EP2279385B1 - Vorrichtung und verfahren zur lufttrennung durch kryogene destillation - Google Patents

Vorrichtung und verfahren zur lufttrennung durch kryogene destillation Download PDF

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Publication number
EP2279385B1
EP2279385B1 EP09742279A EP09742279A EP2279385B1 EP 2279385 B1 EP2279385 B1 EP 2279385B1 EP 09742279 A EP09742279 A EP 09742279A EP 09742279 A EP09742279 A EP 09742279A EP 2279385 B1 EP2279385 B1 EP 2279385B1
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EP
European Patent Office
Prior art keywords
pressure column
level
liquid
low pressure
oxygen
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Not-in-force
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EP09742279A
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English (en)
French (fr)
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EP2279385A2 (de
Inventor
Alain Briglia
Bernard Saulnier
Laurent Samy
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Publication of EP2279385A2 publication Critical patent/EP2279385A2/de
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Publication of EP2279385B1 publication Critical patent/EP2279385B1/de
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—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
    • 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
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/02—Mixing or blending of fluids to yield a certain product
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/40—One fluid being air
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/52—One fluid being oxygen enriched compared to air, e.g. "crude oxygen"

Definitions

  • the present invention applies to an apparatus and a method for producing krypton and xenon by air separation by cryogenic distillation and in particular to a method of separating gases from the air with internal compression (in which oxygen gaseous is produced by vaporization under pressure in the exchange line) where a krypton / xenon mixture is extracted.
  • an air separation unit comprising a double column and wherein the oxygen gas is produced by pressurized vaporization in the exchange line (internal compression apparatus) in which it is intended to extract a krypton mixture xenon
  • the yield of this extraction decreases significantly because the pumped oxygen extracted from the low pressure distillation column leads with it a significant part of the compounds to be valued such as krypton and xenon.
  • the low pressure column is fed by the purge rich in krypton and xenon produced by concentration.
  • the krypton and xenon-rich purge produced above will supply the low pressure column with a distillation stage lower than the withdrawal of the liquid oxygen to be pumped and then vaporized in the main exchanger.
  • the final mixture rich in krypton and xenon is extracted from the bottom of the low pressure column for further processing.
  • this return is injected at the suction of the pump to minimize the withdrawal OL of the column, and thus increase the extraction yield of krypton and xenon
  • Such a method makes it possible to extract about 90% of the xenon present in the air, where a conventional method only allows a yield of about 70% at best. As for the extraction yield of krypton, it reaches about 75% while the performance of a conventional apparatus does not allow the better than a yield of the order of 60%.
  • a medium pressure air flow 1 is sent to the medium pressure column 20 of a double air separation column.
  • the double column also comprises a low pressure column 21 thermally coupled with the medium pressure column 20 by means of a vaporizer 24, which vaporizes the bottom liquid of the low pressure column by heat exchange with the nitrogen gas at the top of the middle column pressure.
  • a flow of high pressure liquid air is expanded in a valve and then divided into two.
  • the flow 3 thus formed is sent to the medium pressure column 20 a few theoretical trays above the entry point of the flow 1.
  • the rest of the liquid air 4 is cooled in the subcooler 26, expanded and sent to the column low pressure 21.
  • a lower rich liquid flow rate enriched in oxygen, krypton and xenon is withdrawn in the vat of the medium pressure column 20, cooled in the subcooler 26, then expanded and sent to a vaporizer 22 where it is partially vaporized by exchange of heat with gaseous air enriched with nitrogen 8 from the medium pressure column 20.
  • the gaseous air is condensed to form a flow 9 which is then sent to the low pressure column 21.
  • the vaporized rich liquid 16 is expanded as intermediate gas and sent to the low pressure column while the remaining intermediate liquid 7 is sent to the low pressure column 21 a few trays above the tank.
  • An upper rich liquid flow 6 is withdrawn between the inlet of the air 1 and the air inlet 3 and / or the withdrawal of the flow 8.
  • This flow 6 is cooled in the subcooler 26, mixed with the rich liquid vaporized 16 and sent to the low pressure column 21. Poor liquid enriched in nitrogen 15 is withdrawn at the top of the medium pressure column 20 and sent to the top of the low pressure column 21 after cooling and expansion.
  • Liquid oxygen 10 is withdrawn from the low pressure column 21 a few trays above the tank and preferably above the arrival of the liquid 7. This liquid is pumped by the pump 23 to serve as a product rich in water. oxygen.
  • Liquid oxygen 11 enriched in krypton and xenon is withdrawn in the bottom of the low pressure column 21 and is subsequently purified to produce a mixture of krypton and xenon.
  • Low pressure nitrogen 13 is withdrawn at the top of the low pressure column 21, heated in the subcooler and heated against the air flows 1.2 (heating not shown).

