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EP0955509A1 - Process and apparatus to produce high purity nitrogen - Google Patents

Process and apparatus to produce high purity nitrogen Download PDF

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Publication number
EP0955509A1
EP0955509A1 EP98116041A EP98116041A EP0955509A1 EP 0955509 A1 EP0955509 A1 EP 0955509A1 EP 98116041 A EP98116041 A EP 98116041A EP 98116041 A EP98116041 A EP 98116041A EP 0955509 A1 EP0955509 A1 EP 0955509A1
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EP
European Patent Office
Prior art keywords
pressure column
low
pressure
liquid
nitrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP98116041A
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German (de)
French (fr)
Other versions
EP0955509B1 (en
Inventor
Dietrich Dipl.-Ing. Rottmann
Horst Dipl.-Ing. Corduan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
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Linde GmbH
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Publication date
Priority claimed from DE19819338A external-priority patent/DE19819338A1/en
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP0955509A1 publication Critical patent/EP0955509A1/en
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Publication of EP0955509B1 publication Critical patent/EP0955509B1/en
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/04084—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J3/04151—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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
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    • F25J3/04151—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
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    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another column
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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/02—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
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
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    • 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
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    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
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    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
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    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
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    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen

Definitions

  • part of the liquid flowing down in the low-pressure column 5 is removed as nitrogen fraction 20, brought to pressure in the liquid state (14 bar in the example) (pump 21) and via line 22 through the subcooler 15 to a product evaporator 23.
  • the nitrogen 24 evaporated under a pressure of 13.4 bar is heated in the main heat exchanger 2 and discharged as a high-purity pressure product 25. If necessary, it can be further compressed in the gaseous state.
  • the high purity pressurized nitrogen product 25 has a total contamination of 10 ppb (including carbon monoxide).

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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 rectification process and assembly for the production of nitrogen has a pressurised column (4) and a low pressure column (5). Process air (1, 3; 1, 3') is introduced to the pressurised column (4) which subsequently discharges an oxygen-enriched fraction (11) into the low pressure column (5). Gaseous nitrogen (18) is discharged from the low pressure column (5) into a condenser head (17), where it is at least partly condensed by indirect heat exchange with an evaporating fluid (13; 13', 44). Gaseous nitrogen (24,24', 25, 29) is discharged from the low-pressure column (5) at a pressure which is higher than the operating pressure of the low-pressure column (5). Part of the liquid nitrogen generated by indirect heat exchange in the condenser head (17), or part of the liquid nitrogen (20) drawn from the low-pressure column (5), is in liquid condition to a pressure (21) which exceeds that the pressure in the low-pressure column (5). The resulting pressurised nitrogen is then evaporated in a product evaporator (23) by indirect heat exchange supplied by another medium (35, 35') to be surrendered as compressed nitrogen (24, 24', 25, 29). The product evaporator can be located inside or outside the columns.

Description

Die Erfindung betrifft ein Verfahren zur Gewinnung von hochreinem Sauerstoff gemäß dem Oberbegriff von Patentanspruch 1.The invention relates to a method for obtaining high-purity oxygen according to the preamble of patent claim 1.

Ein Verfahren mit diesen Schritten ist aus DE 3528374 A1 bekannt. Bei diesem Zweisäulenprozeß weist die Niederdrucksäule einen Kopfkondensator auf, in dem gasförmiger Kopfstickstoff kondensiert und als Rücklauf auf die Niederdrucksäule aufgegeben wird. Diese Art der Erzeugung von Rücklauf für die Niederdrucksäule ermöglicht es, einen Teil des in der Doppelsäule erzeugten Stickstoffs als Druckprodukt abzuführen. Die an Sauerstoff angereicherte Flüssigkeit, die als Sumpfprodukt der Niederdrucksäule anfällt, wird vollständig auf die Verdampfungsseite des Kopfkondensators der Niederdrucksäule geleitet und als Restgas abgeführt.A method with these steps is known from DE 3528374 A1. In this two-column process, the low-pressure column has a top condenser in which gaseous top nitrogen is condensed and fed to the low-pressure column as a return. This type of generation of reflux for the low pressure column makes it possible to remove part of the nitrogen generated in the double column as a printed product. The oxygen-enriched liquid, which is obtained as the bottom product of the low-pressure column, is passed completely to the evaporation side of the top condenser of the low-pressure column and removed as residual gas.

Der Erfindung liegt die Aufgabe zugrunde, bei einem Verfahren der eingangs genannten Art ein hochreines Sauerstoffprodukt zu gewinnen, insbesondere zusätzlich zu einem Druckstickstoffprodukt.The invention has for its object to obtain a high-purity oxygen product in a method of the type mentioned, in particular in addition to a pressure nitrogen product.

Diese Aufgabe wird dadurch gelöst, daß die sauerstoffhaltige flüssige Fraktion, die in die Niederdrucksäule eingespeist wird, mindestens einen theoretischen oder praktischen Boden oberhalb des Sumpfs der Drucksäule entnommen wird, daß Sumpfflüssigkeit der Drucksäule in den Verdampfungsraum des Kopfkondensators der Niederdrucksäule geleitet wird und daß aus dem unteren Bereich der Niederdrucksäule ein hochreines Sauerstoffprodukt entnommen wird.This object is achieved in that the oxygen-containing liquid fraction which is fed into the low-pressure column is taken from at least one theoretical or practical base above the sump of the pressure column, that sump liquid from the pressure column is passed into the evaporation chamber of the top condenser of the low-pressure column and that from the a high-purity oxygen product is removed from the lower region of the low-pressure column.

