EP 1031804A1 EP 00102977 A EP00102977 A EP 00102977A EP 00102977 A EP00102977 A EP 00102977A EP 1031804 A1 EP1031804 A1 EP 1031804A1
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EP
European Patent Office
Prior art keywords
pressure column
nitrogen
low
pressure
feed air
Prior art date
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Granted
Application number
EP00102977A
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German (de)
French (fr)
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EP1031804B1 (en
Inventor
Herbert Grad.-Ing. Schoenecker
Jürgen Dipl.-Ing. Voit
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Linde GmbH
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Linde Gas AG
Linde Technische Gase GmbH
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Priority claimed from DE19908451A external-priority patent/DE19908451A1/en
Application filed by Linde Gas AG, Linde Technische Gase GmbH filed Critical Linde Gas AG
Priority to EP20000102977 priority Critical patent/EP1031804B1/en
Publication of EP1031804A1 publication Critical patent/EP1031804A1/en
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Classifications

    • 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
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • 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
    • F25J3/04309—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 nitrogen
    • F25J3/04315—Lowest pressure or impure nitrogen, so-called waste nitrogen 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
    • F25J2200/20—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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/04—Mixing or blending of fluids with the feed stream
    • 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 method for the low-temperature separation of air with a Rectification system that has at least one pressure column and one low pressure column having feed air in a first compressor to a first pressure compressed, cleaned in a cleaning stage, cooled and at least partially in the pressure column is introduced into at least one liquid fraction from the pressure column the low pressure column is fed and a nitrogen-rich fraction from the Low pressure column warmed up and with feed air downstream of the cleaning stage of the Air is mixed.
  • a process of this type and a corresponding device are known from EP 810412 A, known. There, the nitrogen-rich fraction is mixed before using a Compressor recompressed.
  • the invention has for its object a method of the type mentioned as well as specify a corresponding device that is particularly economical economically are and in particular need relatively low investment costs.
  • This object is achieved in that the mixture of feed air and nitrogen-rich fraction is further compressed in a second compressor to a second pressure p 2 , which is greater than the first pressure p 1 .
  • the first and the second compressor can be designed in one or more stages. They can be driven independently of one another or can be coupled to one another via a common shaft or a gear.
  • the first pressure p 1 is preferably in the vicinity of the operating pressure of the low-pressure column, that is to say the difference between the two pressures mentioned is not more than about 0.5 bar.
  • the specific values depend in individual cases on the desired delivery pressure of or one of the products (for example nitrogen) in one of the columns are generated in gaseous form, or after the pressure of one or more Product streams (oxygen and / or nitrogen) flowing out of one of the columns removed and after pressure increase in the liquid state under delivery pressure be evaporated.
  • the "nitrogen-rich fraction” can be made by pure nitrogen or by a mixture Air gases are formed, the nitrogen content, for example, greater than about Is 50 mol%. It can be from the head or from an intermediate point of the low pressure column subtracted from.
  • Cold can further relax in the process by work-relieving nitrogen-rich fraction are generated from the low pressure column. This can for example from the upper area, preferably from the top of the low pressure column subtracted from. It is beneficial if the returnable and the work-performing too relaxing nitrogen-rich fraction together from the low pressure column deducted and warmed if necessary.
  • the more nitrogen-rich Fraction can, for example, at an intermediate temperature of the main heat exchanger be separated from the stream to be recirculated for cooling feed air.
  • an oxygen-containing fraction from the lower one Area of the low pressure column can be relaxed while working, especially in the same relaxation machine.