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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)

Claims (15)

  1. Verfahren zur Produktion von Krypton und Xenon durch Tieftemperaturzerlegung von Luft in einer Doppelkolonne, die eine Mitteldruckkolonne (20) und eine Niederdruckkolonne (21) umfasst, wobei
    i) verdichtete, abgekühlte und gereinigte gasförmige Luft (1) auf ein erstes Niveau der Mitteldruckkolonne geführt wird,
    ii) verdichtete, abgekühlte und gereinigte flüssige Luft (3) auf ein zweites Niveau der Mitteldruckkolonne oberhalb des ersten Niveaus geführt wird,
    iii) eine mit Sauerstoff, Krypton und Xenon angereicherte Flüssigkeit (5) aus dem Sumpf der Mitteldruckkolonne abgezogen wird,
    iv) eine Flüssigkeit (6) aus der Mitteldruckkolonne auf einem Niveau zwischen dem ersten und dem zweiten Niveau abgezogen wird und zu der Niederdruckkolonne geführt wird,
    v) die mit Sauerstoff, Krypton und Xenon angereicherte Flüssigkeit teilweise verdampft wird, um ein Zwischengas (16) und eine Zwischenflüssigkeit (7) zu bilden,
    vi) ein erster sauerstoffreicher flüssiger Strom (10) auf einem dritten Niveau der Niederdruckkolonne abgezogen, unter Druck gesetzt und verdampft wird,
    vii) die Zwischenflüssigkeit von dem Verdampfer zu der Niederdruckkolonne auf ein Zwischenniveau der Niederdruckkolonne, das niedriger als das dritte Niveau ist, geführt wird und
    viii) ein zweiter sauerstoffreicher flüssiger Strom (11) aus der Niederdruckkolonne auf einem vierten Niveau, das niedriger als das Zwischenniveau ist, abgezogen und gereinigt wird, um ein Gemisch aus Krypton und Xenon zu produzieren.
  2. Verfahren nach Anspruch 1, wobei das Zwischengas (6), das in der Niederdruckkolonne (21) auf einem höheren Niveau verdampft wurde, auf ein Zwischenniveau geführt wird.
  3. Verfahren nach Anspruch 1 oder 2, wobei die mit Sauerstoff, Krypton und Xenon angereicherte Flüssigkeit (5) durch Wärmetausch mit einem Gas (8), das aus der Niederdruckkolonne abgezogen wird, verdampft wird.
  4. Verfahren nach Anspruch 3, wobei das aus der Niederdruckkolonne abgezogene Gas (8) oberhalb des ersten Niveaus abgezogen wird.
  5. Verfahren nach einem der vorhergehenden Ansprüche, wobei die Zwischenflüssigkeit von dem Verdampfer auf ein Zwischenniveau der Niederdruckkolonne, das niedriger als das dritte Niveau ist, geführt wird.
  6. Verfahren nach Anspruch 5, wobei der zweite sauerstoffreiche flüssige Strom (11) aus der Niederdruckkolonne auf ein viertes Niveau, das niedriger als das Zwischenniveau ist, geführt wird.
  7. Verfahren nach einem der Ansprüche 1 bis 4, wobei die Zwischenflüssigkeit mit einem zweiten sauerstoffreichen flüssigen Strom vermischt wird.
  8. Vorrichtung zur Tieftemperaturzerlegung von Luft, das eine Doppelkolonne, die von einer Mitteldruckkolonne (20) und einer Niederdruckkolonne (21) gebildet ist, und einen Verdampfer (22) umfasst, umfassend:
    i) Mittel, um die verdichtete, abgekühlte und gereinigte gasförmige Luft (3) auf ein erstes Niveau der Mitteldruckkolonne zu führen,
    ii) Mittel, um die verdichtete, abgekühlte und gereinigte flüssige Luft auf ein zweites Niveau der Mitteldruckkolonne oberhalb des ersten Niveaus zu führen,
    iii) Mittel, um eine mit Sauerstoff, Krypton und Xenon angereicherte Flüssigkeit (5) aus dem Sumpf der Mitteldruckkolonne abzuziehen,
    iv) Mittel, um eine Flüssigkeit aus der Mitteldruckkolonne auf einem Niveau zwischen dem ersten und dem zweiten Niveau abzuziehen und zu der Niederdruckkolonne zu führen,
    v) Mittel, um mindestens einen Teil der mit Sauerstoff, Krypton und Xenon angereicherten Flüssigkeit zu dem Verdampfer zu führen, wo sie teilweise verdampft wird, um ein Zwischengas (16) und eine Zwischenflüssigkeit (7) zu bilden,
    vi) Mittel, um einen ersten sauerstoffreichen flüssigen Strom (10) auf einem dritten Niveau der Niederdruckkolonne abzuziehen, Mittel (23), um ihn unter Druck zu setzen, und Mittel, um ihn zu verdampfen,
    vii) Mittel, um die Zwischenflüssigkeit von dem Verdampfer zu der Niederdruckkolonne auf ein Zwischenniveau der Niederdruckkolonne zu führen, und
    viii) Mittel, um einen zweiten sauerstoffreichen flüssigen Strom aus der Niederdruckkolonne auf einem vierten Niveau, das niedriger als das dritte Niveau ist, das niedriger als das Zwischenniveau ist, abzuziehen, und Mittel, um ihn zu reinigen, um ein Gemisch aus Krypton und Xenon zu produzieren.
  9. Vorrichtung nach Anspruch 8, die Mittel umfasst, um das Zwischengas von dem Verdampfer (22) zu der Niederdruckkolonne (21) auf ein Niveau, das höher als das Zwischenniveau ist, zu führen.
  10. Vorrichtung nach Anspruch 8 oder 9, die Mittel umfasst, um ein aus der Mitteldruckkolonne (20) abgezogenes Gas zu dem Verdampfer (22) zu führen.
  11. Vorrichtung nach Anspruch 10, die Mittel umfasst, um das aus der Mitteldruckkolonne (20) abgezogene Gas oberhalb des ersten Niveaus abzuziehen.
  12. Vorrichtung nach Anspruch 8 bis 11, die Mittel umfasst, um den ersten sauerstoffreichen Strom unter Druck zu setzen und zu verdampfen, vorzugsweise durch Wärmetausch mit der zu destillierenden Luft.
  13. Verfahren nach einem der Ansprüche 8 bis 12, die Mittel umfasst, um die Zwischenflüssigkeit von dem Verdampfer auf ein Zwischenniveau der Niederdruckkolonne, das niedriger als das dritte Niveau ist, zu führen.
  14. Vorrichtung nach Anspruch 13, die Mittel umfasst, um den zweiten sauerstoffreichen flüssigen Strom (11) aus der Niederdruckkolonne auf einem vierten Niveau abzuziehen, das niedriger als das Zwischenniveau ist.
  15. Verfahren nach einem der Ansprüche 8 bis 12, die Mittel umfasst, um die Zwischenflüssigkeit mit einem zweiten sauerstoffreichen flüssigen Strom zu vermischen.
EP09742279A 2008-04-23 2009-04-08 Vorrichtung und verfahren zur lufttrennung durch kryogene destillation Not-in-force EP2279385B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0852727A FR2930629B1 (fr) 2008-04-23 2008-04-23 Appareil et procede de separation d'air par distillation cryogenique
PCT/FR2009/050625 WO2009136081A2 (fr) 2008-04-23 2009-04-08 Appareil et procédé de séparation d'air par distillation cryogénique

