EP3327393A1 - Method and device for creating a high purity oxygen product flow by the cryogenic decomposition of air - Google Patents

Method and device for creating a high purity oxygen product flow by the cryogenic decomposition of air Download PDF

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Publication number
EP3327393A1
EP3327393A1 EP16020468.1A EP16020468A EP3327393A1 EP 3327393 A1 EP3327393 A1 EP 3327393A1 EP 16020468 A EP16020468 A EP 16020468A EP 3327393 A1 EP3327393 A1 EP 3327393A1
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EP
European Patent Office
Prior art keywords
column
pure oxygen
mass transfer
oxygen
transfer section
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.)
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EP16020468.1A
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German (de)
French (fr)
Inventor
Dimitri GOLUBEV
Stefan Dowy
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Linde GmbH
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Linde GmbH
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Priority to EP16020468.1A priority Critical patent/EP3327393A1/en
Priority to DE102017010786.6A priority patent/DE102017010786A1/en
Publication of EP3327393A1 publication Critical patent/EP3327393A1/en
Withdrawn legal-status Critical Current

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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
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F25J3/04715—The auxiliary column system simultaneously produces oxygen
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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
    • F25J3/04006—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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    • F25J3/02—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
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    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
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    • F25J2290/44—Particular materials used, e.g. copper, steel or alloys thereof or surface treatments used, e.g. enhanced surface

Definitions

  • the invention relates to a method for obtaining a high-purity oxygen product stream by cryogenic separation of air according to the preamble of patent claim 1.
  • the distillation column system for nitrogen-oxygen separation can be designed as a two-column system (for example as a classic Linde double column system), or as a three or more column system.
  • Fig.2 from US 4977746 a method of the type mentioned above with a classic double column, a classic crude argon column and a pure oxygen column is known, which is connected to the crude argon column.
  • a high purity oxygen product stream can be recovered that is largely free of less volatile components.
  • no oxygen-free crude argon can be obtained in this system, but the simple crude argon column is too short.
  • an oxygen content in the percentage range at the top of the crude argon column can be achieved here;
  • the crude argon column then required two pumps, one from the intermediate point of the crude argon column to the top of the pure oxygen column and one from the bottom of the crude argon column to the low pressure column.
  • the invention is therefore based on the object of obtaining both a high-purity oxygen product stream and oxygen-free crude argon without the need for a particularly complex apparatus.
  • the argon transition stream (the "Argon-enriched stream”) is not introduced as usual in the crude argon column, but in the pure oxygen column, at an intermediate point.
  • the upper mass transfer section of the pure oxygen column above the intermediate point also serves for the removal of methane and less volatile components and the argon-oxygen separation.
  • the feed gas for the crude argon column comes from the top of the pure oxygen column and is already enriched in argon (from 11.3% to 15.3% argon, for example).
  • the crude argon column for the production of oxygen-free Rohargon can be made correspondingly smaller and one-piece.
  • oxygen-free is meant here an oxygen content of less than 10 ppm, preferably less than 1 ppm.
  • methane-free oxygen fraction is simultaneously obtained, which is fed to the pure oxygen mass transfer section of the pure oxygen column, from the bottom of which the high-purity oxygen product stream is withdrawn.
  • This oxygen fraction is referred to below as methane-free.
  • methane-free is meant here a methane content which is below 0.1 ppm, for example below 10 ppb, preferably below 1 ppm.
  • the pure oxygen column can consist of two containers which have the pure oxygen mass transfer section or the upper mass transfer section for hydrocarbon removal.
  • the pure oxygen column is realized as a continuous container, in which the ascending gas is passed without pipelines at the intermediate point. In this way, the Verrohrungsaufwand can be reduced.
  • the upper mass transfer section of the pure oxygen column can be formed by structured packing (also referred to as "ordered packing” in German) and the pure oxygen mass transfer section by conventional rectification trays. In this way, the two corresponding column sections may have the same or similar diameter despite different throughput.
  • a packing density of 350 to 750 m 2 / m 3 is used in the upper mass transfer section.
  • the rectification soils are preferably realized by sieve trays.
  • both the upper mass transfer section of the pure oxygen column and the pure oxygen mass transfer section are formed by structured packing.
  • the packing is then preferably designed as a copper packing, ie the sheets from which the packing is made have a copper content of at least 95 mol%, in particular of at least 99%.
  • the packing density in the pure oxygen mass transfer section (7) of the pure oxygen column (5) is more than 1000 m 2 / m 3 and that in the upper mass transfer section (6) of the pure oxygen column (5) is less than 800 m 2 / m 3 ,
  • the invention also relates to a device according to claim 12.
  • the device according to the invention can be supplemented by device features which correspond to the characteristics of individual, several or all dependent method claims.
  • This double column here forms the distillation column system for nitrogen-oxygen separation. It is classically designed with high-pressure column 1 under a main condenser 2, which is located at the lower end of a low-pressure column 3.
  • a gaseous intermediate fraction from the low-pressure column forms the argon-enriched stream 4 from the distillation column system for nitrogen-oxygen separation and is fed to the pure oxygen column 5 at an intermediate point.
  • the inflowing gas flows into the upper mass transfer section 6 of the pure oxygen column 5, where it is depleted of oxygen and methane.
  • the upper mass transfer section 6 thus simultaneously forms the first section of the argon-oxygen separation which otherwise takes place in the following crude argon column 10. This is applied in the sump with the head gas 9 of the pure oxygen column.
  • the crude argon column 10 has a top condenser 11 in which the overhead gas of the crude argon column is completely liquefied except for the crude argon product stream 12.
  • the raw argon product gas 12 is further processed here in a classical pure argon column 13 with removal of the residual nitrogen.
  • a high purity argon product HLAR is withdrawn via line 14 from the bottom of the pure argon column 13.
  • the bottom liquid 15 of the crude argon column is introduced by means of a pump 16 into the pure oxygen column 5, namely at two different locations.
  • a first part 17 is led to the head of the pure oxygen column 5 and there introduced as reflux liquid to the upper mass transfer section 5;
  • a second part 18 of the bottom liquid 15 of the crude argon column 10 is used as a methane-free liquid oxygen fraction and applied to the top of a pure oxygen mass transfer section 7 of the pure oxygen column 5, which is located below the intermediate point is located at which the argon-enriched stream 4 is introduced from the low-pressure column 3.
  • This liquid forms the reflux in the pure oxygen mass transfer section 7.
  • both mass transfer sections 6, 7 of the pure oxygen column 5 are formed by structured packing, the lower mass transfer section 7 having two packing beds, the upper mass transfer section 6 of a.
  • the upper mass transfer section 6 is operated with a lower packing density (specific surface area) than that under 7.
  • the packing density is, for example, 500 m 2 / m 3 in the upper mass transfer section 6 and 1200 m 2 / m 3 in the lower mass transfer section 7.
  • a "similar column diameter is understood here to mean a difference in column diameters of less than 40%. in which the liquid oxygen or the high purity oxygen product stream are only byproducts of relatively small amount (for example, in a system with internally compressed oxygen as the main product), the difference in the column diameters can also be higher.
  • the top condenser 11 of the crude argon column is conventionally cooled by means of oxygen-enriched bottom liquid 22, 23, 24 from the high-pressure column 1 or the subcooling countercurrent 19.
  • the heating of the sump evaporator 8 of the pure argon column is carried out with a partial flow 25 of the cold feed air 26 under high-pressure column pressure.
  • Atmospheric air AIR is drawn in via a line 27 and a filter 28 from a main air compressor and brought there to a pressure of about 6 bar.
  • the compressed air is cooled in a pre-cooler, which is formed here by a direct contact cooler, and cleaned in a cleaning device, which is formed by a pair of switchable molecular sieve adsorber.
  • the purified high-pressure air 32 is introduced into a main heat exchanger 33 and cooled there to about dew point.
  • the cold feed air 26 flows in gaseous form into the high-pressure column 1 via line 77.
  • a part 25 is used in this embodiment for heating the sump of the pure oxygen column 5.
  • the liquid air 34 from the sump evaporator 8 is introduced via line 35 into the evaporation space of the top condenser 36 of the pure argon column 13.
  • a first part 37 of the top gas of the high-pressure column is liquefied in the main condenser 2.
  • This liquid nitrogen obtained is partly used as reflux in the high pressure column 1, partially withdrawn via line 39, cooled in the subcooling countercurrent 19 and withdrawn via lines 40 and 41 as a high purity liquid nitrogen product HLIN.
  • the remainder 42 of the overhead gas is warmed in the main heat exchanger 33 and fed via line 43 for use as a sealing gas (seal gas).
  • stream 43 may be withdrawn as part of stream 50 from an intermediate location of the high pressure column and warmed in the main heat exchanger.
  • the oxygen-enriched bottom liquid 22, 23 is used in a conventional manner for heating and cooling the pure argon column 13 and for cooling the crude argon column 10. Steam 44 and liquids 45/46 from the respective capacitors are introduced separately into the low-pressure column 3.
  • a somewhat less pure nitrogen liquid 47 having, for example, 1 ppm oxygen content is withdrawn from an intermediate point of the high-pressure column and, after supercooling 19, fed via line 48/49 as reflux liquid to the top of the low-pressure column 3.
  • a gaseous nitrogen stream 50 is withdrawn and fed into a nitrogen cycle consisting of a feed gas compressor 51 with aftercooler 52, a cycle compressor 53 with aftercooler 54, two serial turbine-driven booster 55, 56, with aftercoolers 57, 58, two nitrogen turbines 59, 60, a separator 61 and the left part of the main heat exchanger 33 shown in the drawing consists.
  • the invention works in principle, regardless of the specific design of the high-pressure column - for example, with or without pure nitrogen section - and regardless of the nitrogen cycle and in particular its entry and exit points to the high-pressure column.
  • Liquid generated in the nitrogen cycle is fed on the one hand via line 62 into the high-pressure column, on the other hand via lines 63, 49 into the low-pressure column 3.
  • Gaseous nitrogen 64 from the top of the low-pressure column 3 is heated in the supercooling countercurrent 19 and further (line 65) in the main heat exchanger 33 to about ambient temperature.
  • a first portion 66 of the warm impure nitrogen may be introduced via the feed gas compressor 51 into the circuit; another part 67 serves as a cooling gas for an evaporative cooler 72 for cooling cooling water 73.
  • the gaseous oxygen product 68 from the low-pressure column 3 is mixed here with the residual gas 69 from an intermediate point of the low-pressure column 3.
  • the mixture 70 is warmed in the main heat exchanger and finally used as regeneration gas 71 or blown off into the atmosphere ATM.
  • FIG. 2 is different from this FIG. 1 in that the low-pressure column 3 has an additional mass transfer section between the residual gas outlet 69 and the liquid feed 45.
  • the liquid air 34/235 from the liquefaction space of the bottom evaporator 8 of the pure oxygen column 5 is introduced here into the intermediate point which is thus created.
  • the required process and liquefaction refrigerants are not generated in a nitrogen cycle, but by the work-performing expansion of part of the feed air in one or more turbines.
  • the main products are in this process Oxygen products and not nitrogen products as in the other embodiments, each having a nitrogen cycle.
  • the cold generated thereby is registered for the most part by a liquid air stream 301 in the distillation column system, which is introduced into the high-pressure column 1.
  • a part 302 is removed immediately, cooled in the subcooling countercurrent 319 and introduced via line 303 together with the liquid air 34/235 from the evaporator 8 in the low pressure column.
  • FIG. 4 is again largely identical to FIG. 1 ; However, the sump evaporator 8 of the pure oxygen column 5 is not cooled here with air, but with a portion 451 of the gaseous nitrogen stream 450 from the high-pressure column. The liquid nitrogen 452 obtained in this process is fed via lines 453, 449 into the low-pressure column.
  • FIG. 5 In the lower mass transfer section 507 of the pure oxygen column 5, conventional rectification trays, for example sieve trays, are used, whereas in the embodiments described so far only structured packings were used. In this way, the different load in the upper 6 and lower mass transfer section 507 can be compensated.
  • the packing density in the upper mass transfer section 6 is 500 m 2 / m 3 . Otherwise it is different FIG. 5 not from FIG. 1 ,