  • an oxygen-containing fraction is used Example from the bottom of the low pressure column or from the evaporation chamber of the Bottom evaporator of the low pressure column (main condenser) deducted in Main heat exchanger heated to an intermediate temperature and one Relaxation machine fed. Will add another nitrogen-rich Fraction relaxed while working, this is preferably immediately upstream the relaxation work mixed with the oxygen-containing fraction and the two factions to be relaxed are together in the same Relaxation machine (preferably expansion turbine) initiated.
  • the invention also relates to a device for the low-temperature separation of air according to claim 6.
  • the method according to the invention is particularly suitable for methods in which the Operating pressure at the top of the pressure column at 5.7 to 29.7 bar, preferably at 8.7 to 12.7 bar, the operating pressure at the top of the low pressure column at 1.8 to 11.8 bar, is preferably 2.8 to 3.8 bar.
  • Process cold can be caused by work-related relaxation of the process Process stream are generated.
  • the relaxation of one is favorable here Residual gas flow from the low pressure column, for example together with the nitrogen-rich fraction taken from the low pressure column, onto a Intermediate temperature warmed and fed to a relaxation machine.
  • Atmospheric air 1 is drawn in through a filter 2 by a first compressor 3 and compressed to a pressure p 1 of 3 bar.
  • the air 5 is led to a cleaning stage 6, which in the example is formed by a pair of switchable molecular sieve adsorbers.
  • carbon dioxide and water are removed from the feed air.
  • the cleaned feed air flows via lines 7 and 8 to a second compressor 9, which brings it to a pressure p 2 of 9 bar.
  • the heat of compression is removed again in an aftercooler 10.
  • the highly compressed feed air 11 is cooled in a main heat exchanger 12 to approximately dew point and partially liquefied and finally completely fed via line 13 to the pressure column 14 of a two-column rectification system, which also has a low pressure column 15.
  • Pressure column 14 and low pressure column 15 are in a heat-exchanging connection via a common condenser-evaporator (main condenser) 16.
  • the operating pressures (each at the head) in the example are 8.7 bar in the pressure column 14 and 2.8 bar in the low pressure column 15.
  • a first part 18 of the top nitrogen 17 of the pressure column 14 is via the line 18 Main condenser 16 fed and there against evaporating bottom liquid Low pressure column 15 at least partially, preferably essentially completely condensed.
  • the condensate 19 generated in this way is at least partly via line 20 abandoned as a return to the pressure column 14.
  • a subset can be one Internal compression can be supplied by increasing it to a liquid state Pressure and then evaporated against feed air; this variant is not shown in the drawing.
  • part of the condensate 18 as Liquid nitrogen product 21 can be obtained.
  • Another part is connected via line 22 of the gaseous pressure column nitrogen 17 to the main heat exchanger 12, there warmed to about ambient temperature and finally as a pressure nitrogen product 23 deducted.
  • the low pressure column 15 becomes more fluid Oxygen 28 removed from the sump by means of a pump 29 to an increased pressure brought from for example 30 bar and evaporated against feed air 11 and warmed up.
  • oxygen evaporation takes place in the main heat exchanger 12 instead.
  • the oxygen is finally discharged via line 31 as a printed product.
  • impure nitrogen 32 becomes nitrogen-rich Fraction removed and in the counterflow 25 and in the main heat exchanger 12th warmed up.
  • the nitrogen-rich fraction warmed to around ambient temperature 33 is mixed with the cleaned feed air 7, together with this via line 8 the second compressor 9 and further via the lines 11 and 13 of the pressure column 14 fed.
  • the practical unpressurized residual gas is transferred Line 37 from the warm end of the main heat exchanger 12.
  • a first part 38 of the heated unpressurized residual gas 37 can in the cleaning stage 6 as Regeneration gas are used, while the rest 39 in the example in the Atmosphere is blown off.
  • the embodiment can be easily modified, for example Generation of a more enriched nitrogen product in the low pressure column 15.
  • at least one further must be above the feed 27 of the raw oxygen Rectification section may be provided, at the head of which the nitrogen-rich fraction 32 is subtracted.
  • this Impure nitrogen discharge can also pure nitrogen at the top of the low pressure column 15 be won.
  • part of the liquid nitrogen 19 from Main condenser 16 of the low pressure column 15 is supplied as the return liquid become.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

