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EP2312248A1 - Method and device for obtaining pressurised oxygen and krypton/xenon - Google Patents

Method and device for obtaining pressurised oxygen and krypton/xenon Download PDF

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Publication number
EP2312248A1
EP2312248A1 EP09012681A EP09012681A EP2312248A1 EP 2312248 A1 EP2312248 A1 EP 2312248A1 EP 09012681 A EP09012681 A EP 09012681A EP 09012681 A EP09012681 A EP 09012681A EP 2312248 A1 EP2312248 A1 EP 2312248A1
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EP
European Patent Office
Prior art keywords
oxygen
fraction
krypton
xenon
column
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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Application number
EP09012681A
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German (de)
French (fr)
Inventor
Gerhard Pompl
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Linde GmbH
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Linde GmbH
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Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to EP09012681A priority Critical patent/EP2312248A1/en
Publication of EP2312248A1 publication Critical patent/EP2312248A1/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Withdrawn legal-status Critical Current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
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04745—Krypton and/or Xenon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/34—Processes or apparatus using separation by rectification using a side column fed by a stream from the low pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94—Details relating to the withdrawal point
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen

Definitions

  • the invention relates to a method of obtaining pressure oxygen and krypton / xenon according to the preamble of patent claim 1.
  • EP 1139046 A1 EP 1146301 A1 .
  • DE 10213212 A1 DE 10213211 A1 .
  • EP 1357342 A1 or DE 10238282 A1 DE 10302389 A1 .
  • DE 10332863 A1 EP 1544559 A1 .
  • EP 1666824 A1 or EP 1672301 A1 ,
  • the bottoms fraction of the low-pressure column (the second oxygen fraction) is introduced into a krypton-xenon enrichment column (methane discharge column), at the head of which krypton / xenon-poor liquid oxygen is fed.
  • methane discharge column krypton-xenon enrichment column
  • the bottom product of the methane discharge column contains only very small amounts of methane and is enriched in krypton and xenon.
  • the crude krypton-xenon mixture obtained here (the "krypton- and / or xenon-enriched fraction") has a krypton content of 0.1 mol% to 1.0 mol%, preferably 0.5 mol% to 0, 8 mol% and a xenon content of 0.008 mol% to 0.1 mol%, preferably 0.04 mol% to 0.06 mol%.
  • the remainder of the mixture consists predominantly of oxygen with minor amounts of nitrogen, argon, methane and traces of C 2 H 6 , C 2 H 4 , C 3 H 8 , CO 2 and N 2 O.
  • This mixture is the starting product for production from pure krypton in several stages to purities of 99.9999%.
  • the invention is therefore based on the object to provide a method of the type mentioned above and a corresponding device which are more flexible than the known used and or apparatus and / or operationally particularly favorable.
  • both oxygen fractions - the first forming the pressure oxygen product and the second serving as the insert for the krypton-xenon enrichment column - are taken together from the low-pressure column, brought to the elevated pressure and initially only partially evaporated.
  • the two-phase mixture from the partial evaporation is introduced into a separator (phase separator).
  • the liquid phase contains most of the heavier than volatile components, in particular krypton and xenon.
  • the krypton and xenon content of the gas phase is very low, for example less than 1.4 ppm, preferably less than 0.9 ppm krypton and less than 0.06 ppm, preferably less than 0.02 ppm xenon.
  • the gaseous portion is then heated from about the boiling point to near ambient temperature and then forms the pressure oxygen product with which virtually no krypton and xenon is lost.
  • a particularly high yield can be achieved with manageable additional expenditure, for example over 70% krypton yield and over 85% xenon yield.
  • the krypton-xenon enrichment column can be operated at reduced conversion or temporarily shut down completely without affecting pressure oxygen recovery.
  • the excess liquid fraction from the separator is in this case passed by the krypton-xenon recovery and further treated at a suitable point in the process.
  • the inventive method works particularly well at relatively low oxygen product pressures, so if the "increased pressure", for example, between 10 and 30 bar.
  • At least a portion of the third oxygen fraction downstream of the separator is introduced into the krypton-xenon enrichment column as a second oxygen fraction.
  • the introduction can be direct or indirect (for example via the low-pressure column); the third oxygen fraction (or the corresponding part) is utilized in both cases in the krypton-xenon enrichment column.
  • At least a portion of the third oxygen fraction downstream of the precipitator may be returned to the low pressure column.
  • This liquid, which has been returned to the low-pressure column, can likewise be withdrawn again from the low-pressure column at the same or an adjacent location and introduced into the krypton-xenon enrichment column.
  • the corresponding portion of the third oxygen fraction is indirectly fed to the krypton-xenon enrichment column.
  • the krypton-xenon recovery can be formed switchable in the inventive method by at least a portion of the third oxygen fraction downstream of the separator is introduced directly or indirectly into the krypton-xenon enrichment column in a first mode of operation and in a second mode of operation, the entire liquid fraction from the separator past the krypton-xenon enrichment column.
  • the first mode of operation thus corresponds to the normal mode, the second mode of operation of a mode with deactivated krypton-xenon recovery.
  • the first and third oxygen fractions are preferably taken together at least one practical or theoretical tray above the bottom of the low pressure column. Thus they contain compared to the bottoms liquid reduced proportion of krypton and xenon.
  • the second oxygen fraction is preferably taken from the low-pressure column at least one practical or theoretical bottom below the extraction point of the first and third oxygen fraction, in particular from the bottom thereof. Thus, it has a particularly high krypton and xenon content. Between the sampling points of the first and third oxygen fraction on the one hand and On the other hand, the second oxygen fraction is, for example, one to five, preferably two to three, theoretical or practical soils.
  • the invention also relates to a device according to claims 7 to 10.
  • Compressed and prepurified feed air 1 is cooled in a main heat exchanger 2 and optionally partially liquefied and fed via line 3 to a rectification system (feed not shown), which has a double column 4 for nitrogen-oxygen separation and a krypton-xenon enrichment column 5.
  • the double column consists of a high pressure column 6, a low pressure column 7 and a main condenser 8.
  • the feed air is at least partially fed into the high pressure column (not shown) and separated there into liquid crude oxygen 9 and gaseous overhead nitrogen.
  • the top nitrogen is at least partially condensed in the main condenser 8.
  • a portion 10 of the resulting liquid nitrogen is introduced into the low-pressure column 7, as well as the raw oxygen 9. From the lower region of the low-pressure column 7, two oxygen streams 11, 12 taken liquid, with three practical trays are arranged between the two sampling points.
  • the first oxygen stream 11 contains the first and the third oxygen fraction in the sense of the invention. These two are common across the lines 16, 17, and 18th passed through a pump 19 and the lower (cold) region of the main heat exchanger 2 and finally via a control valve 20 which causes no appreciable pressure loss, introduced into a separator (phase separator) 21.
  • the gaseous fraction forms the first oxygen fraction 22 and is reintroduced into the main heat exchanger 2 at about the same temperature where it is warmed to approximately ambient temperature and finally withdrawn via line 23 as gaseous pressure oxygen product.
  • the liquid fraction from the separator 21 forms the third oxygen fraction 24 and, in the example, is returned via line 32 completely to the bottom of the low-pressure column 7.
  • Another portion of the first oxygen stream 11 forms a fourth oxygen fraction 25 and is fed as reflux liquid to the top of the krypton-xenon enrichment column.
  • the second oxygen stream 12 forms the second oxygen fraction which is introduced further down into the krypton-xenon enrichment column 5 in the example immediately above the sump.
  • the krypton-xenon enrichment column is heated by means of a bottom evaporator 26. Gaseous oxygen 27 from the head of the krypton-xenon enrichment column is returned to the low pressure column 7. From the bottom of the krypton-xenon enrichment column, a krypton- and / or xenon-enriched fraction 28 is withdrawn liquid, which otherwise contains mainly oxygen. It can be processed in further steps to a pure krypton product and / or to a pure xenon product.
  • the line 31 is optional.
  • part of the third oxygen fraction 24, which otherwise flows via the lines 32 and 12 can bypass the low-pressure column as a second oxygen fraction into the krypton-xenon enrichment column 5 are initiated.
  • HAC hand indication and control.
  • the entire second oxygen fraction that is to say the feed stream for the lower region of the krypton-xenon enrichment column 5, can also be conducted via the line 31; In this case, the line 12 can be omitted.