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Abstract

Das Verfahren und die Vorrichtung dienen zur Gewinnung eines Hochreinsauerstoffproduktstroms durch Tieftemperaturzerlegung von Luft mit einem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung und einem Zusatzsäulensystem, das eine Rohargonsäule (10) mit Kopfkondensator (11) und eine Reinsauerstoffsäule (5) mit Sumpfverdampfer (8) aufweist. Ein argonangereicherter Strom (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung wird in das Zusatzsäulensystem eingeleitet wird. Ein Rohargonproduktstrom (12) wird vom Kopf der Rohargonsäule (10) abgezogen. Ein Hochreinsauerstoffproduktstrom (90) wird vom Sumpf der Reinsauerstoffsäule (5) abgezogen. Die Reinsauerstoffsäule (5) weist einen Reinsauerstoff-Stoffaustauschabschnitt (7) auf. Der argonangereicherte Strom (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung wird der Reinsauerstoffsäule (5) an einer Zwischenstelle oberhalb des Reinsauerstoff-Stoffaustauschabschnitts (7) zugeführt. Die Reinsauerstoffsäule (5) weist oberhalb der Zwischenstelle einen oberen Stoffaustauschabschnitt (6) zur Argon-Sauerstofftrennung. Kopfgas (9) aus der Reinsauerstoffsäule (5) wird in den Sumpf der Rohargonsäule (10) eingeleitet. Die aus dem oberen Stoffaustauschabschnitt (6) ablaufende Flüssigkeit wird vollständig aus der Reinsauerstoffsäule (5) abgezogen (20). Ein erster Teil (17) der Sumpfflüssigkeit (15) der Rohargonsäule (10) wird zum Kopf der Reinsauerstoffsäule (5) geführt. Ein zweiter Teil der Sumpfflüssigkeit (15) der Rohargonsäule (10) wird als methanfreie flüssige Sauerstofffraktion (18) auf den Kopf des Reinsauerstoff-Stoffaustauschabschnitts (7) der Reinsauerstoffsäule (5) aufgegeben. Mindestens ein Teil des oben aus dem Reinsauerstoff-Stoffaustauschabschnitt (7) austretenden Gases wird in den oberen Stoffaustauschabschnitt (6) eingeleitet.The method and apparatus are for obtaining a high purity oxygen product stream by cryogenic separation of air with a distillation column nitrogen-oxygen separation system and an auxiliary column system comprising a crude argon column (10) with top condenser (11) and a bottom oxygen column (5) with bottom evaporator (8 ) having. An argon-enriched stream (4) from the distillation column system for nitrogen-oxygen separation is introduced into the auxiliary column system. A crude argon product stream (12) is withdrawn from the top of the crude argon column (10). A high purity oxygen product stream (90) is withdrawn from the bottom of the pure oxygen column (5). The pure oxygen column (5) has a pure oxygen mass transfer section (7). The argon-enriched stream (4) from the distillation column nitrogen-oxygen separation system is fed to the pure oxygen column (5) at an intermediate point above the pure oxygen mass transfer section (7). The pure oxygen column (5) has above the intermediate point an upper mass transfer section (6) for argon-oxygen separation. Top gas (9) from the pure oxygen column (5) is introduced into the bottom of the crude argon column (10). The effluent from the upper mass transfer section (6) liquid is completely withdrawn from the pure oxygen column (5) (20). A first part (17) of the bottom liquid (15) of the crude argon column (10) is led to the top of the pure oxygen column (5). A second part of the bottom liquid (15) of the crude argon column (10) is fed as methane-free liquid oxygen fraction (18) to the top of the pure oxygen mass transfer section (7) of the pure oxygen column (5). At least a part of the gas exiting from the pure oxygen mass transfer section (7) above is introduced into the upper mass transfer section (6).

Description

Die Erfindung betrifft ein Verfahren zur Gewinnung eines Hochreinsauerstoffproduktstroms durch Tieftemperaturzerlegung von Luft gemäß dem Oberbegriff des Patentanspruchs 1.The invention relates to a method for obtaining a high-purity oxygen product stream by cryogenic separation of air according to the preamble of patent claim 1.