A low temperature air fractionating system uses a rectification unit comprising pressure and low pressure columns and a nitrogen fraction recycle to the system air feed inlet, to provide bulk nitrogen. A low temperature air fractionating system uses a rectification unit comprising pressure and low pressure columns (14,15) respectively. Feed air (1) is boosted to a pressure p1, by a compressor (3), purified through a system (6), cooled via an exchanger (12), and at least in part fed to the pressure column (14) via a line (13). At least one liquid fraction (24) from the column (14) is fed into the low pressure column via inlet (27), and a nitrogen rich stream (32) is drawn from column (15), heated through exchanger (12), and mixed with clean feedstock air (7) to provide a feed stream (8) which is pressurized to p2 ( greater than p1) by a compressor (9). An Independent claim is also included for a plant for operating the process of the invention.

Description

Die Erfindung betrifft ein Verfahren zur Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das mindestens eine Drucksäule und eine Niederdrucksäule aufweist, wobei Einsatzluft in einem ersten Verdichter auf einen ersten Druck verdichtet, in einer Reinigungsstufe gereinigt, abgekühlt und mindestens teilweise in die Drucksäule eingeleitet wird, mindestens eine Flüssigfraktion aus der Drucksäule in die Niederdrucksäule eingespeist wird und eine stickstoffreiche Fraktion aus der Niederdrucksäule angewärmt und mit Einsatzluft stromabwärts der Reinigungsstufe der Einsatzluft vermischt wird.The invention relates to a method for the low-temperature separation of air with a Rectification system that has at least one pressure column and one low pressure column having feed air in a first compressor to a first pressure compressed, cleaned in a cleaning stage, cooled and at least partially in the pressure column is introduced into at least one liquid fraction from the pressure column the low pressure column is fed and a nitrogen-rich fraction from the Low pressure column warmed up and with feed air downstream of the cleaning stage of the Air is mixed.

Ein Prozeß dieser Art sowie eine entsprechende Vorrichtung sind aus EP 810412 A , bekannt. Dort wird die stickstoffreiche Fraktion vor ihrer Vermischung mittels eines Verdichters rückverdichtet.A process of this type and a corresponding device are known from EP 810412 A, known. There, the nitrogen-rich fraction is mixed before using a Compressor recompressed.

Ein ähnliches Verfahren ist aus der DE-3814187-C2 bekannt. Hier wird unreiner Stickstoff von einer Zwischenstelle der Niederdrucksäule vor die erste Stufe des Luftverdichters zurückgeführt. Einen weiteren ähnlichen Prozeß zeigt US 4848996, wo der unreine Stickstoff am Kopf der Niederdrucksäule abgenommen und der Einsatzluft an einer Zwischenstufe des Luftverdichters zugemischt wird.A similar method is known from DE-3814187-C2. Here becomes impure Nitrogen from an intermediate point of the low pressure column before the first stage of the Air compressor returned. Another similar process shows US 4848996, where the impure nitrogen is removed from the top of the low pressure column and the feed air is mixed in at an intermediate stage of the air compressor.

Die Rückführung der stickstoffreichen Fraktion in die Einsatzluft ist an sich vorteilhaft und erhöht die Produktausbeute. Das Verfahren ist dennoch einer weiteren Verbesserung zugänglich.The return of the nitrogen-rich fraction to the feed air is advantageous in itself and increases product yield. The process is still another Improvement accessible.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art sowie eine entsprechende Vorrichtung anzugeben, die wirtschaftlich besonders günstig sind und insbesondere relativ niedrige Investitionskosten benötigen.The invention has for its object a method of the type mentioned as well as specify a corresponding device that is particularly economical economically are and in particular need relatively low investment costs.

Diese Aufgabe wird dadurch gelöst, daß das Gemisch aus Einsatzluft und stickstoffreicher Fraktion in einem zweiten Verdichter auf einen zweiten Druck p2 weiterverdichtet wird, der größer als der erste Druck p1 ist. This object is achieved in that the mixture of feed air and nitrogen-rich fraction is further compressed in a second compressor to a second pressure p 2 , which is greater than the first pressure p 1 .

Auf diese Weise wird der Aufwand beim Verdichten der Einsatzluft und beim Rückverdichten der stickstoffreichen Fraktion vergleichsweise gering gehalten. Der erste und der zweite Verdichter können ein- oder mehrstufig ausgeführt sein. Sie können unabhängig voneinander angetrieben oder über eine gemeinsame Welle oder ein Getriebe miteinander gekoppelt sein. Vorzugsweise liegt der erste Druck p1 in der Nähe des Betriebsdrucks der Niederdrucksäule, das heißt die Differenz zwischen den beiden genannten Drücken beträgt nicht mehr als etwa 0,5 bar.In this way, the effort involved in compressing the feed air and recompressing the nitrogen-rich fraction is kept comparatively low. The first and the second compressor can be designed in one or more stages. They can be driven independently of one another or can be coupled to one another via a common shaft or a gear. The first pressure p 1 is preferably in the vicinity of the operating pressure of the low-pressure column, that is to say the difference between the two pressures mentioned is not more than about 0.5 bar.