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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

The method involves feeding compressed and pre-cleaned feed air (1) into a rectifier system. An oxygen fraction (24) together with another oxygen fraction (22) is removed from a low pressure column (7), brought into high pressure and partially evaporated. The fractions are separated into gaseous portion and liquid portion in a separator (21). The latter fraction is formed by a part of the gaseous portion, heated and conveyed as a gaseous pressurized oxygen product. The former fraction is formed by the liquid portion and fed back into the rectifier system. An independent claim is also included for a device for obtaining pressurized oxygen and krypton/xenon.

Description

Die Erfindung betrifft ein Verfahren Gewinnung von Drucksauerstoff und Krypton/Xenon gemäß dem Oberbegriff des Patentanspruchs 1.The invention relates to a method of obtaining pressure oxygen and krypton / xenon according to the preamble of patent claim 1.

In diesem Verfahren werden die Erzeugung von gasförmigem Drucksauerstoff durch die so genannte Innenverdichtung und die Erzeugung eines Krypton-Xenon-Konzentrats in einer Krypton-Xenon-Anreicherungssäule kombiniert.In this process, the production of gaseous pressure oxygen is combined by the so-called internal compression and the production of a krypton-xenon concentrate in a krypton-xenon enrichment column.

Innenverdichtungsverfahren sind zum Beispiel bekannt aus DE 830805 , DE 901542 (= US 2712738 / US 2784572 ), DE 952908 , DE 1103363 (= US 3083544 ), DE 1112997 (= US 3214925 ), DE 1124529 , DE 1117616 (= US 3280574 ), DE 1226616 (= US 3216206 ), DE 1229561 (= US 3222878 ), DE 1199293 , DE 1187248 (= US 3371496 ), DE 1235347 , DE 1258882 (= US 3426543 ), DE 1263037 (= US 3401531 ), DE 1501722 (= US 3416323 ), DE 1501723 (= US 3500651 ), DE 2535132 (= US 4279631 ), DE 2646690 , EP 93448 B1 (= US 4555256 ), EP 384483 B1 (= US 5036672 ), EP 505812 B1 (= US 5263328 ), EP 716280 B1 (= US 5644934 ), EP 842385 B1 (= US 5953937 ), EP 758733 B1 (= US 5845517 ), EP 895045 B1 (= US 6038885 ), DE 19803437 A1 , EP 949471 B1 (= US 6185960 B1 ), EP 955509 A1 (= US 6196022 B1 ), EP 1031804 A1 (= US 6314755 ), DE 19909744 A1 , EP 1067345 A1 (= US 6336345 ), EP 1074805 A1 (= US 6332337 ), DE 19954593 A1 , EP 1134525 A1 (= US 6477860 ), DE 10013073 A1 , EP 1139046 A1 , EP 1146301 A1 , EP 1150082 A1 , EP 1213552 A1 , DE 10115258 A1 , EP 1284404 A1 (= US 2003051504 A1 ), EP 1308680 A1 (= US 6612129 B2 ), DE 10213212 A1 , DE 10213211 A1 , EP 1357342 A1 oder DE 10238282 A1 DE 10302389 A1 , DE 10334559 A1 , DE 10334560 A1 , DE 10332863 A1 , EP 1544559 A1 , EP 1585926 A1 , DE 102005029274 A1 EP 1666824 A1 , oder EP 1672301 A1 .Internal compression methods are known, for example DE 830805 . DE 901542 (= US 2712738 / US 2784572 ) DE 952908 . DE 1103363 (= US 3,083,544 ) DE 1112997 (= US 3214925 ) DE 1124529 . DE 1117616 (= US 3280574 ) DE 1226616 (= US 3216206 ) DE 1229561 (= US 3222878 ) DE 1199293 . DE 1187248 (= US 3371496 ) DE 1235347 . DE 1258882 (= US 3426543 ) DE 1263037 (= US 3401531 ) DE 1501722 (= US 3,416,323 ) DE 1501723 (= US 3,500,651 ) DE 2535132 (= US 4279631 ) DE 2646690 . EP 93448 B1 (= US 4555256 ) EP 384483 B1 (= US 5036672 ) EP 505812 B1 (= US 5263328 ) EP 716280 B1 (= US 5644934 ) EP 842385 B1 (= US 5953937 ) EP 758733 B1 (= US 5845517 ) EP 895045 B1 (= US 6038885 ) DE 19803437 A1 . EP 949471 B1 (= US 6,189,960 B1 ) EP 955509 A1 (= US 6196022 B1 ) EP 1031804 A1 (= US 6314755 ) DE 19909744 A1 . EP 1067345 A1 (= US 6336345 ) EP 1074805 A1 (= US 6332337 ) DE 19954593 A1 . EP 1134525 A1 (= US 6477860 ) DE 10013073 A1 . EP 1139046 A1 . EP 1146301 A1 . EP 1150082 A1 . EP 1213552 A1 . DE 10115258 A1 . EP 1284404 A1 (= US 2003051504 A1 ) EP 1308680 A1 (= US 6612129 B2 ) DE 10213212 A1 . DE 10213211 A1 . EP 1357342 A1 or DE 10238282 A1 DE 10302389 A1 . DE 10334559 A1 . DE 10334560 A1 . DE 10332863 A1 . EP 1544559 A1 . EP 1585926 A1 . DE 102005029274 A1 EP 1666824 A1 , or EP 1672301 A1 ,