Verfahren und Vorrichtungen zur Tieftemperaturzerlegung von Luft sind zum Beispiel aus Hausen/Linde, Tieftemperaturtechnik, 2. Auflage 1985, Kapitel 4 (Seiten 281 bis 337 ) oder aus F.G. Kerry, Industrial Gas Handbook: Gas Separation and Purification, Boca Raton: CRC Press, 2006 ; Kapitel 3: Air Separation Technology bekannt.Methods and devices for the cryogenic separation of air are, for example, Hausen / Linde, Cryogenics, 2nd edition 1985, chapter 4 (pages 281 to 337 ) or off FG Kerry, Industrial Gas Handbook: Gas Separation and Purification, Boca Raton: CRC Press, 2006 ; Chapter 3: Air Separation Technology known.

Das Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung kann als Zwei-Säulen-System (zum Beispiel als klassisches Linde-Doppelsäulensystem) ausgebildet sein, oder auch als Drei- oder Mehr-Säulen-System.The distillation column system for nitrogen-oxygen separation can be designed as a two-column system (for example as a classic Linde double column system), or as a three or more column system.

Aus Fig.2 von US 4977746 ist ein Verfahren der eingangs genannten Art mit einer klassischen Doppelsäule, einer klassischen Rohargonsäule und einer Reinsauerstoffsäule bekannt, die mit der Rohargonsäule verbunden ist. Hier kann ein Hochreinsauerstoffproduktstrom gewonnen werden, das weitgehend frei von schwererflüchtigen Komponenten ist. Allerdings kann in diesem System kein sauerstofffreies Rohargon gewonnen werden, dafür ist die einfache Rohargonsäule zu kurz. Hier ist allenfalls ein Sauerstoffgehalt im Prozentbereich am Kopf der Rohargonsäule erreichbar; außerdem benötigte die Rohargonsäule dann zwei Pumpen, eine von der Zwischenstelle der Rohargonsäule zum Kopf der Reinsauerstoffsäule und eine vom Sumpf der Rohargonsäule zur Niederdrucksäule.Out Fig.2 from US 4977746 a method of the type mentioned above with a classic double column, a classic crude argon column and a pure oxygen column is known, which is connected to the crude argon column. Here, a high purity oxygen product stream can be recovered that is largely free of less volatile components. However, no oxygen-free crude argon can be obtained in this system, but the simple crude argon column is too short. At most, an oxygen content in the percentage range at the top of the crude argon column can be achieved here; In addition, the crude argon column then required two pumps, one from the intermediate point of the crude argon column to the top of the pure oxygen column and one from the bottom of the crude argon column to the low pressure column.

Der Erfindung liegt daher die Aufgabe zugrunde, sowohl einen Hochreinsauerstoffproduktstrom als auch sauerstofffreies Rohargon zu gewinnen, ohne dass ein besonders komplexer Apparat notwendig ist.The invention is therefore based on the object of obtaining both a high-purity oxygen product stream and oxygen-free crude argon without the need for a particularly complex apparatus.

Diese Aufgabe wird durch die Merkmale des kennzeichnenden Teils des Patentanspruchs 1 gelöst. Bei der Erfindung wird der Argonübergangsstrom (der "argonangereicherte Strom") nicht wie üblich in die Rohargonsäule eingeleitet, sondern in die Reinsauerstoffsäule, und zwar an einer Zwischenstelle. Der obere Stoffaustauschabschnitt der Reinsauerstoffsäule oberhalb der Zwischenstelle dient gleichzeitig der Entfernung von Methan und schwererflüchtigen Komponenten und der Argon-Sauerstofftrennung. Das Einsatzgas für die Rohargonsäule kommt vom Kopf der Reinsauerstoffsäule und ist bereits weiter an Argon angereichert (von beispielweise 11,3% auf 15,3% Argon).
Die Rohargonsäule zur Herstellung von sauerstofffreiem Rohargon kann dabei entsprechend kleiner und einteilig ausgeführt werden. Unter "sauerstofffrei" wird hier ein Sauerstoffgehalt von weniger als 10 ppm, vorzugsweise weniger als 1 ppm verstanden.This object is solved by the features of the characterizing part of patent claim 1. In the invention, the argon transition stream (the "Argon-enriched stream") is not introduced as usual in the crude argon column, but in the pure oxygen column, at an intermediate point. The upper mass transfer section of the pure oxygen column above the intermediate point also serves for the removal of methane and less volatile components and the argon-oxygen separation. The feed gas for the crude argon column comes from the top of the pure oxygen column and is already enriched in argon (from 11.3% to 15.3% argon, for example).
The crude argon column for the production of oxygen-free Rohargon can be made correspondingly smaller and one-piece. By "oxygen-free" is meant here an oxygen content of less than 10 ppm, preferably less than 1 ppm.

Im Sumpf der Rohargonsäule wird gleichzeitig eine methanfreie Sauerstofffraktion gewonnen, die auf den Reinsauerstoff-Stoffaustauschabschnitt der Reinsauerstoffsäule aufgegeben wird, von dessen Sumpf der Hochreinsauerstoffproduktstrom abgezogen wird. Diese Sauerstofffraktion wird im Weiteren als methanfrei bezeichnet. Unter "methanfrei wird hier ein Methangehalt verstanden, der unter 0,1 ppm, zum Beispiel unter 10 ppb, vorzugsweise unter 1 ppm liegt.In the bottom of the crude argon column, a methane-free oxygen fraction is simultaneously obtained, which is fed to the pure oxygen mass transfer section of the pure oxygen column, from the bottom of which the high-purity oxygen product stream is withdrawn. This oxygen fraction is referred to below as methane-free. By "methane-free" is meant here a methane content which is below 0.1 ppm, for example below 10 ppb, preferably below 1 ppm.

Grundsätzlich kann die Reinsauerstoffsäule aus zwei Behältern bestehen, welche den Reinsauerstoff-Stoffaustauschabschnitt beziehungsweise den oberen Stoffaustauschabschnitt zur Kohlenwasserstoffabtrennung aufweisen. Es ist jedoch günstiger, wenn die Reinsauerstoffsäule als ein durchgehender Behälter realisiert ist, bei dem das aufsteigende Gas ohne Rohrleitungen an der Zwischenstelle vorbeigeführt wird. Auf diese Weise kann der Verrohrungsaufwand vermindert werden.In principle, the pure oxygen column can consist of two containers which have the pure oxygen mass transfer section or the upper mass transfer section for hydrocarbon removal. However, it is more favorable if the pure oxygen column is realized as a continuous container, in which the ascending gas is passed without pipelines at the intermediate point. In this way, the Verrohrungsaufwand can be reduced.

Der obere Stoffaustauschabschnitt der Reinsauerstoffsäule kann durch strukturierte Packung (im Deutschen auch als "geordnete Packung" bezeichnet) und der Reinsauerstoff-Stoffaustauschabschnitt durch konventionelle Rektifizierböden gebildet werden. Auf diese Weise können die beiden entsprechenden Kolonnenabschnitte trotz unterschiedlichen Durchsatzes einen gleichen oder ähnlichen Durchmesser aufweisen. Vorzugsweise wird eine Packungsdichte von 350 bis 750 m2/m3 im oberen Stoffaustauschabschnitt eingesetzt. Die Rektifizierböden werden vorzugsweise durch Siebböden realisiert.The upper mass transfer section of the pure oxygen column can be formed by structured packing (also referred to as "ordered packing" in German) and the pure oxygen mass transfer section by conventional rectification trays. In this way, the two corresponding column sections may have the same or similar diameter despite different throughput. Preferably, a packing density of 350 to 750 m 2 / m 3 is used in the upper mass transfer section. The rectification soils are preferably realized by sieve trays.

Alternativ werden sowohl der obere Stoffaustauschabschnitt der Reinsauerstoffsäule als auch der Reinsauerstoff-Stoffaustauschabschnitt durch strukturierte Packung gebildet. Im Reinsauerstoff-Stoffaustauschabschnitt wird die Packung dann vorzugsweise als Kupferpackung ausgeführt, das heißt die Bleche, aus denen die Packung gefertigt ist, weisen einen Kupfergehalt von mindestens 95 mol-%, insbesondere von mindestens 99% auf.Alternatively, both the upper mass transfer section of the pure oxygen column and the pure oxygen mass transfer section are formed by structured packing. In the pure oxygen mass transfer section, the packing is then preferably designed as a copper packing, ie the sheets from which the packing is made have a copper content of at least 95 mol%, in particular of at least 99%.