Bevorzugte Wertebereiche für die Auslaßdrücke der beiden Verdichter sind:

erster Verdichter (p1):
2 bis 12 bar, vorzugsweise 3 bis 4 bar
zweiter Verdichter (p2):
6 bis 40 bar, vorzugsweise 9 bis 13 bar
Preferred ranges of values for the outlet pressures of the two compressors are:
first compressor (p 1 ):
2 to 12 bar, preferably 3 to 4 bar
second compressor (p 2 ):
6 to 40 bar, preferably 9 to 13 bar

Die konkreten Werte richten sich im Einzelfall nach dem gewünschten Abgabedruck des oder eines der Produkte (zum Beispiel Stickstoff), die in einer der Säulen gasförmig erzeugt werden, beziehungsweise nach dem Druck eines oder mehrerer Produktströme (Sauerstoff und/oder Stickstoff), die flüssig aus einer der Säulen entnommen und nach Druckerhöhung in flüssigem Zustand unter Abgabedruck verdampft werden.The specific values depend in individual cases on the desired delivery pressure of or one of the products (for example nitrogen) in one of the columns are generated in gaseous form, or after the pressure of one or more Product streams (oxygen and / or nitrogen) flowing out of one of the columns removed and after pressure increase in the liquid state under delivery pressure be evaporated.

Die "stickstoffreiche Fraktion" kann durch reinen Stickstoff oder durch ein Gemisch aus Luftgasen gebildet werden, dessen Stickstoffgehalt beispielsweise größer als etwa 50 mol% ist. Sie kann vom Kopf oder von einer Zwischenstelle der Niederdrucksäule abgezogen werden.The "nitrogen-rich fraction" can be made by pure nitrogen or by a mixture Air gases are formed, the nitrogen content, for example, greater than about Is 50 mol%. It can be from the head or from an intermediate point of the low pressure column subtracted from.

Es ist günstig, wenn die Anwärmung der stickstoffreichen Fraktion mindestens teilweise durch indirekten Wärmeaustausch mit der Einsatzluft, beispielsweise stromabwärts des zweiten Verdichters, durchgeführt wird.It is beneficial if the heating of the nitrogen-rich fraction at least partly through indirect heat exchange with the feed air, for example downstream of the second compressor.

Die Vorteile des erfindungsgemäßen Verfahrens kommen besonders zum Tragen, wenn eine Stickstofffraktion aus dem oberen Bereich der Drucksäule entnommen, angewärmt und als Druckstickstoffprodukt abgezogen wird. Die günstige Form der Rückführung einer stickstoffreichen Fraktion aus der Niederdrucksäule in die Einsatzluft bewirkt eine besonders hohe Ausbeute an Druckstickstoffprodukt bei relativ geringem apparativen Aufwand. The advantages of the method according to the invention are particularly evident. when a nitrogen fraction is taken from the top of the pressure column, warmed up and withdrawn as a pressure nitrogen product. The cheap form of Return of a nitrogen-rich fraction from the low pressure column to the Feed air causes a particularly high yield of pressurized nitrogen product at relative low expenditure on equipment.

Kälte kann in dem Verfahren durch arbeitsleistende Entspannung einer weiteren stickstoffreichen Fraktion aus der Niederdrucksäule erzeugt werden. Diese kann beispielsweise aus dem oberen Bereich, vorzugsweise vom Kopf der Niederdrucksäule abgezogen werden. Es ist günstig, wenn die rückzuführende und die arbeitsleistend zu entspannende stickstoffreiche Fraktion gemeinsam aus der Niederdrucksäule abgezogen und gegebenenfalls angewärmt werden. Die weitere stickstoffreiche Fraktion kann beispielsweise bei einer Zwischentemperatur des Hauptwärmetauschers zur Abkühlung von Einsatzluft von dem rückzuführenden Strom abgetrennt werden.Cold can further relax in the process by work-relieving nitrogen-rich fraction are generated from the low pressure column. This can for example from the upper area, preferably from the top of the low pressure column subtracted from. It is beneficial if the returnable and the work-performing too relaxing nitrogen-rich fraction together from the low pressure column deducted and warmed if necessary. The more nitrogen-rich Fraction can, for example, at an intermediate temperature of the main heat exchanger be separated from the stream to be recirculated for cooling feed air.

