EP1006326B1 - Verfahren und Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft - Google Patents

Verfahren und Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft Download PDF

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Publication number
EP1006326B1
EP1006326B1 EP99102628A EP99102628A EP1006326B1 EP 1006326 B1 EP1006326 B1 EP 1006326B1 EP 99102628 A EP99102628 A EP 99102628A EP 99102628 A EP99102628 A EP 99102628A EP 1006326 B1 EP1006326 B1 EP 1006326B1
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EP
European Patent Office
Prior art keywords
krypton
column
oxygen
xenon
pressure
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.)
Expired - Lifetime
Application number
EP99102628A
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German (de)
English (en)
French (fr)
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EP1006326A1 (de
Inventor
Stefan Dipl.-Ing. Lochner
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Linde GmbH
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Linde GmbH
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Publication date
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Publication of EP1006326B1 publication Critical patent/EP1006326B1/de
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Expired - Lifetime 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
    • 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
    • F25J3/04642—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
    • F25J2200/92—Details relating to the feed 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
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen

Definitions

  • the invention is based on a process for obtaining pressurized oxygen, at the compressed and pre-cleaned feed air is introduced into the rectification system and a first oxygen fraction taken from the low pressure column, liquid onto one brought increased pressure, evaporated and as a gaseous pressurized oxygen product is dissipated.
  • the invention has for its object in such a method and in a corresponding device in addition to the pressurized oxygen product on Krypton and to obtain xenon-enriched product in an economically advantageous manner.
  • the Bottom fraction of the low pressure column (the second oxygen fraction) in a krypton-xenon enrichment column (Methane discharge column) initiated on its head Low krypton / xenon liquid oxygen is given up. So the methane, that accumulates in the bottom of the low pressure column via the gaseous Top product of the methane discharge column are removed from the process.
  • the Bottom product of the methane discharge column contains only extremely small amounts methane and is enriched in krypton and xenon.
  • the krypton-xenon enrichment column (which may be called Methane discharge column works) operated under an increased pressure, which preferably corresponds approximately to the desired product pressure in the pressurized oxygen.
  • the operating pressure of the krypton-xenon enrichment column is, for example, 1.5 up to 10 bar, preferably at 2.5 to 7 bar.
  • the liquid oxygen from which the Pressurized oxygen product is formed (the first oxygen fraction) will not like usually deducted from their sump, but above a mass transfer section, which keeps krypton and xenon in the sump of the low pressure column. It forms the Low-krypton / xenon return liquid for the krypton-xenon enrichment column.
  • the mass transfer section below the deduction of the first oxygen fraction is by at least one, preferably one to five, most preferably one to three rectification trays formed, which are arranged directly above the low pressure column sump.
  • a two or more column system for nitrogen-oxygen separation is preferred in the invention used, in addition to the low pressure column Has high pressure column, which is under higher pressure than the low pressure column is operated.
  • the high-pressure column and the low-pressure column are preferably one common condenser-evaporator (main condenser) thermally coupled, in the nitrogen-rich vapor of the high pressure column against an evaporating one condensed oxygen-rich liquid from the low pressure column.
  • the invention is however, it can also be implemented in a single column system in which the low pressure column is formed by a single column.
  • the use of the term low pressure column does not necessarily mean that this column is operated at about atmospheric pressure becomes. It can be used for single, two and multi-column processes Low pressure column can also be operated under increased pressure.
  • the operating pressure the low pressure column is, for example, 1.1 to 4 bar, preferably 1.1 to 2.0 bar.
  • the krypton-xenon enrichment column is below the critical pressure operated by oxygen, depending on the product pressure, for example at 2 to 10 bar, preferably at 5 to 6 bar.
  • the first oxygen fraction is not directly at the bottom of the low pressure column, but at least one practical or theoretical floor above the swamp or taken above the removal of the second oxygen fraction.
  • the information in practical terms applies Plate numbers; if packing, packing or combinations of different types of Mass transfer elements are used, the information is in theoretical Any number can be used to increase the pressure in the liquid state known means or a combination of different known means be used.
  • Krypton-xenon enrichment column results from the inventive method an increase in the yield of krypton and / or Xenon by 20 to 25%.
  • the second fraction of oxygen must be introduced into the krypton-xenon enrichment column are brought to their operating pressure.
  • the second oxygen fraction before being introduced into the krypton-xenon enrichment column however brought to an increased pressure in the liquid state and then introduced liquid into the krypton-xenon enrichment column.
  • the bottom evaporator is the krypton-xenon enrichment column is operated by indirect heat exchange with a partial flow of the feed air.
  • the feed air preferably condenses at least in the bottom evaporator partially.
  • the condensate generated during indirect heat exchange will for example introduced into one of the columns of the rectification system, preferably into the low pressure column.
  • the feed air used as heating medium is preferably upstream of the Bottom evaporator is brought to a pressure which is higher than the highest Operating pressure of the columns of the rectification system is.
  • This pressure is chosen that the condensation temperature of the feed air in the bottom evaporator, for example about 1 to 2 K above the evaporation temperature of the bottom liquid of the krypton-xenon enrichment column lies.
  • This can be achieved, for example, by that the entire feed air is compressed to a very high pressure (for example to high pressure column pressure in the case of a two column system) or that the partial flow used as a heating medium is of a lower level (for example high pressure column pressure) is compressed to this high pressure.
  • a first oxygen fraction 11 is three floors above the Low pressure column sump removed liquid, by means of a pump 12 to one Brought pressure of 9 bar, subcooled in a second countercurrent and over Line 14 abandoned on the head of a krypton-xenon enrichment column 15.
  • the feed point is three trays above the bottom of the krypton-xenon enrichment column 15th
  • a krypton-xenon preconcentrate is made from the bottom of the krypton-xenon enrichment column 15 19 deducted as a krypton and / or xenon enriched fraction. It can be collected in a tank or directly for further process steps Extraction of krypton and / or xenon can be supplied.
  • the head gas 24 of the Krypton-xenon enrichment column 15 forms the pressurized oxygen product and is in the Main heat exchanger warmed against feed air (not shown).
  • the krypton-xenon enrichment column 15 is through indirect heat exchange 20 heated with a second cleaned and cooled feed air stream 21, the under a pressure of 22 bar.
  • the resulting condensate 22 is in the second Counterflow 13 warmed and the high pressure column 2 some floors above the Feed of the first feed air stream 4 fed (23).