Bei den bisher bekannten Methoden zur Krypton-/Xenon-Gewinnung wird die Sumpffraktion der Niederdrucksäule (die zweite Sauerstofffraktion) in eine Krypton-Xenon-Anreicherungssäule (Methan-Ausschleussäule) eingeleitet, auf deren Kopf Krypton-/Xenon-armer Flüssigsauerstoff aufgegeben wird. Damit kann das Methan, das sich im Sumpf der Niederdrucksäule ansammelt über das gasförmige Kopfprodukt der Methan-Ausschleussäule aus dem Verfahren entfernt werden. Das Sumpfprodukt der Methan-Ausschleussäule enthält nur noch äußerst geringe Mengen an Methan und ist an Krypton und Xenon angereichert. Es kann entweder direkt aus der Methan-Ausschleussäule als Krypton-/Xenon-Vorkonzentrat abgezogen oder in die Niederdrucksäule zurückgeleitet und von dort als Vorkonzentrat abgezogen werden. Diese Verfahrensweise ist an sich bekannt und beispielsweise in Hausen/Linde, Tieftemperaturtechnik, 2. Auflage, 1985, Seiten 337 ff . beschrieben. Das hierbei gewonnene Roh-Krypton-Xenon-Gemisch (die "krypton- und/oder xenonangereicherte Fraktion") weist einen Kryptonanteil von 0,1 mol-% bis 1,0 mol-%, bevorzugt 0,5 mol-% bis 0,8 mol-% und einen Xenonanteil von 0,008 mol-% bis 0,1 mol-% bevorzugt 0,04 mol-% bis 0,06 mol-% auf. Der Rest des Gemisches besteht überwiegend aus Sauerstoff mit kleineren Anteilen an Stickstoff, Argon, Methan und Spuren von C2H6, C2H4, C3H8, CO2 und N2O. Dieses Gemisch ist das Ausgangsprodukt für die Produktion von Rein-Krypton in mehreren Stufen bis zu Reinheiten von 99,9999%.In the hitherto known methods for krypton / xenon recovery, the bottoms fraction of the low-pressure column (the second oxygen fraction) is introduced into a krypton-xenon enrichment column (methane discharge column), at the head of which krypton / xenon-poor liquid oxygen is fed. Thus, the methane that accumulates in the bottom of the low pressure column on the gaseous overhead product the methane discharge column are removed from the process. The bottom product of the methane discharge column contains only very small amounts of methane and is enriched in krypton and xenon. It can either be withdrawn directly from the methane discharge column as Krypton- / xenon preconcentrate or returned to the low pressure column and withdrawn from there as Vorkonzentrat. This procedure is known per se and, for example, in Hausen / Linde, Low Temperature Technology, 2nd edition, 1985, pages 337 ff , described. The crude krypton-xenon mixture obtained here (the "krypton- and / or xenon-enriched fraction") has a krypton content of 0.1 mol% to 1.0 mol%, preferably 0.5 mol% to 0, 8 mol% and a xenon content of 0.008 mol% to 0.1 mol%, preferably 0.04 mol% to 0.06 mol%. The remainder of the mixture consists predominantly of oxygen with minor amounts of nitrogen, argon, methane and traces of C 2 H 6 , C 2 H 4 , C 3 H 8 , CO 2 and N 2 O. This mixture is the starting product for production from pure krypton in several stages to purities of 99.9999%.

Verfahren zur Krypton-Xenon-Gewinnung mit Krypton-Xenon-Anreicherungssäule sind außerdem bekannt aus EP 1757884 A2 , DE 10332862 A1 , DE 10332863 A1 , EP 1482266 A1 , DE 10334559 A1 , DE 10248656 A1 , DE 10232430 A1 , EP 1376037 B1 , EP 1308680 B1 , DE 10000017 A1 , EP 1006326 B1 , DE 19855485 A1 , DE 19855486 A1 , EP 1102954 B1 , EP 1082577 B1 und DE 4332870 C2 .Methods for krypton-xenon recovery with krypton-xenon enrichment column are also known EP 1757884 A2 . DE 10332862 A1 . DE 10332863 A1 . EP 1482266 A1 . DE 10334559 A1 . DE 10248656 A1 . DE 10232430 A1 . EP 1376037 B1 . EP 1308680 B1 . DE 10000017 A1 . EP 1006326 B1 . DE 19855485 A1 . DE 19855486 A1 . EP 1102954 B1 . EP 1082577 B1 and DE 4332870 C2 ,

Unter diesen zeigen auch einige die Kombination von Innenverdichtung und Krypton-Xenon-Gewinnung gemäß dem Oberbegriff, insbesondere DE 10232430 A1 , EP 1308680 B1 und EP 1006326 B1 . Alle diese bekannten Prozesse versuchen, mittels spezieller Maßnahmen zu verhindern, dass ein nennenswerter Teil des in der Einsatzluft enthaltenen Kryptons und Xenons mit dem Drucksauerstoffprodukt verloren gehen. Allerdings sind diese speziellen Maßnahmen immer nur unter bestimmten Randbedingungen einsetzbar (beispielsweise in Kombination mit einer Argongewinnung) und/oder integrieren die Drucksauerstoffgewinnung und die Krypton-Xenon-Gewinnung sehr stark.Among these, some also show the combination of internal compaction and krypton-xenon recovery according to the preamble, in particular DE 10232430 A1 . EP 1308680 B1 and EP 1006326 B1 , All these known processes try to prevent by means of special measures that a significant part of the cryptone and xenon contained in the feed air are lost with the pressure oxygen product. However, these special measures can only ever be used under certain boundary conditions (for example in combination with argon recovery) and / or very strongly integrate the pressure oxygen recovery and the krypton-xenon recovery.