Dann ist es günstig, wenn die Packungsdichte (spezifische Oberfläche) im Reinsauerstoff-Stoffaustauschabschnitt der Reinsauerstoffsäule um mindestens den Faktor 1,5 höher als im oberen Stoffaustauschabschnitt ist; der Faktor liegt beispielsweise zwischen 1,5 und 3,4. Die absoluten Packungsdichten betragen beispielsweise:

  • im oberen Stoffaustauschabschnitt: 350 bis 750 m2/m3
  • im Reinsauerstoff-Stoffaustauschabschnitt: 500 bis 1200 m2/m3
Then it is favorable if the packing density (specific surface area) in the pure oxygen mass transfer section of the pure oxygen column is at least a factor of 1.5 higher than in the upper mass transfer section; the factor is for example between 1.5 and 3.4. The absolute packing densities are for example:
  • in the upper mass transfer section: 350 to 750 m 2 / m 3
  • in the pure oxygen mass transfer section: 500 to 1200 m 2 / m 3

Es ist günstig, wenn die Packungsdichte im Reinsauerstoff-Stoffaustauschabschnitt (7) der Reinsauerstoffsäule (5) mehr als 1.000 m2/m3 beträgt, und diejenige im oberen Stoffaustauschabschnitt (6) der Reinsauerstoffsäule (5) weniger als 800 m2/m3.It is favorable if the packing density in the pure oxygen mass transfer section (7) of the pure oxygen column (5) is more than 1000 m 2 / m 3 and that in the upper mass transfer section (6) of the pure oxygen column (5) is less than 800 m 2 / m 3 ,

Die Erfindung betrifft außerdem eine Vorrichtung gemäß Patentanspruch 12. Die erfindungsgemäße Vorrichtung kann durch Vorrichtungsmerkmale ergänzt werden, die den Merkmalen einzelner, mehrerer oder aller abhängigen Verfahrensansprüche entsprechen.The invention also relates to a device according to claim 12. The device according to the invention can be supplemented by device features which correspond to the characteristics of individual, several or all dependent method claims.

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

Figur 1
eine erstes Ausführungsbeispiel der Erfindung mit Ausheizung der Reinsauerstoffsäule mittels Luft und Packungen in der Reinsauerstoffsäule;
Figur 2
ein zweites Ausführungsbeispiel, das einen zusätzlichen Stoffaustauschabschnitt in der Niederdrucksäule des Destillationssäulen-Systems zur Stickstoff-Sauerstoff-Trennung aufweist,
Figur 3
ein drittes Ausführungsbeispiel mit Einleitung flüssiger Luft in die Hochdrucksäule des Destillationssäulen-Systems zur Stickstoff-Sauerstoff-Trennung,
Figur 4
ein viertes Ausführungsbeispiel mit Ausheizung der Reinsauerstoffsäule mit einer Zwischenfraktion der Hochdrucksäule und
Figur 5
ein fünftes Ausführungsbeispiel mit Einsatz von konventionellen Rektifizierböden im Reinsauerstoff-Stoffaustauschabschnitt.
The invention and further details of the invention are explained below with reference to embodiments schematically illustrated in the drawings. Hereby show:
FIG. 1
a first embodiment of the invention with heating of the pure oxygen column by means of air and packings in the pure oxygen column;
FIG. 2
a second embodiment having an additional mass transfer section in the low-pressure column of the nitrogen-oxygen separation distillation column system,
FIG. 3
A third embodiment with introduction of liquid air into the high-pressure column of the distillation column system for nitrogen-oxygen separation,
FIG. 4
a fourth embodiment with heating of the pure oxygen column with an intermediate fraction of the high pressure column and
FIG. 5
a fifth embodiment using conventional rectification soils in the pure oxygen mass transfer section.

Im Folgenden wird zunächst der erfindungswesentliche Teil der Figur 1 beschrieben, der sich in der Zeichnung rechts von der Doppelsäule befindet. Diese Doppelsäule bildet hier das Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung. Sie ist klassisch ausgebildet mit Hochdrucksäule 1 unter einem Hauptkondensator 2, der sich am unteren Ende einer Niederdrucksäule 3 befindet.In the following, the invention essential part of FIG. 1 described in the drawing to the right of the double column. This double column here forms the distillation column system for nitrogen-oxygen separation. It is classically designed with high-pressure column 1 under a main condenser 2, which is located at the lower end of a low-pressure column 3.

Eine gasförmige Zwischenfraktion aus der Niederdrucksäule bildet den argonangereicherten Strom 4 aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung und wird der Reinsauerstoffsäule 5 an einer Zwischenstelle zugeleitet. Das einströmende Gas fließt in den oberen Stoffaustauschabschnitt 6 der Reinsauerstoffsäule 5 und wird dort an Sauerstoff und Methan abgereichert. Der obere Stoffaustauschabschnitt 6 bildet damit gleichzeitig den ersten Abschnitt der Argon-Sauerstoff-Trennung, die ansonsten in der folgenden Rohargonsäule 10 stattfindet. Diese wird im Sumpf mit dem Kopfgas 9 der Reinsauerstoffsäule beaufschlagt. Die Rohargonsäule 10 weist einen Kopfkondensator 11 auf, in der das Kopfgas der Rohargonsäule mit Ausnahme des Rohargonproduktstroms 12 vollständig verflüssigt wird. Das Rohargonproduktgas 12 wird hier in einer klassischen Reinargonsäule 13 unter Abtrennung des Reststickstoffs weiterverarbeitet. Ein hochreines Argonprodukt HLAR wird über Leitung 14 vom Sumpf der Reinargonsäule 13 abgezogen.A gaseous intermediate fraction from the low-pressure column forms the argon-enriched stream 4 from the distillation column system for nitrogen-oxygen separation and is fed to the pure oxygen column 5 at an intermediate point. The inflowing gas flows into the upper mass transfer section 6 of the pure oxygen column 5, where it is depleted of oxygen and methane. The upper mass transfer section 6 thus simultaneously forms the first section of the argon-oxygen separation which otherwise takes place in the following crude argon column 10. This is applied in the sump with the head gas 9 of the pure oxygen column. The crude argon column 10 has a top condenser 11 in which the overhead gas of the crude argon column is completely liquefied except for the crude argon product stream 12. The raw argon product gas 12 is further processed here in a classical pure argon column 13 with removal of the residual nitrogen. A high purity argon product HLAR is withdrawn via line 14 from the bottom of the pure argon column 13.

Die Sumpfflüssigkeit 15 der Rohargonsäule wird mittels einer Pumpe 16 in die Reinsauerstoffsäule 5 eingeleitet, und zwar an zwei verschiedenen Stellen. Ein erster Teil 17 wird zum Kopf der Reinsauerstoffsäule 5 geführt und dort als Rücklaufflüssigkeit auf den oberen Stoffaustauschabschnitt 5 aufgegeben; ein zweiter Teil 18 der Sumpfflüssigkeit 15 der Rohargonsäule 10 wird als methanfreie flüssige Sauerstofffraktion genutzt und auf den Kopf eines Reinsauerstoff-Stoffaustauschabschnitts 7 der Reinsauerstoffsäule 5 aufgegeben, der sich unterhalb der Zwischenstelle befindet, an der der argonangereicherte Strom 4 aus der Niederdrucksäule 3 eingeleitet wird. Diese Flüssigkeit bildet den Rücklauf im Reinsauerstoff-Stoffaustauschabschnitt 7. Die Flüssigkeit, die aus diesem Stoffaustauschabschnitt abläuft wird zu einem ersten Teil im Sumpfverdampfer 8 verdampft und strömt als aufsteigendes Gas zurück in den Reinsauerstoff-Stoffaustauschabschnitt 7 und weiter in den oberen Stoffaustauschabschnitt 6. Der Rest wird flüssig als Hochreinsauerstoffproduktstrom 90 abgezogen und - gegebenenfalls nach Unterkühlung in einem Unterkühlungs-Gegenströmer 19 als flüssiges Hochreinprodukt HLOX gewonnen.The bottom liquid 15 of the crude argon column is introduced by means of a pump 16 into the pure oxygen column 5, namely at two different locations. A first part 17 is led to the head of the pure oxygen column 5 and there introduced as reflux liquid to the upper mass transfer section 5; a second part 18 of the bottom liquid 15 of the crude argon column 10 is used as a methane-free liquid oxygen fraction and applied to the top of a pure oxygen mass transfer section 7 of the pure oxygen column 5, which is located below the intermediate point is located at which the argon-enriched stream 4 is introduced from the low-pressure column 3. This liquid forms the reflux in the pure oxygen mass transfer section 7. The liquid draining from this mass transfer section is vaporized to a first part in the sump evaporator 8 and flows as ascending gas back into the pure oxygen mass transfer section 7 and further into the upper mass transfer section 6. The remainder is withdrawn liquid as Hochreininsauerstoffproduktstrom 90 and - optionally recovered after subcooling in a supercooling countercurrent 19 as a liquid high purity product HLOX.