Alternativ oder zusätzlich kann eine sauerstoffhaltige Fraktion aus dem unteren Bereich der Niederdrucksäule arbeitsleistend entspannt werden, insbesondere in derselben Entspannungsmaschine. Dazu wird eine sauerstoffhaltige Fraktion zum Beispiel vom Sumpf der Niederdrucksäule oder aus dem Verdampfungsraum des Sumpfverdampfers der Niederdrucksäule (Hauptkondensators) abgezogen, im Hauptwärmetauscher auf eine Zwischentemperatur angewärmt und einer Entspannungsmaschine zugeführt. Wird zusätzlich eine weitere stickstoffreiche Fraktion arbeitsleistend entspannt, wird diese vorzugsweise unmittelbar stromaufwärts der arbeitsleistenden Entspannung mit der sauerstoffhaltigen Fraktion vermischt und die beiden zu entspannenden Fraktionen werden gemeinsam in dieselbe Entspannungsmaschine (vorzugsweise Expansionsturbine) eingeleitet.Alternatively or additionally, an oxygen-containing fraction from the lower one Area of the low pressure column can be relaxed while working, especially in the same relaxation machine. For this purpose, an oxygen-containing fraction is used Example from the bottom of the low pressure column or from the evaporation chamber of the Bottom evaporator of the low pressure column (main condenser) deducted in Main heat exchanger heated to an intermediate temperature and one Relaxation machine fed. Will add another nitrogen-rich Fraction relaxed while working, this is preferably immediately upstream the relaxation work mixed with the oxygen-containing fraction and the two factions to be relaxed are together in the same Relaxation machine (preferably expansion turbine) initiated.

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

Das erfindungsgemäße Verfahren ist besonders für Verfahren geeignet, bei denen der Betriebsdruck am Kopf der Drucksäule bei 5,7 bis 29,7 bar, vorzugsweise bei 8,7 bis 12,7 bar, der Betriebsdruck am Kopf der Niederdrucksäule bei 1,8 bis 11,8 bar, vorzugsweise bei 2,8 bis 3,8 bar liegt.The method according to the invention is particularly suitable for methods in which the Operating pressure at the top of the pressure column at 5.7 to 29.7 bar, preferably at 8.7 to 12.7 bar, the operating pressure at the top of the low pressure column at 1.8 to 11.8 bar, is preferably 2.8 to 3.8 bar.

Verfahrenskälte kann bei dem Verfahren durch arbeitsleistende Entspannung eines Prozeßstroms erzeugt werden. Günstig ist hierbei die Entspannung eines Restgasstroms aus der Niederdrucksäule, der beispielsweise gemeinsam mit der stickstoffreichen Fraktion aus der Niederdrucksäule entnommen, auf eine Zwischentemperatur angewärmt und einer Entspannungsmaschine zugeleitet wird. Process cold can be caused by work-related relaxation of the process Process stream are generated. The relaxation of one is favorable here Residual gas flow from the low pressure column, for example together with the nitrogen-rich fraction taken from the low pressure column, onto a Intermediate temperature warmed and fed to a relaxation machine.

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.

Atmosphärische Luft 1 wird über ein Filter 2 von einem ersten Verdichter 3 angesaugt und auf einen Druck p1 von 3 bar verdichtet. Nach Entfernung der Verdichtungswärme in einem Nachkühler 4 wird die Luft 5 zu einer Reinigungsstufe 6 geführt, die in dem Beispiel durch ein Paar von umschaltbaren Molekularsiebadsorbern gebildet wird. In der Reinigungsstufe 6 werden insbesondere Kohlendioxid und Wasser aus der Einsatzluft entfernt. Die gereinigte Einsatzluft strömt über die Leitungen 7 und 8 einem zweiten Verdichter 9 zu, der sie auf einen Druck p2 von 9 bar bringt. Erneut wird die Verdichtungswärme in einem Nachkühler 10 entfernt. Die hochverdichtete Einsatzluft 11 wird in einem Hauptwärmetauscher 12 auf etwa Taupunkt abgekühlt und teilweise verflüssigt und schließlich über Leitung 13 vollständig der Drucksäule 14 eines Zweisäulen-Rektifiziersystems zugeführt, das außerdem eine Niederdrucksäule 15 aufweist. Drucksäule 14 und Niederdrucksäule 15 stehen über einen gemeinsamen Kondensator-Verdampfer (Hauptkondensator) 16 in wärmetauschender Verbindung. Die Betriebsdrücke (jeweils am Kopf) betragen in dem Beispiel 8,7 bar in der Drucksäule 14 und 2,8 bar in der Niederdrucksäule 15.Atmospheric air 1 is drawn in through a filter 2 by a first compressor 3 and compressed to a pressure p 1 of 3 bar. After removal of the heat of compression in an aftercooler 4, the air 5 is led to a cleaning stage 6, which in the example is formed by a pair of switchable molecular sieve adsorbers. In the cleaning stage 6 in particular carbon dioxide and water are removed from the feed air. The cleaned feed air flows via lines 7 and 8 to a second compressor 9, which brings it to a pressure p 2 of 9 bar. The heat of compression is removed again in an aftercooler 10. The highly compressed feed air 11 is cooled in a main heat exchanger 12 to approximately dew point and partially liquefied and finally completely fed via line 13 to the pressure column 14 of a two-column rectification system, which also has a low pressure column 15. Pressure column 14 and low pressure column 15 are in a heat-exchanging connection via a common condenser-evaporator (main condenser) 16. The operating pressures (each at the head) in the example are 8.7 bar in the pressure column 14 and 2.8 bar in the low pressure column 15.