Bei der Produktion von hochreinem Sauerstoff ist die Verringerung des Stickstoff- und Argongehalts im Sauerstoffprodukt relativ unkritisch; diese kann durch eine entsprechend hohe Anzahl von Böden im unteren Abschnitt der Niederdrucksäule erzielt werden. Diese übliche Maßnahme verhindert jedoch nicht, daß sich sämtliche schwererflüchtigen Verunreinigungen im Sauerstoffprodukt ansammeln, also Luftbestandteile, deren Siedepunkt höher als derjenige von Sauerstoff ist und die durch die Vorreinigung stromaufwärts der Einleitung in das Rektifiziersystem nicht entfernt wurden. Solche schwererflüchtigen Luftbestandteile werden beispielsweise durch Krypton, Xenon und Kohlenwasserstoffe gebildet. Es ist bekannt, derartige Verunreinigungen in einem oder mehreren nachfolgenden Rektifizierschritten zu entfernen (siehe beispielsweise EP-299364-B1.In the production of high-purity oxygen, the reduction in the nitrogen and argon content in the oxygen product is relatively uncritical; this can be achieved by a correspondingly high number of trays in the lower section of the low pressure column. However, this customary measure does not prevent all of the less volatile impurities from accumulating in the oxygen product, that is to say air components whose boiling point is higher than that of oxygen and which were not removed by the pre-cleaning upstream of the introduction into the rectification system. Such less volatile air components are formed, for example, by krypton, xenon and hydrocarbons. It is known to remove such impurities in one or more subsequent rectification steps (see for example EP-299364-B1.

Die erfindungsgemäße Lösung kommt ohne zusätzliche Rektifiziersäulen aus und nutzt den unteren Teil der Drucksäule beziehungsweise einen zusätzlichen Stoffaustauschabschnitt im unteren Abschnitt der Drucksäule für die Abtrennung der schwererflüchtigen Verunreinigungen. Dazu wird die sauerstoffhaltige flüssige Fraktion, die in die Niederdrucksäule geleitet wird, nicht aus dem Sumpf der Drucksäule abgezogen, sondern von einer oberhalb des Sumpfs, insbesondere oberhalb der Zuspeisung der Einsatzluft, gelegenen Zwischenstelle. Dazwischen befindet sich ein Stoffaustauschabschnitt im Umfang mindestens eines theoretischen oder praktischen Bodens. Vorzugsweise umfaßt er 1 bis 10, höchst vorzugsweise 2 bis 5 theoretische oder praktische Böden, die zwischen Luftzuspeisung beziehungsweise Drucksäulensumpf einerseits und Entnahmestelle der sauerstoffhaltigen flüssigen Fraktion andererseits angeordnet sind. (Für den Fall, daß in diesem Abschnitt ausschließlich praktische Böden als Stoffaustauschelemente verwendet werden, gelten die Angaben in praktischen Bodenzahlen; falls Packung, Füllkörper oder Kombinationen verschiedener Typen von Stoffaustauschelementen eingesetzt werden, sind die Angaben in theoretischen Bodenzahlen anzuwenden.)The solution according to the invention manages without additional rectification columns and uses the lower part of the pressure column or an additional mass transfer section in the lower section of the pressure column for the separation of the less volatile impurities. For this purpose, the oxygen-containing liquid fraction which is passed into the low-pressure column is not drawn off from the bottom of the pressure column, but from an intermediate point located above the bottom, in particular above the feed of the feed air. In between there is a mass transfer section in the scope of at least one theoretical or practical floor. It preferably comprises 1 to 10, most preferably 2 to 5 theoretical or practical trays which are arranged between the air supply or pressure column sump on the one hand and the point of withdrawal of the oxygen-containing liquid fraction on the other. (In the event that only practical floors are used as mass transfer elements in this section, the information in practical plate numbers applies; if packing, packing or combinations of different types of material exchange elements are used, the data in theoretical plate numbers are to be used.)

Durch die Entnahme des Einsatzes oberhalb der Luftzuspeisung werden schwererflüchtige Bestandteile der Luft wie Kohlenwasserstoffe, Krypton und Xenon aus der Niederdrucksäule ferngehalten. An deren Sumpf wird ein hochreines Sauerstoffprodukt entnommen (Gesamtreinheit 99,5 bis 99,999 vol%, vorzugsweise 99,8 bis 99,999 vol%; Anteil an schwererflüchtigen Komponenten 1 bis 10 ppm, vorzugsweise 3 bis 5 ppm). Der hochreine Sauerstoff kann flüssig und/oder gasförmig direkt am Sumpf der Niederdrucksäule abgezogen werden.By removing the insert above the air feed, less volatile components of the air such as hydrocarbons, krypton and xenon are kept away from the low pressure column. A highly pure oxygen product is taken from the bottom thereof (total purity 99.5 to 99.999 vol%, preferably 99.8 to 99.999 vol%; proportion of less volatile components 1 to 10 ppm, preferably 3 to 5 ppm). The high-purity oxygen can be drawn off in liquid and / or gaseous form directly at the bottom of the low-pressure column.