Der Erfindung liegt daher die Aufgabe zugrunde, eine Verfahren der eingangs genannten Art und eine entsprechende Vorrichtung anzugeben, die flexibler als die bekannten einsetzbar und oder apparativ und/oder betriebstechnisch besonders günstig sind.The invention is therefore based on the object to provide a method of the type mentioned above and a corresponding device which are more flexible than the known used and or apparatus and / or operationally particularly favorable.

Diese Aufgabe wird durch die Merkmale des kennzeichnenden Teils des Patentanspruchs 1 gelöst.This object is solved by the features of the characterizing part of patent claim 1.

Gemäß der Erfindung werden beide Sauerstofffraktionen - die erste, die das Drucksauerstoffprodukt bildet, und die zweite, die als Einsatz für die Krypton-Xenon-Anreicherungssäule dient - gemeinsam aus der Niederdrucksäule entnommen, auf den erhöhten Druck gebracht und zunächst nur partiell verdampft. Das Zwei-PhasenGemisch aus der partiellen Verdampfung wird in einen Abscheider (Phasentrenner) eingeleitet. Die Flüssigphase enthält den Großteil der schwerer als Sauerstoff flüchtigen Bestandteile, also insbesondere Krypton und Xenon. Der Krypton- und Xenon-Gehalt der Gasphase ist sehr gering, beispielsweise weniger als 1,4 ppm, vorzugsweise weniger als 0,9 ppm Krypton und weniger als 0,06 ppm, vorzugsweise weniger als 0,02 ppm Xenon. Der gasförmige Anteil wird anschließend von etwa dem Siedepunkt aus auf nahezu Umgebungstemperatur angewärmt und bildet dann das Drucksauerstoffprodukt, mit dem praktisch kein Krypton und Xenon mehr verloren geht. Der Großteil des in der Luft enthaltenen Kryptons und Xenons strömt mit dem flüssigen Anteil in die Krypton-Xenon-Gewinnung, genauer in die Krypton-Xenon-Anreicherungssäule. Mit dem erfindungsgemäßen Verfahren kann bei überschaubarem Zusatzaufwand eine besonders hohe Ausbeute erreicht werden, zum Beispiel über 70 % Kryptonausbeute und über 85 % Xenonausbeute.According to the invention, both oxygen fractions - the first forming the pressure oxygen product and the second serving as the insert for the krypton-xenon enrichment column - are taken together from the low-pressure column, brought to the elevated pressure and initially only partially evaporated. The two-phase mixture from the partial evaporation is introduced into a separator (phase separator). The liquid phase contains most of the heavier than volatile components, in particular krypton and xenon. The krypton and xenon content of the gas phase is very low, for example less than 1.4 ppm, preferably less than 0.9 ppm krypton and less than 0.06 ppm, preferably less than 0.02 ppm xenon. The gaseous portion is then heated from about the boiling point to near ambient temperature and then forms the pressure oxygen product with which virtually no krypton and xenon is lost. Most of the airborne krypton and xenon flow into the krypton-xenon recovery with the liquid portion, more specifically into the krypton-xenon enrichment column. With the method according to the invention, a particularly high yield can be achieved with manageable additional expenditure, for example over 70% krypton yield and over 85% xenon yield.

Darüber hinaus ist es möglich, Krypton-Xenon-Gewinnung und Stickstoff-Sauerstoff-Trennung bei der Erfindung unabhängig zu betreiben. Die Krypton-Xenon-Anreicherungssäule kann mit verringertem Umsatz betrieben oder zeitweise vollständig abgeschaltet werden, ohne die Drucksauerstoffgewinnung zu beeinträchtigen. Der überschüssige flüssige Anteil aus dem Abscheider wird in diesem Fall an der Krypton-Xenon-Gewinnung vorbeigeführt und an geeigneter Stelle im Verfahren weiterbehandelt.Moreover, it is possible to independently operate krypton-xenon recovery and nitrogen-oxygen separation in the invention. The krypton-xenon enrichment column can be operated at reduced conversion or temporarily shut down completely without affecting pressure oxygen recovery. The excess liquid fraction from the separator is in this case passed by the krypton-xenon recovery and further treated at a suitable point in the process.

Das erfindungsgemäße Verfahren funktioniert besonders gut bei relativ niedrigen Sauerstoff-Produktdrücken, wenn also der "erhöhte Druck" zum Beispiel zwischen 10 und 30 bar liegt.The inventive method works particularly well at relatively low oxygen product pressures, so if the "increased pressure", for example, between 10 and 30 bar.

Gemäß einem weiteren Aspekt der Erfindung wird mindestens ein Teil der dritten Sauerstofffraktion stromabwärts des Abscheiders als zweite Sauerstofffraktion in die Krypton-Xenon-Anreicherungssäule eingeleitet. Die Einleitung kann direkt oder indirekt (zum Beispiel über die Niederdrucksäule) erfolgen; die dritte Sauerstofffraktion (beziehungsweise der entsprechende Teil) wird in beiden Fällen in der Krypton-Xenon-Anreicherungssäule verwertet.In another aspect of the invention, at least a portion of the third oxygen fraction downstream of the separator is introduced into the krypton-xenon enrichment column as a second oxygen fraction. The introduction can be direct or indirect (for example via the low-pressure column); the third oxygen fraction (or the corresponding part) is utilized in both cases in the krypton-xenon enrichment column.

Alternativ oder zusätzlich zu einer direkten Einleitung kann mindestens ein Teil der dritten Sauerstofffraktion stromabwärts des Abscheiders in die Niederdrucksäule zurückgeleitet werden. Diese in die Niederdrucksäule zurückgeleitete Flüssigkeit kann ebenfalls wieder aus der Niederdrucksäule an derselben oder einer benachbarten Stelle entnommen und in die Krypton-Xenon-Anreicherungssäule eingeleitet werden. In diesem Fall wird der entsprechende Teil der dritten Sauerstofffraktion indirekt der Krypton-Xenon-Anreicherungssäule zugeführt.Alternatively, or in addition to direct introduction, at least a portion of the third oxygen fraction downstream of the precipitator may be returned to the low pressure column. This liquid, which has been returned to the low-pressure column, can likewise be withdrawn again from the low-pressure column at the same or an adjacent location and introduced into the krypton-xenon enrichment column. In this case, the corresponding portion of the third oxygen fraction is indirectly fed to the krypton-xenon enrichment column.