Ein erster Teil 18 des Kopfstickstoffs 17 der Drucksäule 14 wird über Leitung 18 dem Hauptkondensator 16 zugeführt und dort gegen verdampfende Sumpfflüssigkeit der Niederdrucksäule 15 mindestens teilweise, vorzugsweise im wesentlichen vollständig kondensiert. Das dabei erzeugte Kondensat 19 wird mindestens zum Teil über Leitung 20 als Rücklauf auf die Drucksäule 14 aufgegeben. (Eine Teilmenge kann einer Innenverdichtung zugeführt werden, indem sie in flüssigem Zustand auf einen erhöhten Druck gebracht und anschließend gegen Einsatzluft verdampft wird; diese Variante ist in der Zeichnung nicht dargestellt.) Bei Bedarf kann ein Teil des Kondensats 18 als Flüssigstickstoffprodukt 21 gewonnen werden. Über Leitung 22 wird ein weiterer Teil des gasförmigen Drucksäulenstickstoffs 17 zum Hauptwärmetauscher 12 geführt, dort auf etwa Umgebungstemperatur angewärmt und schließlich als Druckstickstoffprodukt 23 abgezogen.A first part 18 of the top nitrogen 17 of the pressure column 14 is via the line 18 Main condenser 16 fed and there against evaporating bottom liquid Low pressure column 15 at least partially, preferably essentially completely condensed. The condensate 19 generated in this way is at least partly via line 20 abandoned as a return to the pressure column 14. (A subset can be one Internal compression can be supplied by increasing it to a liquid state Pressure and then evaporated against feed air; this variant is not shown in the drawing.) If necessary, part of the condensate 18 as Liquid nitrogen product 21 can be obtained. Another part is connected via line 22 of the gaseous pressure column nitrogen 17 to the main heat exchanger 12, there warmed to about ambient temperature and finally as a pressure nitrogen product 23 deducted.

Aus dem unteren Bereich der Drucksäule 14, vorzugsweise vom Sumpf, wird flüssiger Rohsauerstoff 24 abgezogen, in einem Gegenströmer 25 unterkühlt, entspannt (26) und in die Niederdrucksäule 15 eingeführt (27), die in dem Beispiel als reine Abtriebssäule ausgebildet ist. Als Hauptprodukt wird der Niederdrucksäule 15 flüssiger Sauerstoff 28 am Sumpf entnommen, mittels einer Pumpe 29 auf einen erhöhten Druck von beispielsweise 30 bar gebracht und gegen Einsatzluft 11 verdampft und angewärmt. Die Sauerstoffverdampfung findet in dem Beispiel im Hauptwärmetauscher 12 statt. Der Sauerstoff wird schließlich über Leitung 31 als Druckprodukt abgeführt.The lower area of the pressure column 14, preferably from the sump, becomes more liquid Crude oxygen 24 drawn off, subcooled in a countercurrent 25, expanded (26) and introduced into the low pressure column 15 (27), which in the example as pure Output column is formed. As the main product, the low pressure column 15 becomes more fluid Oxygen 28 removed from the sump by means of a pump 29 to an increased pressure brought from for example 30 bar and evaporated against feed air 11 and warmed up. In the example, oxygen evaporation takes place in the main heat exchanger 12 instead. The oxygen is finally discharged via line 31 as a printed product.

