EP2312248A1 - Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon - Google Patents

Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon 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
Authority
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.)
Withdrawn
Application number
EP09012681A
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German (de)
English (en)
Inventor
Gerhard Pompl
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Linde GmbH
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to EP09012681A priority Critical patent/EP2312248A1/fr
Publication of EP2312248A1 publication Critical patent/EP2312248A1/fr
Withdrawn legal-status Critical Current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.
EP09012681A 2009-10-07 2009-10-07 Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon Withdrawn EP2312248A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP09012681A EP2312248A1 (fr) 2009-10-07 2009-10-07 Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon

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Application Number Priority Date Filing Date Title
EP09012681A EP2312248A1 (fr) 2009-10-07 2009-10-07 Procédé et dispositif de production d'oxygène sous pression et de crypton/xénon

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EP2312248A1 true EP2312248A1 (fr) 2011-04-20

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR3020866A1 (fr) * 2014-05-07 2015-11-13 Air Liquide Colonne de distillation et appareil de separation d’air par distillation cryogenique pour la production eventuelle d’un melange de krypton et de xenon

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