Die Betriebsdrücke der Säulen können bei dem erfindungsgemäßen Verfahren beispielsweise 6 bis 20, vorzugsweise 7 bis 16 bar in der Drucksäule und beispielsweise 3 bis 8, vorzugsweise 3 bis 6 bar in der Niederdrucksäule betragen. Der Kopfkondensator der Niederdrucksäule wird mindestens teilweise mit Sumpfflüssigkeit der Drucksäule als Kältemittel betrieben. Rücklauf für die Drucksäule wird üblicherweise durch einen Kondensator-Verdampfer erzeugt, über den der Kopf der Drucksäule und der Sumpf der Niederdrucksäule in wärmetauschender Verbindung stehen.The operating pressures of the columns can be, for example, 6 to 20, preferably 7 to 16 bar in the pressure column and, for example, 3 to 8, preferably 3 to 6 bar in the low-pressure column in the process according to the invention. The top condenser of the low pressure column is at least partially Bottom liquid of the pressure column operated as a refrigerant. Return for the pressure column is usually generated by a condenser-evaporator, via which the top of the pressure column and the bottom of the low-pressure column are in heat-exchanging connection.

Insbesondere zur Entfernung von Argon kann eine Restfraktion von einer Zwischenstelle der Niederdrucksäule abgezogen werden. Die Restfraktion wird vorzugsweise durch eine Unreinstickstofffraktion gebildet und oberhalb der Stelle der Einspeisung der sauerstoffhaltigen flüssigen Fraktion aus der Drucksäule entnommen.In particular to remove argon, a residual fraction can be drawn off from an intermediate point of the low pressure column. The residual fraction is preferably formed by an impure nitrogen fraction and is removed from the pressure column above the point at which the oxygen-containing liquid fraction is fed in.

Verfahrenskälte kann durch arbeitsleistende Entspannung einer oder mehrerer der folgenden Fraktionen erzeugt werden:

  • Restgas aus dem Verdampfungsraum des Kopfkondensators der Niederdrucksäule
  • Dampf aus dem mittleren Bereich der Niederdrucksäule (beispielsweise obige Restfraktion)
  • Teilstrom der Einsatzluft
  • Stickstoff aus der Drucksäule oder aus der Niederdrucksäule
Process cold can be generated by relieving pressure on one or more of the following fractions:
  • Residual gas from the evaporation chamber of the top condenser of the low pressure column
  • Steam from the middle area of the low pressure column (e.g. above residual fraction)
  • Partial flow of the feed air
  • Nitrogen from the pressure column or from the low pressure column

Im Falle der arbeitsleistenden Entspannung von Luft wird das Turbinenabgas vorzugsweise der Drucksäule zugeführt oder aus dem Verfahren entfernt, beispielsweise durch Vermischen mit einem anderen Reststrom. Die entspannte Luft darf jedenfalls nicht in die Niederdrucksäule eingespeist werden, da dies eine erneute Verunreinreingung durch schwererflüchtige Komponenten bewirken würde.In the case of work-relieving expansion of air, the turbine exhaust gas is preferably fed to the pressure column or removed from the process, for example by mixing with another residual stream. In any case, the relaxed air must not be fed into the low-pressure column, since this would cause renewed contamination by less volatile components.

Mittels Innenverdichtung kann das hochreine Sauerstoffprodukt auf einen Druck gebracht werden, der höher als der Niederdrucksäulendruck ist, indem mindestens ein Teil des Sauerstoffprodukts flüssig aus der Niederdrucksäule herausgeführt und unter einem Druck, der höher als der Betriebsdruck der Niederdrucksäule ist, verdampft wird. Als Heizmittel beim Verdampfen kann beispielsweise entsprechend hoch verdichtete Luft verwendet werden.By means of internal compression, the high-purity oxygen product can be brought to a pressure which is higher than the low-pressure column pressure, in that at least part of the oxygen product is led out of the low-pressure column in liquid form and is evaporated under a pressure which is higher than the operating pressure of the low-pressure column. Correspondingly highly compressed air can, for example, be used as the heating medium during evaporation.

Zur Druckstickstoffgewinnung ist es günstig, wenn eine Stickstofffraktion flüssig aus der Niederdrucksäule oder deren Kopfkondensator entnommen wird und der Druck der Stickstofffraktion in flüssigem Zustand auf einen Wert erhöht wird, der höher als der Betriebsdruck der Niederdrucksäule ist. Auf diese Weise kann - gegebenenfalls zusätzlich zur Direktentnahme von Stickstoff aus der Drucksäule - gasförmiger Stickstoff unter einem Druck gewonnen werden, der höher als der Betriebsdruck der Niederdrucksäule ist. Der flüssig auf Druck gebrachte Stickstoff kann in die Drucksäule zurückgeleitet oder unter Umgehung der Drucksäule in indirektem Wärmeaustausch verdampft werden.For the production of pressurized nitrogen, it is advantageous if a nitrogen fraction is removed in liquid form from the low-pressure column or its top condenser and the pressure of the nitrogen fraction in the liquid state is increased to a value which is higher than the operating pressure of the low-pressure column. In this way, gaseous nitrogen can be obtained under a pressure which is higher than the operating pressure of the low-pressure column, if necessary in addition to the direct removal of nitrogen from the pressure column. The liquid pressurized liquid can be returned to the pressure column or can be evaporated by indirect heat exchange bypassing the pressure column.

