EP1162424A2 - Procédé et installation de production d'argon - Google Patents

Procédé et installation de production d'argon Download PDF

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Publication number
EP1162424A2
EP1162424A2 EP01113971A EP01113971A EP1162424A2 EP 1162424 A2 EP1162424 A2 EP 1162424A2 EP 01113971 A EP01113971 A EP 01113971A EP 01113971 A EP01113971 A EP 01113971A EP 1162424 A2 EP1162424 A2 EP 1162424A2
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EP
European Patent Office
Prior art keywords
column
argon
pressure
crude
crude argon
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.)
Granted
Application number
EP01113971A
Other languages
German (de)
English (en)
Other versions
EP1162424B1 (fr
EP1162424A3 (fr
Inventor
Theo Sentis
Joachim Krey
Thorsten Möller
Jens Juckel
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.)
Air Liquide AGS GmbH
Original Assignee
Messer AGS 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 Messer AGS GmbH filed Critical Messer AGS GmbH
Publication of EP1162424A2 publication Critical patent/EP1162424A2/fr
Publication of EP1162424A3 publication Critical patent/EP1162424A3/fr
Application granted granted Critical
Publication of EP1162424B1 publication Critical patent/EP1162424B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
    • F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
    • 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
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04684—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser and a bottom re-boiler
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04793—Rectification, e.g. columns; Reboiler-condenser
    • F25J3/048—Argon recovery
    • 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
    • F25J2235/58—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
    • 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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/12—Particular process parameters like pressure, temperature, ratios