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP99102628A 1998-12-01 1999-02-11 Verfahren und Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft Expired - Lifetime EP1006326B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19855487A DE19855487A1 (de) 1998-12-01 1998-12-01 Verfahren und Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft
DE19855487 1998-12-01

Publications (2)

Publication Number Publication Date
EP1006326A1 EP1006326A1 (de) 2000-06-07
EP1006326B1 true EP1006326B1 (de) 2004-04-21

Family

ID=7889673

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99102628A Expired - Lifetime EP1006326B1 (de) 1998-12-01 1999-02-11 Verfahren und Vorrichtung zur Gewinnung von Drucksauerstoff und Krypton/Xenon durch Tieftemperaturzerlegung von Luft

Country Status (8)

Country Link
US (1) US6301929B1 (zh)
EP (1) EP1006326B1 (zh)
JP (1) JP2000180050A (zh)
KR (1) KR100660243B1 (zh)
CN (1) CN1123754C (zh)
DE (2) DE19855487A1 (zh)
DK (1) DK1006326T3 (zh)
ES (1) ES2219942T3 (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009014556A1 (de) 2009-03-24 2010-09-30 Linde Aktiengesellschaft Verfahren zur Beheizung einer Trennkolonne
EP2312248A1 (de) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Verfahren und Vorrichtung Gewinnung von Drucksauerstoff und Krypton/Xenon
CN105387684A (zh) * 2014-09-02 2016-03-09 林德股份公司 低温分馏空气的方法和空气分馏设备

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10153252A1 (de) * 2001-10-31 2003-05-15 Linde Ag Verfahren und Vorrichtung zur Gewinnung von Krypton und/oder Xenon durch Tieftemperaturzerlegung von Luft
DE10228111A1 (de) * 2002-06-24 2004-01-15 Linde Ag Luftzerlegungsverfahren und -anlage mit Mischsäule und Krypton-Xenon-Gewinnung
US6694775B1 (en) * 2002-12-12 2004-02-24 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon
CN101634514B (zh) * 2009-08-13 2012-01-25 上海启元科技发展有限公司 全精馏制备纯氪和纯氙的方法
CN101913580B (zh) * 2010-07-16 2012-12-19 杭州杭氧股份有限公司 从液氧中提取惰性气体氪氙的方法与装置
CN102721262A (zh) * 2012-07-04 2012-10-10 开封空分集团有限公司 粗氪氙的提取装置及利用该装置提取粗氪氙的工艺
CN103968641B (zh) * 2014-05-19 2019-04-02 上海启元空分技术发展股份有限公司 一种控制氪氙精馏塔入塔气体流量的方法
US11460246B2 (en) * 2019-12-18 2022-10-04 Air Products And Chemicals, Inc. Recovery of krypton and xenon from liquid oxygen
CN117531333B (zh) * 2024-01-08 2024-04-02 西安瑞恒测控设备有限公司 气相色谱仪在氪氙检测中的过滤系统

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB969799A (en) * 1962-02-27 1964-09-16 Roman Stoklosinski Improvements in the recovery of krypton and xenon from air separation plants
GB8610766D0 (en) * 1986-05-02 1986-06-11 Colley C R Yield of krypton xenon in air separation
US5122173A (en) * 1991-02-05 1992-06-16 Air Products And Chemicals, Inc. Cryogenic production of krypton and xenon from air
US5067976A (en) * 1991-02-05 1991-11-26 Air Products And Chemicals, Inc. Cryogenic process for the production of an oxygen-free and methane-free, krypton/xenon product
US5309719A (en) * 1993-02-16 1994-05-10 Air Products And Chemicals, Inc. Process to produce a krypton/xenon enriched stream from a cryogenic nitrogen generator
DE4332870C2 (de) * 1993-09-27 2003-02-20 Linde Ag Verfahren und Vorrichtung zur Gewinnung eines Krypton-/Xenon-Konzentrats durch Tieftemperaturzerlegung von Luft

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009014556A1 (de) 2009-03-24 2010-09-30 Linde Aktiengesellschaft Verfahren zur Beheizung einer Trennkolonne
EP2312248A1 (de) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Verfahren und Vorrichtung Gewinnung von Drucksauerstoff und Krypton/Xenon
CN105387684A (zh) * 2014-09-02 2016-03-09 林德股份公司 低温分馏空气的方法和空气分馏设备
CN105387684B (zh) * 2014-09-02 2021-02-26 林德股份公司 低温分馏空气的方法和空气分馏设备

Also Published As

Publication number Publication date
ES2219942T3 (es) 2004-12-01
US6301929B1 (en) 2001-10-16
CN1255620A (zh) 2000-06-07
KR100660243B1 (ko) 2006-12-20
DE19855487A1 (de) 2000-06-08
CN1123754C (zh) 2003-10-08
JP2000180050A (ja) 2000-06-30
DK1006326T3 (da) 2004-08-09
EP1006326A1 (de) 2000-06-07
DE59909230D1 (de) 2004-05-27
KR20000047816A (ko) 2000-07-25

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