Soll dieser Druckstickstoff in besonders hoher Reinheit gewonnen werden, wird die Stickstofffraktion mindestens einen theoretischen oder praktischen Boden unterhalb des Kopfs der Niederdrucksäule entnommen und mindestens ein Teil der flüssigen Stickstofffraktion unter einem Druck, der höher als der Betriebsdruck der Niederdrucksäule ist, durch indirekten Wärmeaustausch verdampft und als hochreines Druckstickstoffprodukt abgeführt. Als Heizmittel bei dem indirekten Wärmeaustausch kann beispielsweise ein Gas aus dem oberen Bereich der Drucksäule und/oder ein Gas aus dem unteren Bereich der Niederdrucksäule verwendet werden. Details über diesen Wärmeaustauschschritt sind den älteren Patentanmeldungen DE 19735154 und WO 98/19122 zu entnehmen. Unter hochreinem Druckstickstoff ist beispielsweise Stickstoff mit einer Gesamtverunreinigung von 1 ppm oder weniger, insbesondere zwischen 1 ppm und 10-3 ppb und unter einem überatmosphärischen Druck, insbesondere von über 3 bar zu verstehen.If this pressure nitrogen is to be obtained in a particularly high purity, the nitrogen fraction is removed from at least one theoretical or practical base below the top of the low pressure column and at least a part of the liquid nitrogen fraction is evaporated by indirect heat exchange under a pressure which is higher than the operating pressure of the low pressure column dissipated as a high-purity pressure nitrogen product. A gas from the upper region of the pressure column and / or a gas from the lower region of the low-pressure column can be used, for example, as the heating means in the indirect heat exchange. Details of this heat exchange step can be found in the older patent applications DE 19735154 and WO 98/19122. High-purity pressure nitrogen is understood to mean, for example, nitrogen with a total contamination of 1 ppm or less, in particular between 1 ppm and 10 -3 ppb and under a superatmospheric pressure, in particular of more than 3 bar.

Der oberhalb der Entnahme der Stickstofffraktion gelegene Abschnitt der Niederdrucksäule dient zur Abtrennung von leichterflüchtigen Verunreinigungen. Dieser Abschnitt kann aus Packungen oder Füllkörpern gebildet sein, deren Stoffaustauschwirkung mindestens einem theoretischen Boden entspricht oder aus einem oder mehreren konventionellen Rektifizierböden, beispielsweise Siebböden. Er kann aus bis zu 10, vorzugsweise aus 2 bis 5 theoretischen beziehungsweise praktischen Böden bestehen. Die leichterflüchtigen Verunreinigungen werden als gasförmige Restfraktion aus dem Verflüssigungsraum des Kopfkondensators der Niederdrucksäule abgezogen.The section of the low-pressure column located above the removal of the nitrogen fraction serves to separate off more volatile impurities. This section can be formed from packings or packing elements, the mass transfer effect of which corresponds to at least one theoretical plate, or from one or more conventional rectifying plates, for example sieve plates. It can consist of up to 10, preferably 2 to 5 theoretical or practical trays. The more volatile impurities are withdrawn as a gaseous residual fraction from the liquefaction space of the top condenser of the low pressure column.

Um die besonders hohe Reinheit der Stickstofffraktion aus der Niederdrucksäule zu erhalten, wird diese nicht in die Drucksäule eingeleitet, sondern durch indirekten Wärmeaustausch verdampft und in unveränderter Konzentration als hochreines Druckstickstoffprodukt entnommen. Das Verdampfen des flüssig auf Druck gebrachten Stickstoffs durch indirekten Wärmeaustausch kann wie oben beschrieben erfolgen.In order to maintain the particularly high purity of the nitrogen fraction from the low-pressure column, it is not introduced into the pressure column, but is evaporated by indirect heat exchange and removed in unchanged concentration as a high-purity pressure nitrogen product. Evaporation of the pressurized liquid nitrogen by indirect heat exchange can be carried out as described above.

Wird ein Teil des in der Drucksäule gewonnenen Stickstoffs als Rücklauf für die Niederdrucksäule eingesetzt, wird diese Stickstoffmenge gewöhnlich am Kopf der Drucksäule abgezogen. Indem der Drucksäule mindestens einen theoretischen oder praktischen Boden unterhalb des Kopfs eine flüssige Rohstickstofffraktion entnommen und an einer Stelle auf die Niederdrucksäule aufgegeben wird, die mindestens einen theoretischen oder praktischen Boden oberhalb der Stelle der Entnahme der flüssigen Stickstofffraktion liegt, kann bereits die Drucksäule zur Abtrennung leichterflüchtiger Verunreinigungen eingesetzt werden. Dadurch ergeben sich Vorteile für die Reinheit des hochreinen Druckstickstoffprodukts.If part of the nitrogen obtained in the pressure column is used as the return for the low pressure column, this amount of nitrogen is usually drawn off at the top of the pressure column. By removing a liquid crude nitrogen fraction from the pressure column at least one theoretical or practical bottom underneath the head and placing it on the low-pressure column at a location that is at least one theoretical or practical bottom above the point where the liquid nitrogen fraction was removed, the pressure column can already be used to separate more volatile substances Impurities are used. This results in advantages for the purity of the high-purity pressure nitrogen product.

Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von hochreinem Sauerstoff gemäß den Patentansprüchen 9 beziehungsweise 10.The invention also relates to a device for obtaining high-purity oxygen according to claims 9 and 10, respectively.

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

Figur 1
ein erstes Ausführungsbeispiel der Erfindung mit gasförmiger und/oder flüssiger Entnahme des hochreinen Sauerstoffprodukts aus der Niederdrucksäule und
Figur 2
eine zweites Ausführungsbeispiel mit Innenverdichtung des Sauerstoffprodukts.
The invention and further details of the invention are explained in more detail below with reference to exemplary embodiments illustrated in the drawings. Here show:
Figure 1
a first embodiment of the invention with gaseous and / or liquid removal of the high-purity oxygen product from the low pressure column and
Figure 2
a second embodiment with internal compression of the oxygen product.