Die Krypton-Xenon-Gewinnung kann bei dem erfindungsgemäße Verfahren abschaltbar ausgebildet sein, indem in einem ersten Betriebsmodus mindestens ein Teil der dritten Sauerstofffraktion stromabwärts des Abscheiders direkt oder indirekt in die Krypton-Xenon-Anreicherungssäule eingeleitet wird und in einem zweiten Betriebsmodus der gesamte flüssige Anteil aus dem Abscheider an der Krypton-Xenon-Anreicherungssäule vorbeigeführt wird. Der erste Betriebsmodus entspricht also dem Normalbetrieb, der zweite Betriebmodus einer Verfahrensweise mit abgeschalteter Krypton-Xenon-Gewinnung.The krypton-xenon recovery can be formed switchable in the inventive method by at least a portion of the third oxygen fraction downstream of the separator is introduced directly or indirectly into the krypton-xenon enrichment column in a first mode of operation and in a second mode of operation, the entire liquid fraction from the separator past the krypton-xenon enrichment column. The first mode of operation thus corresponds to the normal mode, the second mode of operation of a mode with deactivated krypton-xenon recovery.

Die erste und die dritte Sauerstofffraktion werden vorzugsweise gemeinsam mindestens einen praktischen oder theoretischen Boden oberhalb des Sumpfs aus der Niederdrucksäule entnommen. Damit enthalten sie einen gegenüber der Sumpfflüssigkeit verringerten Anteil an Krypton und Xenon.The first and third oxygen fractions are preferably taken together at least one practical or theoretical tray above the bottom of the low pressure column. Thus they contain compared to the bottoms liquid reduced proportion of krypton and xenon.

Die zweite Sauerstofffraktion wird vorzugsweise mindestens einen praktischen oder theoretischen Boden unterhalb der Entnahmestelle der ersten und dritten Sauerstofffraktion aus der Niederdrucksäule entnommen, insbesondere von deren Sumpf. Damit weist sie einen besonders hohen Krypton- und Xenon-Gehalt auf. Zwischen den Entnahmestellen der ersten und dritten Sauerstofffaktion einerseits und der zweiten Sauerstofffraktion andererseits liegen beispielsweise ein bis fünf, vorzugsweise zwei bis drei theoretische oder praktische Böden.The second oxygen fraction is preferably taken from the low-pressure column at least one practical or theoretical bottom below the extraction point of the first and third oxygen fraction, in particular from the bottom thereof. Thus, it has a particularly high krypton and xenon content. Between the sampling points of the first and third oxygen fraction on the one hand and On the other hand, the second oxygen fraction is, for example, one to five, preferably two to three, theoretical or practical soils.

Die Erfindung betrifft außerdem eine Vorrichtung gemäß den Patentansprüchen 7 bis 10.The invention also relates to a device according to claims 7 to 10.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand eines in der Zeichnung schematisch und stark vereinfacht dargestellten ersten Ausführungsbeispiels näher erläutert.The invention and further details of the invention are explained in more detail below with reference to a schematically and greatly simplified in the drawing illustrated first embodiment.

Verdichtete und vorgereinigte Einsatzluft 1 wird in einem Hauptwärmetauscher 2 abgekühlt und gegebenenfalls teilweise verflüssigt und über Leitung 3 einem Rektifiziersystem zugeführt (Zuführung nicht dargestellt), das eine Doppelsäule 4 zur Stickstoff-Sauerstoff-Trennung und eine Krypton-Xenon-Anreicherungssäule 5 aufweist. Die Doppelsäule besteht aus einer Hochdrucksäule 6, einer Niederdrucksäule 7 und einem Hauptkondensator 8. Die Einsatzluft wird wenigstens zum Teil in die Hochdrucksäule eingespeist (nicht dargestellt) und dort in flüssigen Rohsauerstoff 9 und gasförmigen Kopfstickstoff getrennt. Der Kopfstickstoff wird im Hauptkondensator 8 mindestens teilweise kondensiert. Ein Teil 10 des dabei gebildeten flüssigen Stickstoffs wird in die Niederdrucksäule 7 eingeleitet, ebenso wie der Rohsauerstoff 9. Aus dem unteren Bereich der Niederdrucksäule 7 werden zwei Sauerstoffströme 11, 12 flüssig entnommen, wobei zwischen den beiden Entnahmestellen drei praktische Böden angeordnet sind.Compressed and prepurified feed air 1 is cooled in a main heat exchanger 2 and optionally partially liquefied and fed via line 3 to a rectification system (feed not shown), which has a double column 4 for nitrogen-oxygen separation and a krypton-xenon enrichment column 5. The double column consists of a high pressure column 6, a low pressure column 7 and a main condenser 8. The feed air is at least partially fed into the high pressure column (not shown) and separated there into liquid crude oxygen 9 and gaseous overhead nitrogen. The top nitrogen is at least partially condensed in the main condenser 8. A portion 10 of the resulting liquid nitrogen is introduced into the low-pressure column 7, as well as the raw oxygen 9. From the lower region of the low-pressure column 7, two oxygen streams 11, 12 taken liquid, with three practical trays are arranged between the two sampling points.

Der Abzug der übrigen gasförmigen Produkte aus der Niederdrucksäule (Reinstickstoff vom Kopf der Niederdrucksäule, Unrein-Stickstoff von einer Zwischenstelle ist in der Zeichnung nicht dargestellt. Diese Produkte werden als Rückströme 13, 14, 15 im Hauptwärmetauscher angewärmt und schließlich unter etwa Umgebungstemperatur abgezogen. Außerdem können Sauerstoff und/oder Stickstoff als Flüssigprodukte gewonnen werden und über eine Argonübergangsleitung kann die Niederdrucksäule mit einer Argongewinnung verbunden sein (alles ebenfalls in der Zeichnung nicht dargestellt).The withdrawal of the other gaseous products from the low-pressure column (pure nitrogen from the top of the low-pressure column, impure nitrogen from an intermediate point is not shown in the drawing.) These products are warmed up as reflux streams 13, 14, 15 in the main heat exchanger and finally withdrawn below ambient temperature For example, oxygen and / or nitrogen can be obtained as liquid products, and the low-pressure column can be connected to argon recovery via an argon transfer line (all also not shown in the drawing).