Die aus dem oberen Stoffaustauschabschnitt der Reinsauerstoffsäule 5 ablaufende Flüssigkeit wird an der Zwischenstelle vollständig durch eine Sammeleinrichtung 21 aufgefangen und über Leitung 20 in die Niederdrucksäule 3 zurückgeleitet.The effluent from the upper mass transfer section of the pure oxygen column 5 liquid is completely collected at the intermediate point by a collecting device 21 and returned via line 20 into the low-pressure column 3.

In dem Ausführungsbeispiel werden beide Stoffaustauschabschnitte 6, 7 der Reinsauerstoffsäule 5 durch strukturierte Packung gebildet, wobei der untere Stoffaustauschabschnitt 7 zwei Packungsbetten aufweist, der obere Stoffaustauschabschnitt 6 eines. Um die unterschiedlichen Belastungen bei ähnlichem oder gleichem Kolonnendurchmesser auszugleichen, wird der obere Stoffaustauschabschnitt 6 mit einer niedrigeren Packungsdichte (spezifischen Oberfläche) als der unter 7 betrieben. Die Packungsdichte beträgt beispielsweise 500 m2/m3 im oberen Stoffaustauschabschnitt 6 und 1.200 m2/m3 im unteren Stoffaustauschabschnitt 7. Unter einem "ähnlichen Kolonnendurchmesser wird hier ein Unterschied in den Kolonnendurchmessern von weniger als 40 % verstanden. Im Falle einer Luftzerlegungsanlage, bei welcher der Flüssigsauerstoff beziehungsweise der Hochreinsauerstoffproduktstrom nur Nebenprodukte relativ geringer Menge sind (beispielsweise bei einer Anlage mit innenverdichtetem Sauerstoff als Hauptprodukt), kann der Unterschied in den Kolonnendurchmessern auch höher ausfallen.In the exemplary embodiment, both mass transfer sections 6, 7 of the pure oxygen column 5 are formed by structured packing, the lower mass transfer section 7 having two packing beds, the upper mass transfer section 6 of a. In order to compensate for the different loads at similar or the same column diameter, the upper mass transfer section 6 is operated with a lower packing density (specific surface area) than that under 7. The packing density is, for example, 500 m 2 / m 3 in the upper mass transfer section 6 and 1200 m 2 / m 3 in the lower mass transfer section 7. A "similar column diameter is understood here to mean a difference in column diameters of less than 40%. in which the liquid oxygen or the high purity oxygen product stream are only byproducts of relatively small amount (for example, in a system with internally compressed oxygen as the main product), the difference in the column diameters can also be higher.

Der Kopfkondensator 11 der Rohargonsäule wird konventionell mittels sauerstoffangereicherter Sumpfflüssigkeit 22, 23, 24 aus der Hochdrucksäule 1 beziehungsweise dem Unterkühlungs-Gegenströmer 19 gekühlt. Die Beheizung des Sumpfverdampfers 8 der Reinargonsäule erfolgt mit einem Teilstrom 25 der kalten Einsatzluft 26 unter Hochdrucksäulendruck.The top condenser 11 of the crude argon column is conventionally cooled by means of oxygen-enriched bottom liquid 22, 23, 24 from the high-pressure column 1 or the subcooling countercurrent 19. The heating of the sump evaporator 8 of the pure argon column is carried out with a partial flow 25 of the cold feed air 26 under high-pressure column pressure.

Nun folgt die Beschreibung des Luftzerlegungsprozesses der Figur 1 im engeren Sinne, der grundsätzlich unabhängig von der Erfindung ist.Now follows the description of the air separation process of FIG. 1 in the narrower sense, which is fundamentally independent of the invention.

Atmosphärische Luft AIR wird über eine Leitung 27 und ein Filter 28 von einem Hauptluftverdichter angesaugt und dort auf einen Druck von etwa 6 bar gebracht. Die verdichtete Luft wird in einer Vorkühleinrichtung, die hier durch einen Direktkontaktkühler gebildet wird, abgekühlt und in einer Reinigungseinrichtung gereinigt, die durch ein Paar umschaltbarer Molsiebadsorber gebildet wird.Atmospheric air AIR is drawn in via a line 27 and a filter 28 from a main air compressor and brought there to a pressure of about 6 bar. The compressed air is cooled in a pre-cooler, which is formed here by a direct contact cooler, and cleaned in a cleaning device, which is formed by a pair of switchable molecular sieve adsorber.

Die gereinigte Hochdruckluft 32 wird in einen Hauptwärmetauscher 33 eingeleitet und dort auf etwa Taupunkt abgekühlt. Die kalte Einsatzluft 26 strömt zum größten Teil über Leitung 77 gasförmig in die Hochdrucksäule 1 ein. Ein Teil 25 wird bei diesem Ausführungsbeispiel für die Beheizung des Sumpfs der Reinsauerstoffsäule 5 eingesetzt. Die flüssige Luft 34 aus dem Sumpfverdampfer 8 wird über Leitung 35 in den Verdampfungsraum des Kopfkondensators 36 der Reinargonsäule 13 eingeleitet.The purified high-pressure air 32 is introduced into a main heat exchanger 33 and cooled there to about dew point. The cold feed air 26 flows in gaseous form into the high-pressure column 1 via line 77. A part 25 is used in this embodiment for heating the sump of the pure oxygen column 5. The liquid air 34 from the sump evaporator 8 is introduced via line 35 into the evaporation space of the top condenser 36 of the pure argon column 13.

Ein erster Teil 37 des Kopfgases der Hochdrucksäule wird im Hauptkondensator 2 verflüssigt. Dabei gewonnener Flüssigstickstoff wird zum Teil als Rücklauf in der Hochdrucksäule 1 eingesetzt, zum Teil über Leitung 39 abgezogen, im Unterkühlungs-Gegenströmer 19 abgekühlt und über die Leitungen 40 und 41 als hochreines Flüssigstickstoffprodukt HLIN abgezogen. Der Rest 42 des Kopfgases wird im Hauptwärmetauscher 33 angewärmt und über Leitung 43 einer Verwendung als Sperrgas (Sealgas) zugeführt. Alternativ kann der Strom 43 als ein Teil des Stroms 50 von einer Zwischenstelle der Hochdrucksäule entnommen und im Hauptwärmetauscher angewärmt werden.A first part 37 of the top gas of the high-pressure column is liquefied in the main condenser 2. This liquid nitrogen obtained is partly used as reflux in the high pressure column 1, partially withdrawn via line 39, cooled in the subcooling countercurrent 19 and withdrawn via lines 40 and 41 as a high purity liquid nitrogen product HLIN. The remainder 42 of the overhead gas is warmed in the main heat exchanger 33 and fed via line 43 for use as a sealing gas (seal gas). Alternatively, stream 43 may be withdrawn as part of stream 50 from an intermediate location of the high pressure column and warmed in the main heat exchanger.

Die sauerstoffangereicherte Sumpfflüssigkeit 22, 23, wird auf konventionelle Weise zur Heizung und Kühlung der Reinargonsäule 13 sowie zur Kühlung der Rohargonsäule 10 eingesetzt. Dampf 44 und Flüssigkeiten 45/46 aus den entsprechenden Kondensatoren werden separat in die Niederdrucksäule 3 eingeleitet.The oxygen-enriched bottom liquid 22, 23 is used in a conventional manner for heating and cooling the pure argon column 13 and for cooling the crude argon column 10. Steam 44 and liquids 45/46 from the respective capacitors are introduced separately into the low-pressure column 3.