Bei dem Verfahren der Figur 1 wird verdichtete und gereinigte Luft 1 in einem Hauptwärmetauscher 2 abgekühlt und einer Drucksäule 4 unter einem Druck von 14 bar zugeleitet (3). Das Rektifiziersystem weist außerdem eine Niederdrucksäule 5 auf, die mit einem Druck von 5 bar betrieben wird und mit der Drucksäule über einen gemeinsamen Kondensator-Verdampfer (Hauptkondensator) 6 in wärmetauschender Verbindung steht. Ein Teil 8 des am Kopf der Drucksäule entnommenen Stickstoffs 7 wird im Hauptkondensator 6 verflüssigt und über die Leitungen 9 und 10 als Rücklauf auf die Drucksäule aufgegeben. Am Hauptkondensator 6 kann über Leitung 57 ein Restdampf, der insbesondere leichterflüchtige Verunreinigungen wie Helium, Neon und/oder Wasserstoff enthält, entnommen werden. Eine sauerstoffhaltige flüssige Fraktion 411 aus der Drucksäule wird nach Unterkühlung 15 in die Niederdrucksäule 5 eingedrosselt (412).In the method of FIG. 1, compressed and cleaned air 1 is cooled in a main heat exchanger 2 and fed to a pressure column 4 under a pressure of 14 bar (3). The rectification system also has a low pressure column 5, which is operated at a pressure of 5 bar and with the pressure column via a common condenser-evaporator (main condenser) 6 is in heat-exchanging connection. A portion 8 of the nitrogen 7 removed at the top of the pressure column is liquefied in the main condenser 6 and fed via lines 9 and 10 as a return to the pressure column. A residual vapor, which contains in particular more volatile impurities such as helium, neon and / or hydrogen, can be removed from the main condenser 6 via line 57. An oxygen-containing liquid fraction 411 from the pressure column is throttled into the low-pressure column 5 after supercooling 15 (412).

Die Niederdrucksäule 5 weist einen Kopfkondensator 17 auf, in dessen Verflüssigungsraum gasförmiger Stickstoff 18 vom Kopf der Niederdrucksäule 5 kondensiert; das Kondensat 19 wird mindestens teilweise in die Niederdrucksäule zurückgeleitet. Ein Restdampf, der insbesondere leichterflüchtige Verunreinigungen wie Helium, Neon und/oder Wasserstoff enthält, wird bei 51 aus dem Kopfkondensator 17 (wie dargestellt) oder alternativ aus der im Kopfkondensator kondensierten Fraktion 19 entnommen.The low pressure column 5 has a top condenser 17, in the liquefaction space of which gaseous nitrogen 18 condenses from the top of the low pressure column 5; the condensate 19 is at least partially returned to the low pressure column. A residual vapor, which contains in particular more volatile impurities such as helium, neon and / or hydrogen, is withdrawn at 51 from the top condenser 17 (as shown) or alternatively from the fraction 19 condensed in the top condenser.

Erfindungsgemäß wird der Kopfkondensator 17 der Niederdrucksäule 5 nicht oder nicht ausschließlich mit Sumpfflüssigkeit der Niederdrucksäule betrieben (siehe Stand der Technik nach DE 3528374 A1), sondern mit Sumpfflüssigkeit 457 der Drucksäule 4. Die sauerstoffhaltige flüssige Fraktion 411, die in die Niederdrucksäule 5 eingedrosselt (412) wird, stammt von einer Zwischenstelle oberhalb eines zusätzlichen Stoffaustauschabschnitts 458 im unteren Bereich der Drucksäule. Der zusätzliche Stoffaustauschabschnitt 458 weist in dem Beispiel fünf theoretische Böden auf. Im Sumpf der Niederdrucksäule 5 wird ein hochreines Sauerstoffprodukt mit einer Reinheit von 99,99 vol% erzeugt und flüssig (459) und/oder gasförmig (460, 461) unter dem Druck der Niederdrucksäule abgezogen. Über eine Restfraktion (Unreinstickstofffraktion) 462 aus der Niederdrucksäule 5 wird Argon ausgeschleust. Der Unreinstickstoff wird vorzugsweise mit den übrigen Restströmen 31, 57, 51 und 53 vereint.According to the invention, the top condenser 17 of the low-pressure column 5 is not operated or not operated exclusively with bottom liquid of the low-pressure column (see prior art according to DE 3528374 A1), but with bottom liquid 457 of the pressure column 4. The oxygen-containing liquid fraction 411, which is throttled into the low-pressure column 5 (412 ) comes from an intermediate point above an additional mass transfer section 458 in the lower region of the pressure column. The additional mass transfer section 458 has five theoretical plates in the example. In the bottom of the low-pressure column 5, a high-purity oxygen product with a purity of 99.99 vol% is generated and drawn off in liquid (459) and / or gaseous (460, 461) under the pressure of the low-pressure column. Argon is discharged from the low-pressure column 5 via a residual fraction (impure nitrogen fraction) 462. The impure nitrogen is preferably combined with the remaining streams 31, 57, 51 and 53.

Das Ausführungsbeispiel dient außerdem zur Gewinnung von hochreinem Druckstickstoff. Dazu wird unterhalb eines Stoffaustauschabschnitts 54, der in dem Beispiel drei theoretische Böden aufweist, ein Teil der in der Drucksäule 4 herabfließenden Flüssigkeit als flüssige Rohstickstofffraktion 55 entnommen und in den Kopf der Niederdrucksäule 5 eingedrosselt (56).The exemplary embodiment also serves to obtain high-purity pressure nitrogen. For this purpose, a part of that in the pressure column 4 is located below a mass transfer section 54, which in the example has three theoretical plates flowing down liquid taken as a liquid raw nitrogen fraction 55 and throttled in the head of the low pressure column 5 (56).