Der erste Sauerstoffstrom 11 enthält die erste und die dritte Sauerstofffraktion in Sinne der Erfindung. Diese beiden werden gemeinsam über die Leitungen 16, 17, und 18 durch eine Pumpe 19 und den unteren (kalten) Bereich des Hauptwärmetauschers 2 geführt und schließlich über ein Regelventil 20, das keinen nennenswerten Druckverlust bewirkt, in einen Abscheider (Phasentrenner) 21 eingeleitet. Der gasförmige Anteil bildet die erste Sauerstofffraktion 22 und wird bei etwa der gleichen Temperatur wieder in den Hauptwärmetauscher 2 eingeleitet und dort auf etwa Umgebungstemperatur angewärmt und schließlich über Leitung 23 als gasförmiges Drucksauerstoffprodukt abgezogen.The first oxygen stream 11 contains the first and the third oxygen fraction in the sense of the invention. These two are common across the lines 16, 17, and 18th passed through a pump 19 and the lower (cold) region of the main heat exchanger 2 and finally via a control valve 20 which causes no appreciable pressure loss, introduced into a separator (phase separator) 21. The gaseous fraction forms the first oxygen fraction 22 and is reintroduced into the main heat exchanger 2 at about the same temperature where it is warmed to approximately ambient temperature and finally withdrawn via line 23 as gaseous pressure oxygen product.

Der flüssige Anteil aus dem Abscheider 21 bildet erfindungsgemäß die dritte Sauerstofffraktion 24 und wird in dem Beispiel über Leitung 32 vollständig in den Sumpf der Niederdrucksäule 7 zurückgeleitet.According to the invention, the liquid fraction from the separator 21 forms the third oxygen fraction 24 and, in the example, is returned via line 32 completely to the bottom of the low-pressure column 7.

Ein anderer Teil des ersten Sauerstoffstroms 11 bildet eine vierte Sauerstofffraktion 25 und wird als Rücklaufflüssigkeit auf den Kopf der Krypton-Xenon-Anreicherungssäule aufgegeben.Another portion of the first oxygen stream 11 forms a fourth oxygen fraction 25 and is fed as reflux liquid to the top of the krypton-xenon enrichment column.

Der zweite Sauerstoffstrom 12 bildet die zweite Sauerstofffraktion, die weiter unten in die Krypton-Xenon-Anreicherungssäule 5 eingeleitet wird, in dem Beispiel unmittelbar oberhalb des Sumpfs.The second oxygen stream 12 forms the second oxygen fraction which is introduced further down into the krypton-xenon enrichment column 5 in the example immediately above the sump.

Die Krypton-Xenon-Anreicherungssäule wird mittels eines Sumpfverdampfers 26 beheizt. Gasförmiger Sauerstoff 27 vom Kopf der Krypton-Xenon-Anreicherungssäule wird in die Niederdrucksäule 7 zurückgeleitet. Vom Sumpf der Krypton-Xenon-Anreicherungssäule wird eine krypton- und/oder xenonangereicherte Fraktion 28 flüssig abgezogen, die ansonsten hauptsächlich Sauerstoff enthält. Sie kann in weiteren Schritten zu einem Rein-Krypton-Produkt und/oder zu einem Rein-Xenon-Produkt weiterverarbeitet werden.The krypton-xenon enrichment column is heated by means of a bottom evaporator 26. Gaseous oxygen 27 from the head of the krypton-xenon enrichment column is returned to the low pressure column 7. From the bottom of the krypton-xenon enrichment column, a krypton- and / or xenon-enriched fraction 28 is withdrawn liquid, which otherwise contains mainly oxygen. It can be processed in further steps to a pure krypton product and / or to a pure xenon product.

Der Flüssigkeitsstände in der Krypton-Xenon-Anreicherungssäule 5 und im Abscheider 21 werden jeweils mittels eines Flüssigkeitsstandsreglers 29, 30 geregelt (LIC = level indication and control).The liquid levels in the krypton-xenon enrichment column 5 and in the separator 21 are each controlled by means of a liquid level controller 29, 30 (LIC = level indication and control).

Die Leitung 31 ist fakultativ. Über sie kann in einem zweiten Ausführungsbeispiel ein Teil der ansonsten über die Leitungen 32 und 12 fließenden dritten Sauerstofffraktion 24 unter Umgehung der Niederdrucksäule als zweite Sauerstofffraktion in die Krypton-Xenon-Anreicherungssäule 5 eingeleitet werden. Der Durchfluss durch die Leitung 31 wird mittels eines von Hand betätigten Ventils 32 eingestellt (HIC = hand indication and control). Alternativ kann in einem dritten Ausführungsbeispiel auch die gesamte zweite Sauerstofffraktion, also der Einsatzstrom für den unteren Bereich der Krypton-Xenon-Anreicherungssäule 5 über die Leitung 31 geführt werden; hierbei kann die Leitung 12 entfallen.The line 31 is optional. In a second exemplary embodiment, part of the third oxygen fraction 24, which otherwise flows via the lines 32 and 12, can bypass the low-pressure column as a second oxygen fraction into the krypton-xenon enrichment column 5 are initiated. The flow through the conduit 31 is adjusted by means of a manually operated valve 32 (HIC = hand indication and control). Alternatively, in a third exemplary embodiment, the entire second oxygen fraction, that is to say the feed stream for the lower region of the krypton-xenon enrichment column 5, can also be conducted via the line 31; In this case, the line 12 can be omitted.

Claims (10)