Am Kopf der Niederdrucksäule 15 wird unreiner Stickstoff 32 als stickstoffreiche Fraktion entnommen und im Gegenströmer 25 und im Hauptwärmetauscher 12 angewärmt. Die auf etwa Umgebungstemperatur angewärmte stickstoffreiche Fraktion 33 wird der gereinigten Einsatzluft 7 zugemischt, gemeinsam mit dieser über Leitung 8 dem zweiten Verdichter 9 und weiter über die Leitungen 11 und 13 der Drucksäule 14 zugeführt.At the top of the low-pressure column 15, impure nitrogen 32 becomes nitrogen-rich Fraction removed and in the counterflow 25 and in the main heat exchanger 12th warmed up. The nitrogen-rich fraction warmed to around ambient temperature 33 is mixed with the cleaned feed air 7, together with this via line 8 the second compressor 9 and further via the lines 11 and 13 of the pressure column 14 fed.

Ein Teil 34 des über Leitung 32 aus der Niederdrucksäule 15 abgezogenen unreinen Stickstoffs kann bei einer Zwischentemperatur aus dem Hauptwärmetauscher 12 herausgeführt, arbeitsleistend entspannt (35) und über Leitung 36 wieder dem Hauptwärmetauscher 12 zugeleitet werden. Das praktische drucklose Restgas tritt über Leitung 37 aus dem warmen Ende des Hauptwärmetauschers 12 aus. Ein erster Teil 38 des angewärmten drucklosen Restgases 37 kann in der Reinigungsstufe 6 als Regeneriergas eingesetzt werden, während der Rest 39 in dem Beispiel in die Atmosphäre abgeblasen wird.A part 34 of the impure withdrawn via line 32 from the low pressure column 15 Nitrogen can escape from the main heat exchanger 12 at an intermediate temperature led out, work relieved (35) and via line 36 again Main heat exchanger 12 are supplied. The practical unpressurized residual gas is transferred Line 37 from the warm end of the main heat exchanger 12. A first part 38 of the heated unpressurized residual gas 37 can in the cleaning stage 6 as Regeneration gas are used, while the rest 39 in the example in the Atmosphere is blown off.

Das Ausführungsbeispiel kann leicht abgewandelt werden, beispielsweise zur Erzeugung eines stärker angereicherten Stickstoffprodukts in der Niederdrucksäule 15. Dazu muß oberhalb der Zuspeisung 27 des Rohsauerstoffs mindestens ein weiterer Rektifizierabschnitt vorgesehen sein, an dessen Kopf die stickstoffreiche Fraktion 32 abgezogen wird. Mit Hilfe eines weiteren Abschnitts oberhalb dieses Unreinstickstoffabzugs kann am Kopf der Niederdrucksäule 15 auch reiner Stickstoff gewonnen werden. In beiden Fällen muß ein Teil des flüssigen Stickstoffs 19 von Hauptkondensator 16 der Niederdrucksäule 15 als Rücklaufflüssigkeit zugeführt werden.The embodiment can be easily modified, for example Generation of a more enriched nitrogen product in the low pressure column 15. For this purpose, at least one further must be above the feed 27 of the raw oxygen Rectification section may be provided, at the head of which the nitrogen-rich fraction 32 is subtracted. With the help of another section above this Impure nitrogen discharge can also pure nitrogen at the top of the low pressure column 15 be won. In both cases, part of the liquid nitrogen 19 from Main condenser 16 of the low pressure column 15 is supplied as the return liquid become.

Alternativ oder zusätzlich zu der dargestellten Drucksauerstoffgewinnung mittels Innenverdichtung kann gasförmiger Sauerstoff direkt über dem Sumpf der Niederdrucksäule 15 oder einige Böden oberhalb als Produkt entnommen werden; auch die Gewinnung von Sauerstoff aus dem Sumpf der Niederdrucksäule 15 als Flüssigprodukt ist möglich, beispielsweise durch eine Entnahme aus der Leitung 28 stromaufwärts der Pumpe 29.As an alternative or in addition to the pressure oxygen production shown by means of Internal compression can create gaseous oxygen directly above the sump Low pressure column 15 or some trays above are removed as a product; also the extraction of oxygen from the bottom of the low pressure column 15 as Liquid product is possible, for example by removal from line 28 upstream of the pump 29.