Nach Durchlaufen eines Stoffaustauschabschnitts 52, der in dem Beispiel drei theoretische Böden aufweist, wird ein Teil der in der Niederdrucksäule 5 herabfließenden Flüssigkeit als Stickstofffraktion 20 entnommen, in flüssigem Zustand auf Druck (im Beispiel 14 bar) gebracht (Pumpe 21) und über Leitung 22 durch den Unterkühler 15 zu einem Produktverdampfer 23 geführt. Der unter einem Druck von 13,4 bar verdampfte Stickstoff 24 wird im Hauptwärmetauscher 2 angewärmt und als hochreines Druckprodukt 25 abgeführt. Er kann gegebenenfalls in gasförmigem Zustand weiter verdichtet werden. In dem Beispiel weist das hochreine Druckstickstoffprodukt 25 eine Gesamtverunreinigung von 10 ppb (einschließlich Kohlenmonoxid) auf. Bei Bedarf kann ein Teil des gasförmigen Stickstoffs 7 vom Kopf der Drucksäule im Hauptwärmetauscher 2 angewärmt und als weiteres Druckprodukt geringerer Reinheit gewonnen werden (nicht dargestellt). In diesem Fall ist es möglich, auf die Überleitung von Flüssigstickstoff 55 aus der Drucksäule 4 in die Niederdrucksäule 5 zu verzichten.After passing through a mass transfer section 52, which in the example has three theoretical plates, part of the liquid flowing down in the low-pressure column 5 is removed as nitrogen fraction 20, brought to pressure in the liquid state (14 bar in the example) (pump 21) and via line 22 through the subcooler 15 to a product evaporator 23. The nitrogen 24 evaporated under a pressure of 13.4 bar is heated in the main heat exchanger 2 and discharged as a high-purity pressure product 25. If necessary, it can be further compressed in the gaseous state. In the example, the high purity pressurized nitrogen product 25 has a total contamination of 10 ppb (including carbon monoxide). If necessary, part of the gaseous nitrogen 7 can be warmed from the top of the pressure column in the main heat exchanger 2 and can be obtained as a further pressure product of lower purity (not shown). In this case, it is possible to dispense with the transfer of liquid nitrogen 55 from the pressure column 4 into the low pressure column 5.

Auf der Verflüssigungsseite des Produktverdampfers 23 wird ein (anderer) Teil 35 des gasförmigen Stickstoffs 7 vom Kopf der Drucksäule 4 kondensiert. Die dabei entstehende Flüssigkeit 36 wird als zusätzlicher Rücklauf auf die Drucksäule 4 aufgegeben. Der Produktverdampfer 23 ist in dem Beispiel als Fallfilmverdampfer ausgebildet, in dem eine nur partielle Verdampfung stattfindet. Flüssig verbliebener Stickstoff 45 wird in die Niederdrucksäule 5 zurückgeführt. Auch am Produktverdampfer 23 wird ein Restdampf, der insbesondere leichterflüchtige Verunreinigungen wie Helium, Neon und/oder Wasserstoff enthält, entnommen (Leitung 53).On the liquefaction side of the product evaporator 23, a (other) part 35 of the gaseous nitrogen 7 is condensed from the top of the pressure column 4. The resulting liquid 36 is added to the pressure column 4 as an additional return. In the example, the product evaporator 23 is designed as a falling film evaporator in which only partial evaporation takes place. Liquid nitrogen 45 is returned to the low pressure column 5. A residual vapor, which in particular contains more volatile impurities such as helium, neon and / or hydrogen, is also removed from the product evaporator 23 (line 53).

Bei Bedarf kann ein Teil der flüssigen Stickstofffraktion 20 aus der Niederdrucksäule als Flüssigprodukt 30 gewonnen werden. Der unreine Sauerstoff 31, der durch Verdampfung der Sumpfflüssigkeit 457 der Drucksäule 5 im Kopfkondensator 17 der Niederdrucksäule entsteht, wird über die Restgasleitung 432 in den Wärmetauschern 14, 15 und 2 angewärmt und als Nebenprodukt oder Restgas abgeführt (27). Er kann beispielsweise für die Regenerierung einer Vorrichtung zur Luftreinigung eingesetzt werden.If necessary, part of the liquid nitrogen fraction 20 can be obtained from the low pressure column as a liquid product 30. The impure oxygen 31, which is created by evaporation of the bottom liquid 457 of the pressure column 5 in the top condenser 17 of the low pressure column, is heated via the residual gas line 432 in the heat exchangers 14, 15 and 2 and removed as a by-product or residual gas (27). It can be used, for example, for the regeneration of an air purification device.

Kälte wird bei dem Verfahren nach Figur 1 durch arbeitsleistende Entspannung 33 des Restgases 432 erzeugt. Die in der Entspannungsmaschine 33 gewonnene mechanische Energie kann beispielsweise zur Nachverdichtung des im Produktverdampfer 23 verdampften Druckstickstoffprodukts 24 oder zur Druckerhöhung im Restgas stromaufwärts der Entspannungsmaschine 33 verwendet werden, vorzugsweise durch direkte mechanische Kopplung von Entspannungsmaschine 33 und einem entsprechenden Verdichter. Es ist günstig, wenn die Restdämpfe 57, 51 und 53 ebenfalls in die Restgasleitung 432 eingeführt werden.In the method according to FIG. 1, cold is generated by expansion 33 of the residual gas 432 which performs work. The mechanical energy obtained in the expansion machine 33 can be used, for example, for the post-compression of the pressurized nitrogen product 24 evaporated in the product evaporator 23 or for increasing the pressure in the residual gas upstream of the expansion machine 33, preferably by direct mechanical coupling of the expansion machine 33 and a corresponding compressor. It is advantageous if the residual vapors 57, 51 and 53 are also introduced into the residual gas line 432.