Verfahren zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem, das eine Niederdrucksäule (7) zur Stickstoff-Sauerstoff-Trennung und eine Krypton-Xenon-Anreicherungssäule (5) aufweist, wobei bei dem Verfahren • verdichtete und vorgereinigte Einsatzluft (1, 3) in das Rektifiziersystem eingeleitet wird und • eine erste Sauerstofffraktion flüssig aus der Niederdrucksäule (3) entnommen (11, 16), flüssig auf einen erhöhten Druck gebracht (19), verdampft (2), angewärmt (2) und als gasförmiges Drucksauerstoffprodukt (23) abgeführt wird, wobei bei dem Verfahren ferner • eine zweite Sauerstofffraktion (12, 31) in den unteren oder mittleren Bereich der Krypton-Xenon-Anreicherungssäule (5) eingeleitet wird, • dem unteren Bereich der Krypton-Xenon-Anreicherungssäule (15) eine krypton-und/oder xenonangereicherte Fraktion (19) entnommen wird, dadurch gekennzeichnet, dass • eine dritte Sauerstofffraktion gemeinsam mit der ersten Sauerstofffraktion der Niederdrucksäule entnommen (11, 16), auf den erhöhten Druck gebracht (19) wird, die erste und die dritte Sauerstofffraktion anschließend gemeinsam teilweise verdampft (2) und in einem Abscheider (21) in einen gasförmigen Anteil und einen flüssigen Anteil getrennt werden, wobei • die erste Sauerstofffraktion (22) durch mindestens einen Teil des gasförmigen Anteils gebildet, anschließend angewärmt (2) und als gasförmiges Drucksauerstoffprodukt (23) abgeführt wird und • die dritte Sauerstofffraktion (24) durch den flüssigen Anteil gebildet und anschließend in das Rektifiziersystem zurückgeleitet (33, 31) wird. A process for recovering pressure oxygen and krypton / xenon by cryogenic separation of air in a rectification system comprising a low pressure column (7) for nitrogen-oxygen separation and a krypton-xenon enrichment column (5), the method • compressed and pre-cleaned feed air (1, 3) is introduced into the rectification system and A first fraction of oxygen liquid (11, 16) removed from the low pressure column (3), brought liquid to an elevated pressure (19), evaporated (2), warmed (2) and discharged as gaseous pressure oxygen product (23), wherein the Method further A second oxygen fraction (12, 31) is introduced into the lower or middle region of the krypton-xenon enrichment column (5), A krypton and / or xenon enriched fraction (19) is taken from the lower region of the krypton-xenon enrichment column (15), characterized in that • a third oxygen fraction taken together with the first oxygen fraction of the low pressure column (11, 16), brought to the elevated pressure (19), the first and third oxygen fraction then together partially evaporated (2) and in a separator (21) in one gaseous portion and a liquid portion are separated, wherein The first oxygen fraction (22) is formed by at least part of the gaseous fraction, subsequently heated (2) and removed as gaseous pressure oxygen product (23) and The third oxygen fraction (24) is formed by the liquid fraction and then returned to the rectification system (33, 31). Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass mindestens ein Teil der dritten Sauerstofffraktion stromabwärts des Abscheiders als zweite Sauerstofffraktion (12, 31) in die Krypton-Xenon-Anreicherungssäule (5) eingeleitet wird.A method according to claim 1, characterized in that at least a portion of the third oxygen fraction downstream of the separator as second oxygen fraction (12, 31) is introduced into the krypton-xenon enrichment column (5). Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass mindestens ein Teil der dritten Sauerstofffraktion (24) stromabwärts des Abscheiders in die Niederdrucksäule zurückgeleitet (33) wird.A method according to claim 1 or 2, characterized in that at least a portion of the third oxygen fraction (24) downstream of the separator in the low-pressure column is returned (33). Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass in einem ersten Betriebsmodus mindestens ein Teil der dritten Sauerstofffraktion (24) stromabwärts des Abscheiders direkt (31) oder indirekt (12) in die Krypton-Xenon-Anreicherungssäule (15) eingeleitet wird und in einem zweiten Betriebsmodus der gesamte flüssige Anteil aus dem Abscheider an der Krypton-Xenon-Anreicherungssäule vorbeigeführt (33) wird.Method according to one of claims 1 to 3, characterized in that in a first mode of operation at least a portion of the third oxygen fraction (24) downstream of the separator directly (31) or indirectly (12) is introduced into the krypton-xenon enrichment column (15) and in a second mode of operation, all the liquid portion from the separator passes (33) past the krypton-xenon enrichment column. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, dass die erste und die dritte Sauerstofffraktion (11) mindestens einen praktischen oder theoretischen Boden oberhalb des Sumpfs aus der Niederdrucksäule (3) entnommen werden.Method according to one of claims 1 to 4, characterized in that the first and the third oxygen fraction (11) at least one practical or theoretical soil above the bottom of the low pressure column (3) are removed. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass die zweite Sauerstofffraktion mindestens einen praktischen oder theoretischen Boden unterhalb der Entnahmestelle der ersten und dritten Sauerstofffraktion aus der Niederdrucksäule (3) entnommen wird, insbesondere von deren Sumpf.Method according to one of claims 1 to 5, characterized in that the second oxygen fraction at least one practical or theoretical soil below the sampling point of the first and third oxygen fraction from the low pressure column (3) is removed, in particular from the bottom thereof. Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft mit einem Rektifiziersystem, das eine Niederdrucksäule (7) zur Stickstoff-Sauerstoff-Trennung und eine Krypton-Xenon-Anreicherungssäule (5) aufweist, und mit • Mitteln zum Einleiten verdichteter und vorgereinigter Einsatzluft (1, 3) in das Rektifiziersystem, • Mitteln zum Entnehmen (11, 16) einer ersten Sauerstofffraktion in flüssigem Zustand aus der Niederdrucksäule (3), • Mitteln, um die erste Sauerstofffraktion in flüssigem Zustand auf einen erhöhten Druck zu bringen (19), sie zu verdampfen (2), anzuwärmen (2) und als gasförmiges Drucksauerstoffprodukt (23) abzuführen, • Mitteln zum Einleiten einer zweiten Sauerstofffraktion (12, 31) in den unteren oder mittleren Bereich der Krypton-Xenon-Anreicherungssäule (5), sowie mit • Mitteln zum Entnehmen einer krypton- und/oder xenonangereicherten Fraktion (19) aus dem unteren Bereich der Krypton-Xenon-Anreicherungssäule (15), gekennzeichnet durch • Mittel zum Entnehmen (11, 16) einer dritten Sauerstofffraktion gemeinsam mit der ersten Sauerstofffraktion aus der Niederdrucksäule, • Mittel, um die erste und die dritte Sauerstofffraktion gemeinsam auf den erhöhten Druck zu bringen (19) und anschließend gemeinsam teilweise zu verdampfen (2), • einen Abscheider (21) zum Trennen der teilweise verdampften gemeinsamen ersten und dritten Sauerstofffraktion in einen gasförmigen Anteil und einen flüssigen Anteil, • Mittel zur Entnahme des gasförmigen Anteils als die erste Sauerstofffraktion (22) aus dem Abscheider (21), zum anschließenden Anwärmen (2) der ersten Sauerstofffraktion (22) und zu deren Abführen als gasförmiges Drucksauerstoffprodukt (23) und • Mittel zur Entnahme des flüssigen Anteils als die dritte Sauerstofffraktion (24) aus dem Abscheider (21) und zum anschließenden Zurückleiten (33, 31) der dritten Sauerstofffraktion in das Rektifiziersystem. Apparatus for recovering pressure oxygen and krypton / xenon by cryogenic separation of air with a rectification system comprising a low pressure column (7) for nitrogen-oxygen separation and a krypton-xenon enrichment column (5), and with Means for introducing compressed and pre-cleaned feed air (1, 3) into the rectification system, Means for removing (11, 16) a first oxygen fraction in the liquid state from the low-pressure column (3), Means for raising the first oxygen fraction in a liquid state to an elevated pressure (19), evaporating it (2), heating it (2) and removing it as a gaseous pressure oxygen product (23), • Means for introducing a second oxygen fraction (12, 31) in the lower or central region of the krypton-xenon enrichment column (5), as well as with Means for removing a krypton- and / or xenon-enriched fraction (19) from the lower region of the krypton-xenon enrichment column (15), marked by Means for removing (11, 16) a third oxygen fraction together with the first oxygen fraction from the low-pressure column, Means for bringing the first and third oxygen fractions together to the elevated pressure (19) and then partially evaporating them together (2), A separator (21) for separating the partially vaporized common first and third oxygen fraction into a gaseous fraction and a liquid fraction, • means for removing the gaseous fraction as the first oxygen fraction (22) from the separator (21), for subsequent heating (2) of the first oxygen fraction (22) and for their removal as gaseous pressure oxygen product (23) and • means for withdrawing the liquid fraction as the third oxygen fraction (24) from the separator (21) and then returning (33, 31) the third oxygen fraction to the rectification system. Vorrichtung nach Anspruch 7, mit Mitteln zum Einleiten mindestens eines Teils der dritten Sauerstofffraktion stromabwärts des Abscheiders als zweite Sauerstofffraktion (12, 31) in die Krypton-Xenon-Anreicherungssäule (5).Apparatus according to claim 7, including means for introducing at least a portion of the third oxygen fraction downstream of the separator as a second oxygen fraction (12, 31) into the krypton-xenon enrichment column (5). Vorrichtung nach Anspruch 7 oder 8, mit Mitteln zum Zurückleiten (33) mindestens eines Teils der dritten Sauerstofffraktion (24) stromabwärts des Abscheiders in die Niederdrucksäule.Apparatus according to claim 7 or 8, including means for returning (33) at least a portion of the third oxygen fraction (24) downstream of the separator to the low pressure column. Vorrichtung nach einem der Ansprüche 7 bis 9, mit Regel- und/oder Steuereinrichtungen, die so ausgestaltet sind, dass in einem ersten Betriebsmodus mindestens ein Teil der dritten Sauerstofffraktion (24) stromabwärts des Abscheiders direkt (31) oder indirekt (12) in die Krypton-Xenon-Anreicherungssäule (15) eingeleitet wird und in einem zweiten Betriebsmodus der gesamte flüssige Anteil aus dem Abscheider an der Krypton-Xenon-Anreicherungssäule vorbeigeführt (33) wirdApparatus according to any one of claims 7 to 9, comprising control and / or regulating means arranged such that, in a first mode of operation, at least a portion of the third oxygen fraction (24) downstream of the separator directly (31) or indirectly (12) into the Krypton-xenon enrichment column (15) is introduced and in a second mode of operation, the entire liquid portion from the separator on the krypton-xenon enrichment column is passed (33)
EP09012681A 2009-10-07 2009-10-07 Method and device for obtaining pressurised oxygen and krypton/xenon Withdrawn EP2312248A1 (en)