Publications (2)

Publication Number Publication Date
EP2279385A2 EP2279385A2 (de) 2011-02-02
EP2279385B1 true EP2279385B1 (de) 2012-02-22

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EP09742279A Not-in-force EP2279385B1 (de) 2008-04-23 2009-04-08 Vorrichtung und verfahren zur lufttrennung durch kryogene destillation

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US (1) US20110041552A1 (de)
EP (1) EP2279385B1 (de)
JP (1) JP2011519010A (de)
CN (1) CN102016470A (de)
AT (1) ATE546701T1 (de)
FR (1) FR2930629B1 (de)
WO (1) WO2009136081A2 (de)
ZA (1) ZA201007374B (de)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6155515B2 (ja) * 2014-06-24 2017-07-05 大陽日酸株式会社 空気分離方法、及び空気分離装置
EP2993432A1 (de) * 2014-09-02 2016-03-09 Linde Aktiengesellschaft Verfahren zur tieftemperaturzerlegung von luft und luftzerlegungsanlage
CN109520207B (zh) * 2017-09-18 2022-04-08 乔治洛德方法研究和开发液化空气有限公司 用于通过低温蒸馏分离空气的方法和单元
CN108302899A (zh) * 2018-03-29 2018-07-20 浙江新锐空分设备有限公司 一种利用液化空气提取贫氪氙产品的空分系统及方法
CN113465292B (zh) * 2021-07-05 2023-02-21 乔治洛德方法研究和开发液化空气有限公司 一种增加空气精馏装置氪/氙产量的方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5956974A (en) * 1998-01-22 1999-09-28 Air Products And Chemicals, Inc. Multiple expander process to produce oxygen
GB9902101D0 (en) * 1999-01-29 1999-03-24 Boc Group Plc Separation of air
FR2795496B1 (fr) * 1999-06-22 2001-08-03 Air Liquide Appareil et procede de separation d'air par distillation cryogenique
FR2807150B1 (fr) * 2000-04-04 2002-10-18 Air Liquide Procede et appareil de production d'un fluide enrichi en oxygene par distillation cryogenique
FR2844039B1 (fr) * 2002-09-04 2005-04-29 Air Liquide Procede et installation de production d'oxygene et de gaz rares par distillation cryogenique d'air
US7296437B2 (en) * 2002-10-08 2007-11-20 L'air Liquide, Societe Anonyme A Directoire Et Conseil De Surveillance Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for separating air by cryogenic distillation and installation for implementing this process
US6662593B1 (en) * 2002-12-12 2003-12-16 Air Products And Chemicals, Inc. Process and apparatus for the cryogenic separation of air

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ZA201007374B (en) 2011-06-29
US20110041552A1 (en) 2011-02-24
EP2279385A2 (de) 2011-02-02
WO2009136081A2 (fr) 2009-11-12
JP2011519010A (ja) 2011-06-30
CN102016470A (zh) 2011-04-13
ATE546701T1 (de) 2012-03-15
WO2009136081A3 (fr) 2010-04-08
FR2930629A1 (fr) 2009-10-30
FR2930629B1 (fr) 2010-05-07

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