Insbesondere bei relativ hohem Bedarf an Flüssigprodukt 30 kann zusätzlich oder alternativ zu der in Figur 1 dargestellten Restgasturbine eine Luftturbine eingesetzt werden. Ein Teil der verdichteten und gereinigten Luft 1 wird dabei im Hauptwärmetauscher 2 nur auf eine Zwischentemperatur abgekühlt und anschließend arbeitsleistend entspannt. Die entspannte Luft kann angewärmt und vor den Luftverdichter zurückgeführt werden. Die in der Luftturbine erzeugte mechanische Energie kann zur Nachverdichtung der Luft vor der arbeitsleistenden Entspannung eingesetzt werden.In particular, if there is a relatively high demand for liquid product 30, an air turbine can be used in addition or as an alternative to the residual gas turbine shown in FIG. A part of the compressed and cleaned air 1 is cooled in the main heat exchanger 2 only to an intermediate temperature and then relaxed while performing work. The relaxed air can be warmed up and returned to the air compressor. The mechanical energy generated in the air turbine can be used to recompress the air before relieving work.

Für den Fall, daß das hochreine Sauerstoffprodukt unter einem Druck benötigt wird, der höher als der Betriebsdruck der Niederdrucksäule ist, kann der flüssig aus der Niederdrucksäule abgezogene hochreine Sauerstoff über Leitung 563 einer Flüssigpumpe 562 zugeführt und in einem Produktverdampfer Einsatzluft verdampft werden. In dem Beispiel der Figur 2 dient der Hauptwärmetauscher 2 als Produktverdampfer für den hochreinen Sauerstoff, alternativ könnte ein separater Produktverdampfer vorgesehen sein. Nach (weiterer) Anwärmung im Hauptwärmetauscher 2 wird das Drucksauerstoffprodukt bei 564 abgezogen.In the event that the high-purity oxygen product is required under a pressure which is higher than the operating pressure of the low-pressure column, the high-purity oxygen which has been drawn off liquid from the low-pressure column can be fed via line 563 to a liquid pump 562 and feed air can be evaporated in a product evaporator. In the example in FIG. 2, the main heat exchanger 2 serves as a product evaporator for the high-purity oxygen; alternatively, a separate product evaporator could be provided. After (further) heating in the main heat exchanger 2, the pressurized oxygen product is drawn off at 564.

Claims (10)