Claims (6)

Verfahren zur Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das mindestens eine Drucksäule (14) und eine Niederdrucksäule (15) aufweist, wobei Einsatzluft (1) in einem ersten Verdichter (3) auf einen ersten Druck p1 verdichtet (3), in einer Reinigungsstufe (6) gereinigt, abgekühlt (12) und mindestens teilweise in die Drucksäule (14) eingeleitet (13) wird, mindestens eine Flüssigfraktion (24) aus der Drucksäule (14) in die Niederdrucksäule (15) eingespeist (26, 27) wird und eine stickstoffreiche Fraktion (32) aus der Niederdrucksäule (15) angewärmt (25, 12) und mit Einsatzluft (7) stromabwärts der Reinigungsstufe (6) der Einsatzluft vermischt wird, dadurch gekennzeichnet, daß das Gemisch (8) aus Einsatzluft und stickstoffreicher Fraktion in einem zweiten Verdichter (9) auf einen zweiten Druck p2 weiterverdichtet wird, der größer als der erste Druck p1 ist.Method for the low-temperature separation of air with a rectification system, which has at least one pressure column (14) and one low-pressure column (15), wherein feed air (1) compresses (3) to a first pressure p 1 (3) in a first compressor (3) in a cleaning stage (6) cleaned, cooled (12) and at least partially introduced (13) into the pressure column (14), at least one liquid fraction (24) from the pressure column (14) is fed (26, 27) into the low pressure column (15) and a nitrogen-rich fraction (32) from the low-pressure column (15) is heated (25, 12) and mixed with feed air (7) downstream of the cleaning stage (6) of the feed air, characterized in that the mixture (8) of feed air and nitrogen-rich fraction in a second compressor (9) is further compressed to a second pressure p 2 which is greater than the first pressure p 1 . Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Anwärmung der stickstoffreichen Fraktion (32) mindestens teilweise durch indirekten Wärmeaustausch (12) mit Einsatzluft (11) durchgeführt wird.A method according to claim 1, characterized in that the nitrogen-rich fraction (32) is at least partially heated by indirect heat exchange (12) with feed air (11). Verfahren nach einem der Ansprüche 1 oder 2, dadurch gekennzeichnet, daß eine Stickstofffraktion (17, 22) aus dem oberen Bereich der Drucksäule (14) entnommen, angewärmt (12) und als Druckstickstoffprodukt (23) abgezogen wird.Method according to one of claims 1 or 2, characterized in that a nitrogen fraction (17, 22) is removed from the upper region of the pressure column (14), heated (12) and withdrawn as a pressure nitrogen product (23). Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß eine weitere stickstoffreiche Fraktion (32, 34) aus der Niederdrucksäule (15) arbeitsleistend entspannt (35) wird.Method according to one of claims 1 to 3, characterized in that a further nitrogen-rich fraction (32, 34) from the low-pressure column (15) is expanded (35) while performing work. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß sauerstoffhaltige Fraktion aus dem unteren Bereich der Niederdrucksäule arbeitsleistend entspannt wird.Method according to one of claims 1 to 4, characterized in that the oxygen-containing fraction from the lower region of the low-pressure column is relaxed while performing work. Vorrichtung zur Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das mindestens eine Drucksäule (14) und eine Niederdrucksäule (15) aufweist, und mit einer Einsatzluftleitung (1, 5, 7, 8, 11, 13), die über einen ersten Verdichter (3), eine Reinigungsstufe (6) und einen Hauptwärmetauscher (12) in die Drucksäule (14) führt, mit einer Flüssigkeitsleitung (24, 27) zur Einführung einer Flüssigfraktion aus der Drucksäule (14) in die Niederdrucksäule (15) und mit einer Rückführleitung (32, 33) für eine stickstoffreiche Fraktion aus der Niederdrucksäule (15), die durch den Hauptwärmetauscher (12) führt und stromabwärts der Reinigungsstufe (6) in die Einsatzluftleitung (7) mündet, dadurch gekennzeichnet, daß ein zweiter Verdichter in der Einsatzluftleitung (8, 11) stromabwärts der Einmündung der Rückführleitung (33) angeordnet ist.Device for the low-temperature separation of air with a rectification system, which has at least one pressure column (14) and a low-pressure column (15), and with a feed air line (1, 5, 7, 8, 11, 13), which via a first compressor (3) , a cleaning stage (6) and a main heat exchanger (12) leads into the pressure column (14), with a liquid line (24, 27) for introducing a liquid fraction from the pressure column (14) into the low pressure column (15) and with a return line (32 , 33) for a nitrogen-rich fraction from the low pressure column (15), which leads through the main heat exchanger (12) and opens into the feed air line (7) downstream of the cleaning stage (6), characterized in that a second compressor in the feed air line (8, 11) is arranged downstream of the mouth of the return line (33).
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