Eine etwas weniger reine Stickstoffflüssigkeit 47 mit beispielsweise 1 ppm Sauerstoffgehalt wird von einer Zwischenstelle der Hochdrucksäule abgezogen und nach Unterkühlung 19 über Leitung 48/49 als Rücklaufflüssigkeit auf den Kopf der Niederdrucksäule 3 aufgegeben. An derselben Zwischenstelle der Hochdrucksäule wird ein gasförmiger Stickstoffstrom 50 abgezogen und in einen Stickstoffkreislauf eingespeist, der aus einem Feedgasverdichter 51 mit Nachkühler 52, einem Kreislaufverdichter 53 mit Nachkühler 54, zwei seriellen turbinengetriebenen Nachverdichtern 55, 56, mit Nachkühlern 57, 58, zwei Stickstoffturbinen 59, 60, einem Abscheider 61 und dem in der Zeichnung links dargestellten Teil des Hauptwärmetauschers 33 besteht. Die Erfindung funktioniert jedoch prinzipiell unabhängig von der speziellen Ausführung der Hochdrucksäule - zum Beispiel mit oder ohne Reinstickstoffabschnitt - und unabhängig von dem Sickstoffkreislauf und insbesondere dessen Ein- und Ausspeisestellen an der Hochdrucksäule.A somewhat less pure nitrogen liquid 47 having, for example, 1 ppm oxygen content is withdrawn from an intermediate point of the high-pressure column and, after supercooling 19, fed via line 48/49 as reflux liquid to the top of the low-pressure column 3. At the same intermediate point of the high-pressure column a gaseous nitrogen stream 50 is withdrawn and fed into a nitrogen cycle consisting of a feed gas compressor 51 with aftercooler 52, a cycle compressor 53 with aftercooler 54, two serial turbine-driven booster 55, 56, with aftercoolers 57, 58, two nitrogen turbines 59, 60, a separator 61 and the left part of the main heat exchanger 33 shown in the drawing consists. However, the invention works in principle, regardless of the specific design of the high-pressure column - for example, with or without pure nitrogen section - and regardless of the nitrogen cycle and in particular its entry and exit points to the high-pressure column.

Im Stickstoffkreislauf erzeugte Flüssigkeit wird einerseits über Leitung 62 in die Hochdrucksäule, andererseits über die Leitungen 63, 49 in die Niederdrucksäule 3 eingespeist. Gasförmiger Stickstoff 64 vom Kopf der Niederdrucksäule 3 wird im Unterkühlungs-Gegenströmer 19 und weiter (Leitung 65) im Hauptwärmetauscher 33 auf etwa Umgebungstemperatur angewärmt. Ein erster Teil 66 des warmen Unreinstickstoffs kann über den Feedgasverdichter 51 in den Kreislauf eingeführt werden; ein anderer Teil 67 dient als Kühlgas für einen Verdunstungskühler 72 zur Abkühlung von Kühlwasser 73.Liquid generated in the nitrogen cycle is fed on the one hand via line 62 into the high-pressure column, on the other hand via lines 63, 49 into the low-pressure column 3. Gaseous nitrogen 64 from the top of the low-pressure column 3 is heated in the supercooling countercurrent 19 and further (line 65) in the main heat exchanger 33 to about ambient temperature. A first portion 66 of the warm impure nitrogen may be introduced via the feed gas compressor 51 into the circuit; another part 67 serves as a cooling gas for an evaporative cooler 72 for cooling cooling water 73.

Das gasförmige Sauerstoffprodukt 68 aus der Niederdrucksäule 3 wird hier mit dem Restgas 69 von einer Zwischenstelle der Niederdrucksäule 3 vermischt. Das Gemisch 70 wird im Hauptwärmetauscher angewärmt und schließlich als Regeneriergas 71 verwendet oder in die Atmosphäre ATM abgeblasen.The gaseous oxygen product 68 from the low-pressure column 3 is mixed here with the residual gas 69 from an intermediate point of the low-pressure column 3. The mixture 70 is warmed in the main heat exchanger and finally used as regeneration gas 71 or blown off into the atmosphere ATM.

Figur 2 unterscheidet sich dadurch von Figur 1, dass die Niederdrucksäule 3 einen zusätzlichen Stoffaustauschabschnitt zwischen dem Restgasabzug 69 und der Flüssigzuspeisung 45 aufweist. In die dadurch neu entstehende Zwischenstelle wird hier die Flüssigluft 34 /235 aus dem Verflüssigungsraum des Sumpfverdampfers 8 der Reinsauerstoffsäule 5 eingeleitet. FIG. 2 is different from this FIG. 1 in that the low-pressure column 3 has an additional mass transfer section between the residual gas outlet 69 and the liquid feed 45. The liquid air 34/235 from the liquefaction space of the bottom evaporator 8 of the pure oxygen column 5 is introduced here into the intermediate point which is thus created.

Bei Figur 3 wird im Gegensatz zu den vorbeschriebenen Ausführungsbeispielen die benötigte Verfahrens- und Verflüssigungskälte nicht in einem Stickstoffkreislauf erzeugt, sondern durch die arbeitsleistende Entspannung eines Teils der Einsatzluft in einer oder mehreren Turbinen. Die Hauptprodukte sind in diesem Verfahren Sauerstoffprodukte und nicht Stickstoffprodukte wie in den anderen Ausführungsbeispielen, die jeweils einen Stickstoffkreislauf aufweisen.at FIG. 3 In contrast to the above-described embodiments, the required process and liquefaction refrigerants are not generated in a nitrogen cycle, but by the work-performing expansion of part of the feed air in one or more turbines. The main products are in this process Oxygen products and not nitrogen products as in the other embodiments, each having a nitrogen cycle.

Die dadurch erzeugte Kälte wird zum Großteil durch einen Flüssigluftstrom 301 in das Destillationssäulen-System eingetragen, der in die Hochdrucksäule 1 eingeleitet wird. Ein Teil 302 wird gleich wieder entnommen, im Unterkühlungs-Gegenströmer 319 abgekühlt und über Leitung 303 gemeinsam mit der Flüssigluft 34/235 aus dem Verdampfer 8 in die Niederdrucksäule eingeleitet.The cold generated thereby is registered for the most part by a liquid air stream 301 in the distillation column system, which is introduced into the high-pressure column 1. A part 302 is removed immediately, cooled in the subcooling countercurrent 319 and introduced via line 303 together with the liquid air 34/235 from the evaporator 8 in the low pressure column.

Figur 4 ist wieder weitgehend identisch mit Figur 1 ; der Sumpfverdampfer 8 der Reinsauerstoffsäule 5 wird hier jedoch nicht mit Luft, sondern mit einem Teil 451 des gasförmigen Stickstoffstroms 450 aus der Hochdrucksäule gekühlt. Der hierbei gewonnene Flüssigstickstoff 452 wird über die Leitungen 453, 449 in die Niederdrucksäule eingespeist. FIG. 4 is again largely identical to FIG. 1 ; However, the sump evaporator 8 of the pure oxygen column 5 is not cooled here with air, but with a portion 451 of the gaseous nitrogen stream 450 from the high-pressure column. The liquid nitrogen 452 obtained in this process is fed via lines 453, 449 into the low-pressure column.