Verfahren zur Gewinnung von hochreinem Sauerstoff 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 wird, • eine sauerstoffhaltige flüssige Fraktion (411) aus der Drucksäule (4) entnommen und in die Niederdrucksäule (5) eingespeist wird und • gasförmiger Stickstoff (18) aus der Niederdrucksäule (5) in einem Kopfkondensator (17) durch indirekten Wärmeaustausch mit einer verdampfenden Flüssigkeit (457) mindestens teilweise kondensiert wird,
dadurch gekennzeichnet, daß • die sauerstoffhaltige flüssige Fraktion (411), die in die Niederdrucksäule (5) eingespeist wird, mindestens einen theoretischen oder praktischen Boden oberhalb des Sumpfs der Drucksäule (4) entnommen wird, daß • mindestens ein Teil der Sumpfflüssigkeit (457) der Drucksäule (4) in den Verdampfungsraum des Kopfkondensators (17) der Niederdrucksäule (5) geleitet wird und daß • aus dem unteren Bereich der Niederdrucksäule (5) ein hochreines Sauerstoffprodukt (459, 460, 461, 563, 564) entnommen wird. Process for the production of high-purity oxygen by low-temperature separation of air in a rectification system, which has a pressure column (4) and a low-pressure column (5), the method Feed air (1, 3) is introduced into the pressure column (4), • an oxygen-containing liquid fraction (411) is removed from the pressure column (4) and fed into the low-pressure column (5) and Gaseous nitrogen (18) is at least partially condensed from the low-pressure column (5) in a top condenser (17) by indirect heat exchange with an evaporating liquid (457),
characterized in that • The oxygen-containing liquid fraction (411), which is fed into the low-pressure column (5), at least one theoretical or practical base above the bottom of the pressure column (4) is removed that • at least part of the bottom liquid (457) of the pressure column (4) is passed into the evaporation chamber of the top condenser (17) of the low pressure column (5) and that • A high-purity oxygen product (459, 460, 461, 563, 564) is removed from the lower area of the low-pressure column (5). Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß eine Restfraktion (462) von einer Zwischenstelle der Niederdrucksäule abgezogen wird.A method according to claim 1, characterized in that a residual fraction (462) is withdrawn from an intermediate point of the low pressure column. Verfahren nach Anspruch 1 oder 2, eine gasförmige Fraktion (31) aus dem Verdampfungsraum des Kopfkondensators (17) der Niederdrucksäule und/oder eine gasförmige Fraktion (462) aus der Niederdrucksäule arbeitsleistend entspannt (33) werden.The method of claim 1 or 2, a gaseous fraction (31) from the evaporation chamber of the top condenser (17) of the low-pressure column and / or a gaseous fraction (462) from the low-pressure column are expanded to perform work. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß Luft arbeitsleistend entspannt wird.Method according to one of claims 1 to 3, characterized in that air is expanded to perform work. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß mindestens ein Teil (563) des hochreinen Sauerstoffprodukts flüssig aus der Niederdrucksäule (5) herausgeführt und unter einem Druck, der höher als der Betriebsdruck der Niederdrucksäule (5) ist, verdampft (2) wird.Method according to one of claims 1 to 4, characterized in that at least a part (563) of the high-purity oxygen product is liquid from the Low pressure column (5) led out and evaporated (2) under a pressure which is higher than the operating pressure of the low pressure column (5). Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß eine Stickstofffraktion (20) flüssig aus der Niederdrucksäule (5) oder deren Kopfkondensator (17) entnommen wird und der Druck der Stickstofffraktion (20) in flüssigem Zustand auf einen Wert erhöht (21) wird, der höher als der Betriebsdruck der Niederdrucksäule (5) ist.Method according to one of claims 1 to 5, characterized in that a liquid nitrogen fraction (20) is removed from the low-pressure column (5) or its top condenser (17) and the pressure of the nitrogen fraction (20) increases to a value in the liquid state (21 ), which is higher than the operating pressure of the low pressure column (5). Verfahren nach Anspruch 6, dadurch gekennzeichnet, daß die flüssige Stickstofffraktion (20) mindestens einen theoretischen oder praktischen Boden unterhalb des Kopfs der Niederdrucksäule entnommen und mindestens ein Teil der flüssigen Stickstofffraktion (22) unter einem Druck, der höher als der Betriebsdruck der Niederdrucksäule (5) ist, durch indirekten Wärmeaustausch (23) verdampft und als hochreines Druckstickstoffprodukt (24, 25) abgeführt wird.Method according to claim 6, characterized in that the liquid nitrogen fraction (20) removes at least one theoretical or practical base below the head of the low pressure column and at least a part of the liquid nitrogen fraction (22) under a pressure which is higher than the operating pressure of the low pressure column (5 ) is evaporated by indirect heat exchange (23) and discharged as a high-purity pressure nitrogen product (24, 25). Verfahren nach einem der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß der Drucksäule (4) mindestens einen theoretischen oder praktischen Boden unterhalb des Kopfs eine flüssige Rohstickstofffraktion (55) entnommen und an einer Stelle auf die Niederdrucksäule (5) aufgegeben wird, die mindestens einen theoretischen oder praktischen Boden oberhalb der Stelle der Entnahme der flüssigen Stickstofffraktion (20) liegt.Method according to one of claims 1 to 7, characterized in that a liquid crude nitrogen fraction (55) is taken from the pressure column (4) at least one theoretical or practical base below the head and is added to the low-pressure column (5) at one point, the at least one theoretical or practical soil is above the point of withdrawal of the liquid nitrogen fraction (20). Vorrichtung zur Gewinnung von hochreinem Sauerstoff durch Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das eine Drucksäule (4) und eine Niederdrucksäule (5) aufweist, und mit • einer Einsatzluftleitung (1, 3), die in die Drucksäule (4) führt, • einer Rohsauerstoffleitung (411) zur Einleitung einer sauerstoffhaltigen flüssigen Fraktion aus der Drucksäule (4) in die Niederdrucksäule (5) und mit • einem Kopfkondensator (17) zur mindestens teilweisen Kondensation von gasförmigem Stickstoff (18) aus der Niederdrucksäule (5) durch indirekten Wärmeaustausch mit einer verdampfenden Flüssigkeit (457),
gekennzeichnet durch • einen Stoffaustauschabschnitt (458), der in der Drucksäule (4) unterhalb der Rohsauerstoffleitung (411) und insbesondere oberhalb der Einsatzluftleitung (3) angeordnet ist und mindestens einen theoretischen oder praktischen Boden aufweist, • durch eine Sumpfflüssigkeitsleitung (457) zur Einleitung der Sumpfflüssigkeit der Drucksäule (4) in den Verdampfungsraum des Kopfkondensators (17) der Niederdrucksäule (5) und durch • eine Produktleitung zur Entnahme von hochreinem Sauerstoffprodukt (459, 460, 461, 563, 564) aus dem unteren Bereich der Niederdrucksäule (5). Device for obtaining high-purity oxygen by low-temperature separation of air with a rectification system, which has a pressure column (4) and a low-pressure column (5), and with An emergency air line (1, 3) leading into the pressure column (4), • a raw oxygen line (411) for introducing an oxygen-containing liquid fraction from the pressure column (4) into the low-pressure column (5) and with A top condenser (17) for at least partially condensing gaseous nitrogen (18) from the low pressure column (5) by indirect heat exchange with an evaporating liquid (457),
marked by A mass transfer section (458) which is arranged in the pressure column (4) below the raw oxygen line (411) and in particular above the feed air line (3) and has at least one theoretical or practical base, • by a bottom liquid line (457) for introducing the bottom liquid of the pressure column (4) into the evaporation chamber of the top condenser (17) of the low pressure column (5) and through • A product line for removing high-purity oxygen product (459, 460, 461, 563, 564) from the lower area of the low-pressure column (5). Vorrichtung nach Anspruch 9, gekennzeichnet durch eine Restfraktionsleitung (462, 432), die mit einer Zwischenstelle der Niederdrucksäule (5) verbunden ist.Apparatus according to claim 9, characterized by a residual fraction line (462, 432) which is connected to an intermediate point of the low pressure column (5).
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