Definitions

  • the invention relates to a method and an apparatus for the production of argon, at the compressed, pre-cleaned and cooled air in a rectification system at least one rectification column and one crude argon column is broken down, according to the Features of the preamble of claims 1 and 6.
  • Such a method with a device for the production of argon with up to 10 ppm Contamination content is known from EP 0 377 117 B2, in which one from the so-called argon belly area of a low-pressure column of a two-stage Rectification withdrawn argon-rich oxygen fraction one with one Raw argon condenser supplied equipped in raw argon column and in this same pressure conditions as in the low pressure column by means of at least 150 theoretical floors (levels) as well as structured packings or packing in gaseous raw argon and in a heavy-boiling first liquid residual fraction disassembled, the crude argon of a further fine cleaning in a conventional Way with bottoms and with a top condenser and with a sump evaporator equipped pure argon column for the production of pure argon.
  • EP 0 628 777 B1 describes a method and an apparatus for Obtaining argon with up to 10 ppm residual oxygen known, in which the from the separation of air in a rectification system with at least one Rectification column obtained argon-containing oxygen fraction in a crude argon column and a semi-pure column equipped with a crude argon condenser into one Argon product is broken down, the residual fraction of the semi-pure column as Return liquid for the crude argon column is used, the number of to Argon rectification used theoretical soils in the form of conventional soils and / or ordered packings and / or packing in the crude argon / semi-pure column is at least 30 or 60, so that no crude argon condenser in the Crude argon column is required, which reduces the expenditure on equipment and the Operating costs can be reduced.
  • the invention has for its object a method and an apparatus initially mentioned type with little equipment and low Operating costs available for the particularly economical extraction of raw argon to deliver.
  • the raw argon present at the top of the raw argon column is replaced by indirect Heat exchange with a liquid removed from the process condenses and at least partially fed back into the columns as reflux liquid. A part the condensed crude argon fraction is withdrawn as a product and for further processing Treatment of the pure argon column.
  • any liquid air fraction present is at least partially fed into the pressure column, since this measure also Reduced oxygen concentration in the bath of the top condenser of the crude argon column.
  • the reflux conditions in the crude argon column are those in the lower column area liquid residual fraction (bottom product) evaporated at least partially.
  • Sump heating can also be particularly advantageous in the air separation plant existing high pressure air flow from 10 to 100 bar before its relaxation and Allocation to other rectification columns can be used.
  • the raw argon liquefied at the top of the raw argon column is subjected to a fine cleaning in one with a variable number of arranged in different areas conventional floors and / or ordered packings and / or packing, one Pure argon condenser and a bottom evaporator equipped pure argon column subjected to the raw argon in pure argon and in a second low-boiling Residual fraction is broken down.
  • the gaseous nitrogen-argon mixture present at the top of the pure argon column is achieved through indirect heat exchange in the pure argon condenser (top condenser Pure argon column) liquefied, with the liquefied fraction returning to the Pure argon column fed and the non-liquefied portion as a gaseous flushing stream is blown off into the system environment.
  • the invention also relates to a device for the production of argon according to the Features of claims 6 to 9.
  • the argon production which is reduced in pressure according to the invention, can be significantly improved reduced number of theoretical floors in the form of in a variable number in conventional floors arranged in different areas of the crude argon column and / or orderly packings and / or fillers, thereby reducing the overall height the crude argon column significantly reduced and thus the apparatus and process engineering Effort is reduced, so that an inexpensive production of argon is guaranteed with 0.1 to 10 ppm residual oxygen.
  • the figure of the drawing shows a process diagram of an argon production according to the invention.
  • the crude argon 6 present at the top of the crude argon column 5 with 0.1 to 10 ppm Residual oxygen content is obtained through indirect heat exchange with one from the process withdrawn liquid condensed and at least partially as reflux liquid fed back into the raw argon column 5.
  • condensation of crude argon 6 from the bottom of the pressure column 1 Liquid supplied via line 9 is used to do this via a valve in the room a raw argon condenser 10 is expanded into it.
  • Part of the condensed Crude argon fraction is via line 15 as a low-oxygen crude argon precursor withdrawn and fed to a pure argon column 16 for further treatment.
  • the one in the bottom Liquid residual fraction 7 present at least partially in the region of the crude argon column 5 evaporated in an evaporator by a process stream.
  • Evaporating agent withdrawn from the bottom of the pressure column 1 oxygen-rich Use liquid only after passing the evaporator and before the entry into the crude argon condenser 10 is relaxed.
  • An existing one in the air separation plant can also be particularly advantageous a pressure of 10 to 100 bar air flow to operate the bottom evaporator 11 are used in the raw argon column 5. This high pressure air flow is relaxed only after passing the evaporator and on the pressure and Low pressure column 1, 2 divided. The portion not evaporated in the crude argon column 5 liquid residual fraction 7 is fed back by means of a conveyor 14 via a Line 13 fed back into the low pressure column 2.
  • a part of the raw argon 6 liquefied in the raw argon condenser 10 is called low-oxygen argon precursor with a residual oxygen content of 0.1 to 10 ppm fed via line 15 into the pure argon column 16.
  • the pure argon column 16 is arranged so far below the crude argon condenser 10 that the geodetic height of the liquid column of pure argon the pressure difference between the crude argon and pure argon column 5, 16 and that during transport of the liquid compensates for any pressure losses.
  • the pure argon column 16 is variable Number of differently arranged conventional floors and / or ordered Packings and / or fillers equipped and separates the incoming low-oxygen Crude argon product in an argon-nitrogen mixture 17 and in an oxygen and low nitrogen pure argon product, which is a liquid pure argon product 27 from the Bottom of the pure argon column 16 is withdrawn.
  • the gaseous argon-nitrogen mixture present at the top of the pure argon column 16 17 is partially by indirect heat exchange in a pure argon condenser 21 liquefied, the liquefied fraction as reflux back into the pure argon column 16 is fed and the non-liquefied portion as a gaseous nitrogen purge stream is blown off into the plant environment via a line 22.
  • a pure argon condenser 21 finds one from the pressure column 1 via a line 23 supplied gaseous fraction use, which is initially in a Pure argon evaporator 24 condenses before one with one over one Relaxation valve 25 provided line 26 into the pure argon condenser 21 is relaxed.
  • a liquid residual fraction 18 obtained in the bottom of the pure argon column 16 becomes partial evaporated in the pure argon evaporator 24 and the non-evaporated liquid portion as liquid pure argon product 27 deducted.
  • the argon production according to the invention is with or without additional crude argon column bottom evaporation in all common air separation plants with one Rectification system with at least one rectification column and one crude argon column with the advantages shown.