In Figur 5 werden im unteren Stoffaustauschabschnitt 507 der Reinsauerstoffsäule 5 konventionelle Rektifizierböden, beispielsweise Siebböden eingesetzt, während bei den bisher beschrieben Ausführungsbeispielen ausschließlich strukturierte Packungen zum Einsatz kamen. Auch auf diese Weise lässt sich die unterschiedliche Belastung im oberen 6 und unteren Stoffaustauschabschnitt 507 ausgleichen. Hier beträgt die Packungsdichte im oberen Stoffaustauschabschnitt 6 500 m2/m3. Ansonsten unterscheidet sich Figur 5 nicht von Figur 1.In FIG. 5 In the lower mass transfer section 507 of the pure oxygen column 5, conventional rectification trays, for example sieve trays, are used, whereas in the embodiments described so far only structured packings were used. In this way, the different load in the upper 6 and lower mass transfer section 507 can be compensated. Here, the packing density in the upper mass transfer section 6 is 500 m 2 / m 3 . Otherwise it is different FIG. 5 not from FIG. 1 ,

Claims (12)

Verfahren zur Gewinnung eines Hochreinsauerstoffproduktstroms durch Tieftemperaturzerlegung von Luft mit einem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung und einem Zusatzsäulensystem, das eine Rohargonsäule (10) mit Kopfkondensator (11) und eine Reinsauerstoffsäule (5) mit Sumpfverdampfer (8) aufweist, wobei - ein argonangereicherter Strom (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung in das Zusatzsäulensystem eingeleitet wird, - ein Rohargonproduktstrom (12) als End- oder Zwischenprodukt vom Kopf der Rohargonsäule (10) abgezogen wird, - ein Hochreinsauerstoffproduktstrom (90) vom Sumpf der Reinsauerstoffsäule (5) abgezogen wird, - die Reinsauerstoffsäule (5) einen Reinsauerstoff-Stoffaustauschabschnitt (7) aufweist und - eine methanfreie flüssige Sauerstofffraktion (18) auf den Kopf des Reinsauerstoff-Stoffaustauschabschnitts (7) der Reinsauerstoffsäule aufgegeben wird, dadurch gekennzeichnet, dass - der argonangereicherte Strom (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung der Reinsauerstoffsäule (5) an einer Zwischenstelle zugeführt wird, - die Reinsauerstoffsäule (5) oberhalb der Zwischenstelle einen oberen Stoffaustauschabschnitt (6) aufweist, der zur Argon-Sauerstofftrennung genutzt wird, - Kopfgas (9) aus der Reinsauerstoffsäule (5) in den Sumpf der Rohargonsäule (10) eingeleitet wird, - die aus dem oberen Stoffaustauschabschnitt (6) ablaufende Flüssigkeit vollständig aus der Reinsauerstoffsäule (5) abgezogen (20) wird, - ein erster Teil (17) der Sumpfflüssigkeit (15) der Rohargonsäule (10) zum Kopf der Reinsauerstoffsäule (5) geführt und dort als Rücklaufflüssigkeit aufgegeben wird, - der Reinsauerstoff-Stoffaustauschabschnitt (7) unterhalb der Zwischenstelle in der Reinsauerstoffsäule (5) angeordnet ist, - ein zweiter Teil der Sumpfflüssigkeit (15) der Rohargonsäule (10) die methanfreie flüssige Sauerstofffraktion (18) bildet und auf den Kopf des Reinsauerstoff-Stoffaustauschabschnitts (7) der Reinsauerstoffsäule (5) aufgegeben wird und - mindestens ein Teil des oben aus dem Reinsauerstoff-Stoffaustauschabschnitt (7) austretenden Gases in den obere Stoffaustauschabschnitt (6) eingeleitet wird. A process for recovering a high purity oxygen product stream by cryogenic separation of air with a nitrogen-oxygen separation distillation column system and an auxiliary column system comprising a crude argon column (10) with top condenser (11) and a pure oxygen column (5) with bottom evaporator (8) - an argon-enriched stream (4) from the distillation column system for nitrogen-oxygen separation is introduced into the additional column system, a crude argon product stream (12) is withdrawn as end product or intermediate product from the top of the crude argon column (10), a high-purity oxygen product stream (90) is withdrawn from the bottom of the pure oxygen column (5), - The pure oxygen column (5) has a pure oxygen mass transfer section (7) and - a methane-free liquid oxygen fraction (18) is added to the top of the pure oxygen mass transfer section (7) of the pure oxygen column, characterized in that the argon-enriched stream (4) is fed from the distillation column system for nitrogen-oxygen separation of the pure oxygen column (5) at an intermediate point, - the pure oxygen column (5) above the intermediate point has an upper mass transfer section (6), which is used for argon-oxygen separation, - head gas (9) from the pure oxygen column (5) is introduced into the bottom of the crude argon column (10), the liquid draining from the upper mass transfer section (6) is completely withdrawn from the pure oxygen column (5) (20), - A first part (17) of the bottoms liquid (15) of the crude argon column (10) to the head of the pure oxygen column (5) and fed there as reflux liquid, the pure oxygen mass transfer section (7) is arranged below the intermediate point in the pure oxygen column (5), - A second part of the bottoms liquid (15) of the crude argon column (10) forms the methane-free liquid oxygen fraction (18) and is fed to the top of the pure oxygen mass transfer section (7) of the pure oxygen column (5) and - At least a portion of the above from the pure oxygen mass transfer section (7) exiting gas is introduced into the upper mass transfer section (6). Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Reinsauerstoffsäule als ein durchgehender Behälter realisiert ist, bei dem das aufsteigende Gas ohne Rohrleitungen an der Zwischenstelle vorbeigeführt wird.A method according to claim 1, characterized in that the pure oxygen column is realized as a continuous container in which the rising gas is passed without pipes at the intermediate point. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass der obere Stoffaustauschabschnitt (6) der Reinsauerstoffsäule durch geordnete Packung und der Reinsauerstoff-Stoffaustauschabschnitt (7) durch konventionelle Rektifizierböden gebildet wird.A method according to claim 1 or 2, characterized in that the upper mass transfer section (6) of the pure oxygen column is formed by parent packing and the pure oxygen mass transfer section (7) by conventional rectification plates. Verfahren nach Anspruch 3, dadurch gekennzeichnet, dass konventionelle Rektifizierböden durch Siebböden gebildet werden.A method according to claim 3, characterized in that conventional rectification soils are formed by sieve plates. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass sowohl der obere Stoffaustauschabschnitt (6) der Reinsauerstoffsäule als auch der Reinsauerstoff-Stoffaustauschabschnitt (7) durch strukturierte Packung gebildet werden.A method according to claim 1 or 2, characterized in that both the upper mass transfer section (6) of the pure oxygen column and the pure oxygen mass transfer section (7) are formed by structured packing. Verfahren nach Anspruch 5, dadurch gekennzeichnet, dass die Packungsdichte im Reinsauerstoff-Stoffaustauschabschnitt (7) der Reinsauerstoffsäule (5) um mindestens den Faktor 1,5 höher als im oberen Stoffaustauschabschnitt (6).A method according to claim 5, characterized in that the packing density in the pure oxygen mass transfer section (7) of the pure oxygen column (5) by at least a factor of 1.5 higher than in the upper mass transfer section (6). Verfahren nach Anspruch 5 oder 6, dadurch gekennzeichnet, dass die Packungsdichte im Reinsauerstoff-Stoffaustauschabschnitt (7) der Reinsauerstoffsäule (5) mehr als 1.000 m2/m3 beträgt.A method according to claim 5 or 6, characterized in that the packing density in the pure oxygen mass transfer section (7) of the pure oxygen column (5) is more than 1,000 m 2 / m 3 . Verfahren nach einem der Ansprüche 5 bis 7, dadurch gekennzeichnet, dass Packungsdichte im oberen Stoffaustauschabschnitt (6) der Reinsauerstoffsäule (5) weniger als 800 m2/m3 beträgt.Method according to one of claims 5 to 7, characterized in that the packing density in the upper mass transfer section (6) of the pure oxygen column (5) is less than 800 m 2 / m 3 . Verfahren nach einem der Ansprüche 1 bis 8, dadurch gekennzeichnet, dass die Rohargonsäule (10) einteilig ausgebildet ist.Method according to one of claims 1 to 8, characterized in that the crude argon column (10) is integrally formed. Verfahren nach einem der Ansprüche 1 bis 9, dadurch gekennzeichnet, dass für den Austausch von Flüssigkeiten innerhalb des Zusatzsäulensystems und zwischen Zusatzsäulensystem und Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung nur eine einzige Pumpe (16) zum Anheben von Sumpfflüssigkeit (15) der Rohargonsäule (10) eingesetzt wird.Method according to one of claims 1 to 9, characterized in that for the exchange of liquids within the Zusatzsäulensystems and between additional column system and distillation column system for nitrogen-oxygen separation, only a single pump (16) for lifting bottom liquid (15) of the crude argon column (10) is used. Verfahren nach einem der Ansprüche 1 bis 10, dadurch gekennzeichnet, dass die Rohargonsäule (10) mindestens 120, insbesondere mindesten 140 theoretische Böden aufweist.Method according to one of claims 1 to 10, characterized in that the crude argon column (10) has at least 120, in particular at least 140 theoretical plates. Vorrichtung zur Gewinnung eines Hochreinsauerstoffproduktstroms durch Tieftemperaturzerlegung von Luft mit - einem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung und - einem Zusatzsäulensystem, das eine Rohargonsäule (10) mit Kopfkondensator (11) und eine Reinsauerstoffsäule (5) mit Sumpfverdampfer (8) aufweist, - Mitteln zum Einleiten eines argonangereicherten Stroms (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung in das Zusatzsäulensystem, - Mitteln zum Abziehen eines Rohargonproduktstroms (12) vom Kopf der Rohargonsäule (10), - Mitteln zum Abziehen eines Hochreinsauerstoffproduktstroms (90) vom Sumpf der Reinsauerstoffsäule (5), - einem Reinsauerstoff-Stoffaustauschabschnitt (7), der in der Reinsauerstoffsäule (5) angeordnet ist und mit - Mitteln zum Aufgeben einer methanfreien flüssigen Sauerstofffraktion (18) auf den Kopf des Reinsauerstoff-Stoffaustauschabschnitts (7) der Reinsauerstoffsäule, dadurch gekennzeichnet, dass - die Mitteln zum Einleiten eines argonangereicherten Stroms (4) aus dem Destillationssäulen-System zur Stickstoff-Sauerstoff-Trennung in das Zusatzsäulensystem mit der Reinsauerstoffsäule (5) an einer Zwischenstelle verbunden sind, wobei die Zwischenstelle oberhalb des Reinsauerstoff-Stoffaustauschabschnitts (7) angeordnet ist, und dass - die Reinsauerstoffsäule (5) oberhalb der Zwischenstelle einen oberen Stoffaustauschabschnitt (6) zur Argon-Sauerstofftrennung aufweist, wobei die Vorrichtung ferner - Mittel zum Einleiten von Kopfgas (9) aus der Reinsauerstoffsäule (5) in den Sumpf der Rohargonsäule (10), - Mittel zum vollständigen Abziehen aus der Reinsauerstoffsäule (5) der aus dem oberen Stoffaustauschabschnitt (6) ablaufenden Flüssigkeit, - Mittel zum Aufgeben eines ersten Teils (17) der Sumpfflüssigkeit (15) der Rohargonsäule (10) auf den Kopf der Reinsauerstoffsäule (5), - Mittel zum Aufgeben eines zweiten Teils der Sumpfflüssigkeit (15) der Rohargonsäule (10) als die methanfreie flüssige Sauerstofffraktion (18) auf den Kopf des Reinsauerstoff-Stoffaustauschabschnitts (7) der Reinsauerstoffsäule (5) und - Mittel zum Einleiten mindestens eines Teils des oben aus dem Reinsauerstoff-Stoffaustauschabschnitt (7) austretenden Gases in den obere Stoffaustauschabschnitt (6) aufweist.Apparatus for recovering a high purity oxygen product stream by cryogenic separation of air with - A distillation column system for nitrogen-oxygen separation and - An additional column system comprising a crude argon column (10) with top condenser (11) and a pure oxygen column (5) with bottom evaporator (8), Means for introducing an argon-enriched stream (4) from the distillation column system for nitrogen-oxygen separation in the additional column system, Means for withdrawing a crude argon product stream (12) from the top of the crude argon column (10), Means for withdrawing a high purity oxygen product stream (90) from the bottom of the pure oxygen column (5), - A pure oxygen mass transfer section (7), which is arranged in the pure oxygen column (5) and with - means for adding a methane-free liquid oxygen fraction (18) to the top of the pure oxygen mass transfer section (7) of the pure oxygen column, characterized in that - The means for introducing an argon-enriched stream (4) from the distillation column system for nitrogen-oxygen separation in the additional column system with the pure oxygen column (5) at an intermediate point are connected, wherein the intermediate point above the pure oxygen mass transfer section (7) is arranged, and that - the pure oxygen column (5) above the intermediate point has an upper mass transfer section (6) for argon-oxygen separation, the device further - means for introducing head gas (9) from the pure oxygen column (5) into the bottom of the crude argon column (10), - Means for complete removal from the pure oxygen column (5) of the effluent from the upper mass transfer section (6) liquid, - means for applying a first part (17) of the bottom liquid (15) of the crude argon column (10) to the top of the pure oxygen column (5), - Means for applying a second part of the bottom liquid (15) of the crude argon column (10) as the methane-free liquid oxygen fraction (18) to the head of the pure oxygen mass transfer section (7) of the pure oxygen column (5) and Means for introducing at least part of the gas leaving the top of the pure oxygen mass transfer section (7) into the upper mass transfer section (6) having.
EP16020468.1A 2016-11-25 2016-11-25 Method and device for creating a high purity oxygen product flow by the cryogenic decomposition of air Withdrawn EP3327393A1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021078405A1 (en) * 2019-10-23 2021-04-29 Linde Gmbh Method and system for low-temperature air separation
WO2021204424A3 (en) * 2020-04-09 2021-12-02 Linde Gmbh Process for cryogenic fractionation of air, air fractionation plant and integrated system composed of at least two air fractionation plants
WO2023030679A1 (en) * 2021-09-01 2023-03-09 Linde Gmbh Method for the low-temperature separation of air and air separation plant
WO2024052279A1 (en) * 2022-09-06 2024-03-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Air separation unit and air separation method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0299364A2 (en) * 1987-07-09 1989-01-18 Linde Aktiengesellschaft Process and apparatus for air separation by rectification
US4977746A (en) 1989-01-20 1990-12-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and plant for separating air and producing ultra-pure oxygen
EP0467395A1 (en) * 1990-07-20 1992-01-22 Praxair Technology, Inc. Variable density structured packing cryogenic distillation system
DE10152356A1 (en) * 2001-10-24 2002-12-12 Linde Ag Recovering argon in a low temperature decomposition comprises removing an oxygen fraction deficient in volatile components from an intermediate point of a rectification section and fed to a pure oxygen column
EP3067649A1 (en) * 2015-03-13 2016-09-14 Linde Aktiengesellschaft Distillation column system and method for the production of oxygen by cryogenic decomposition of air