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FR3020866A1 (en) * 2014-05-07 2015-11-13 Air Liquide DISTILLATION COLUMN AND CRYOGENIC DISTILLATION AIR SEPARATION APPARATUS FOR THE POSSIBLE PRODUCTION OF A MIXTURE OF KRYPTON AND XENON
CN114279169A (en) * 2022-01-21 2022-04-05 浙江智海化工设备工程有限公司 Medium-pressure and low-pressure oxygen air separation and krypton-xenon concentration integrated equipment and concentration process
CN114812098A (en) * 2022-05-13 2022-07-29 河南心连心深冷能源股份有限公司 Device and method for extracting poor krypton, xenon or oxygen-enriched gas by main condensation evaporator

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US6694775B1 (en) * 2002-12-12 2004-02-24 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon
EP1585926A1 (en) 2002-12-19 2005-10-19 Karges-Faulconbridge, Inc. System for liquid extraction, and methods
DE10302389A1 (en) 2003-01-22 2003-06-18 Linde Ag Device for the low temperature decomposition of air comprises a rectification system consisting of a high pressure column, a low pressure column, and a condenser-evaporator system for heating the low pressure column
EP1482266A1 (en) 2003-05-28 2004-12-01 Linde Aktiengesellschaft Process and device for the recovery of Krypton and/or Xenon by cryogenic separation of air
DE10334559A1 (en) 2003-05-28 2004-12-16 Linde Ag Process for recovering krypton/xenon by the cryogenic separation of air comprises feeding an argon-enriched vapor from a crude argon rectification system into a sump evaporator
DE10334560A1 (en) 2003-05-28 2004-12-16 Linde Ag Method for recovering krypton and xenon from air, comprises separating nitrogen and oxygen and feeding krypton- and xenon-containing fraction into enrichment column, stream of pure air being decompressed and fed into column
DE10332862A1 (en) 2003-07-18 2005-02-10 Linde Ag Cryogenic assembly to extract krypton and/or xenon gas from air has intermediate pipe on the methane removal column alongside a base panel above the sump
DE10332863A1 (en) 2003-07-18 2004-02-26 Linde Ag Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream
EP1544559A1 (en) 2003-12-20 2005-06-22 Linde AG Process and device for the cryogenic separation of air
DE102005029274A1 (en) 2004-08-17 2006-02-23 Linde Ag Obtaining gaseous pressure product, by cryogenic separation of air implementing normal operation, emergency operation, and bypass operation
EP1666824A1 (en) 2004-12-03 2006-06-07 Linde Aktiengesellschaft Process and device for the recovery of Argon by cryogenic separation of air
EP1672301A1 (en) 2004-12-03 2006-06-21 Linde AG Apparatus for the cryogenic separation of a gaseous mixture in particular of air
EP1757884A2 (en) 2005-08-26 2007-02-28 Linde Aktiengesellschaft Process for the recovery of Krypton and/or Xenon by cryogenic separation of air

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3020866A1 (en) * 2014-05-07 2015-11-13 Air Liquide DISTILLATION COLUMN AND CRYOGENIC DISTILLATION AIR SEPARATION APPARATUS FOR THE POSSIBLE PRODUCTION OF A MIXTURE OF KRYPTON AND XENON
CN114279169A (en) * 2022-01-21 2022-04-05 浙江智海化工设备工程有限公司 Medium-pressure and low-pressure oxygen air separation and krypton-xenon concentration integrated equipment and concentration process
CN114812098A (en) * 2022-05-13 2022-07-29 河南心连心深冷能源股份有限公司 Device and method for extracting poor krypton, xenon or oxygen-enriched gas by main condensation evaporator

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