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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)
EP01113971A 2000-06-10 2001-06-08 Procédé et installation de production d'argon Expired - Lifetime EP1162424B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10028871 2000-06-10
DE10028871A DE10028871A1 (de) 2000-06-10 2000-06-10 Verfahren und Vorrichtung zur Gewinnung von Argon

Publications (3)

Publication Number Publication Date
EP1162424A2 true EP1162424A2 (fr) 2001-12-12
EP1162424A3 EP1162424A3 (fr) 2002-01-09
EP1162424B1 EP1162424B1 (fr) 2009-02-25

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP01113971A Expired - Lifetime EP1162424B1 (fr) 2000-06-10 2001-06-08 Procédé et installation de production d'argon

Country Status (3)

Country Link
EP (1) EP1162424B1 (fr)
AT (1) ATE423951T1 (fr)
DE (2) DE10028871A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007192466A (ja) * 2006-01-19 2007-08-02 Nippon Steel Corp 深冷空気分離装置およびその制御方法
FR3107341A1 (fr) * 2020-02-18 2021-08-20 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé et appareil de séparation d’air par distillation cryogénique

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0341512A1 (fr) * 1988-04-29 1989-11-15 Air Products And Chemicals, Inc. Système de régulation pour maximiser la récupération de l'argon des unités cryogéniques de séparation d'air
EP0538520A1 (fr) * 1991-10-22 1993-04-28 Odessky Institut Nizkotemperaturnoi Tekhniki I Energetiki Procédé de séparation d'air
EP0594214A1 (fr) * 1992-10-23 1994-04-27 Praxair Technology, Inc. Procédé de rectification cryogénique intégré thermiquement à une colonne d'argon
EP0684437A1 (fr) * 1994-05-27 1995-11-29 The BOC Group plc Séparation d'air
US5592833A (en) * 1994-02-24 1997-01-14 Linde Aktiengesellschaft Process and apparatus for the recovery of pure argon
EP0786633A1 (fr) * 1995-06-20 1997-07-30 Nippon Sanso Corporation Procede et appareil de separation de l'argon
EP1055891A1 (fr) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Système de séparation cryogénique pour la séparation des gaz de l'air

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4406051A1 (de) * 1994-02-24 1995-08-31 Linde Ag Verfahren und Vorrichtung zur Gewinnung von reinem Argon

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0341512A1 (fr) * 1988-04-29 1989-11-15 Air Products And Chemicals, Inc. Système de régulation pour maximiser la récupération de l'argon des unités cryogéniques de séparation d'air
EP0538520A1 (fr) * 1991-10-22 1993-04-28 Odessky Institut Nizkotemperaturnoi Tekhniki I Energetiki Procédé de séparation d'air
EP0594214A1 (fr) * 1992-10-23 1994-04-27 Praxair Technology, Inc. Procédé de rectification cryogénique intégré thermiquement à une colonne d'argon
US5592833A (en) * 1994-02-24 1997-01-14 Linde Aktiengesellschaft Process and apparatus for the recovery of pure argon
EP0684437A1 (fr) * 1994-05-27 1995-11-29 The BOC Group plc Séparation d'air
EP0786633A1 (fr) * 1995-06-20 1997-07-30 Nippon Sanso Corporation Procede et appareil de separation de l'argon
EP1055891A1 (fr) * 1999-05-25 2000-11-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Système de séparation cryogénique pour la séparation des gaz de l'air

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007192466A (ja) * 2006-01-19 2007-08-02 Nippon Steel Corp 深冷空気分離装置およびその制御方法
FR3107341A1 (fr) * 2020-02-18 2021-08-20 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé et appareil de séparation d’air par distillation cryogénique

Also Published As

Publication number Publication date
DE50114720D1 (de) 2009-04-09
EP1162424B1 (fr) 2009-02-25
EP1162424A3 (fr) 2002-01-09
DE10028871A1 (de) 2001-12-20
ATE423951T1 (de) 2009-03-15

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