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0299364A2 (en) * 1987-07-09 1989-01-18 Linde Aktiengesellschaft Process and apparatus for air separation by rectification
US4977746A (en) 1989-01-20 1990-12-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and plant for separating air and producing ultra-pure oxygen
EP0467395A1 (en) * 1990-07-20 1992-01-22 Praxair Technology, Inc. Variable density structured packing cryogenic distillation system
DE10152356A1 (en) * 2001-10-24 2002-12-12 Linde Ag Recovering argon in a low temperature decomposition comprises removing an oxygen fraction deficient in volatile components from an intermediate point of a rectification section and fed to a pure oxygen column
EP3067649A1 (en) * 2015-03-13 2016-09-14 Linde Aktiengesellschaft Distillation column system and method for the production of oxygen by cryogenic decomposition of air

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Megapur-Produktion in der Luftzerlegungsanlage Frankfurt", GAS AKTUELL, MESSER GRIESHEIM,. KREFELD, DE, vol. 39, 1 January 1990 (1990-01-01), pages 4 - 8, XP009143412, ISSN: 0340-6067 *
"PROCESS AND FACILITY WITH PARTICULARLY HIGH AVAILABILITY", NOT KNOWN, MASON PUBLICATIONS, HAMPSHIRE, GB, no. 397, 1 May 1997 (1997-05-01), pages 276 - 279, XP000726402, ISSN: 0374-4353 *
F.G. KERRY: "Industrial Gas Handbook: Gas Separation and Purification", 2006, CRC PRESS, article "Air Separation Technology bekannt"
HAUSEN; LINDE: "Tieftemperaturtechnik", 1985, pages: 281 - 337

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2021078405A1 (en) * 2019-10-23 2021-04-29 Linde Gmbh Method and system for low-temperature air separation
WO2021204424A3 (en) * 2020-04-09 2021-12-02 Linde Gmbh Process for cryogenic fractionation of air, air fractionation plant and integrated system composed of at least two air fractionation plants
WO2023030679A1 (en) * 2021-09-01 2023-03-09 Linde Gmbh Method for the low-temperature separation of air and air separation plant
WO2024052279A1 (en) * 2022-09-06 2024-03-14 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Air separation unit and air separation method

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