EP0611936B1 - Verfahren und Anlage zur Herstellung von ultrareinem Stickstoff durch Luftdestillation - Google Patents

Verfahren und Anlage zur Herstellung von ultrareinem Stickstoff durch Luftdestillation Download PDF

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Publication number
EP0611936B1
EP0611936B1 EP94400257A EP94400257A EP0611936B1 EP 0611936 B1 EP0611936 B1 EP 0611936B1 EP 94400257 A EP94400257 A EP 94400257A EP 94400257 A EP94400257 A EP 94400257A EP 0611936 B1 EP0611936 B1 EP 0611936B1
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Prior art keywords
column
nitrogen
reboiler
condenser
bottom liquid
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EP94400257A
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English (en)
French (fr)
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EP0611936A1 (de
Inventor
Pascal Arriulou
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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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
    • F25J3/04763—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
    • F25J3/04781—Pressure changing devices, e.g. for compression, expansion, liquid pumping
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • 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
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • 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
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • 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
    • F25J2215/10—Hydrogen
    • 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
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
    • F25J2240/10—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream the 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
    • 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
    • F25J2240/42—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval the 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • F25J2250/42—One fluid being nitrogen
    • 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
    • F25J2250/50—One fluid being oxygen
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/939—Partial feed stream expansion, air

Definitions

  • the invention aims to add a degree of freedom to the process by allowing the reflux rates of the two columns to be adjusted independently, in particular in order to reduce the size of the second column, and therefore the corresponding investment.
  • the subject of the invention is a process of the aforementioned type, characterized in that a second flow of nitrogen from the high pressure cycle is condensed by vaporization of tank liquid from the first column and at least part of the condensed nitrogen by vaporization of the bottom liquid from the first column is introduced under reflux at the head of the first column.
  • the invention also relates to an installation intended for the implementation of such a method.
  • This installation of the type comprising a double distillation column which itself comprises a first nitrogen / oxygen separation column supplied by the air to be treated, and a second nitrogen / hydrogen separation column whose head is coupled to the tank of the first column by a vaporizer- condenser and which comprises a tank vaporizer, means for drawing off a gas enriched in hydrogen, and a nitrogen refrigeration cycle the high pressure part of which feeds the tank vaporizer of the second column then this second column itself, means for expanding liquid from the bottom of the second column and for introducing it into the first column, means for withdrawing the ultra-pure nitrogen from the production of the second column, characterized in that it also comprises means for condensing high pressure cycle nitrogen by vaporizing the liquid from the bottom of the first column, and means for introducing into reflux at the top of the first column at least part of the liquid zote from said means of condensation.
  • the installation shown in FIG. 1 essentially comprises an atmospheric air compressor 1, an apparatus 2 for purifying the air of water and CO 2 by adsorption, a heat exchange line 3, a turbine 4 for expansion air, a double distillation column 5, consisting itself of an oxygen / nitrogen separation column 6 and of a nitrogen / hydrogen separation column 7, and a sub-cooler 8.
  • Column 6 includes a head condenser 9 and a tank vaporizer 10, which also serves as a head condenser for column 7. The latter is also equipped with a tank vaporizer 11.
  • the installation also includes a nitrogen refrigeration cycle 12, the cycle compressor of which is indicated at 13.
  • the air to be treated, compressed at 1 and purified at 2 is cooled at 3 to an intermediate temperature T.
  • T the air to be treated, compressed at 1 and purified at 2
  • the air to be treated is cooled at 3 to an intermediate temperature T.
  • T the air to be treated, compressed at 1 and purified at 2
  • a bypass 15 of the turbine 4, equipped with an expansion valve 16 makes it possible to adjust the cooling power thus produced.
  • the resulting gas LRV (liquid rich vaporized) is then warmed to room temperature in 3 and then discharged from the installation, as waste gas, via a line 18.
  • liquid from the bottom of the column 7 is also, after sub-cooling at 8 and expansion in an expansion valve 22, introduced at the top of the column 6.
  • the air is separated in column 6 into a liquid rich in oxygen and in cycle nitrogen, and part of the cycle nitrogen is purified into hydrogen in column 7.
  • the separated hydrogen is evacuated from the vaporizer-condenser 10 via a vent 23 provided in its condensation passages of the head gas of the column 7.
  • ultra-pure nitrogen for example at a hydrogen concentration of less than 10 -9 (1 ppb), which is collected in the tank of column 7, and a production rate of Ultra-pure gaseous nitrogen is drawn off at the bottom of this column via a line 24, warmed to ambient temperature at 3 and recovered via a production line 25.
  • ordinary purity nitrogen for example at a hydrogen concentration of the order of ppm (10 -6 )
  • the invention is particularly advantageous when the ultra-pure nitrogen to be produced represents only a fraction of the total nitrogen production of the installation.

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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)

Claims (8)

  1. Verfahren zur Herstellung von ultrareinem Stickstoff durch Destillation von Luft, bei dem:
    - die zu verarbeitende Luft in einer ersten Kolonne (6) in Stickstoff am Kopf und in sauerstoffreiche Flüssigkeit am Sumpf zerlegt wird;
    - der Stickstoff am Kopf in einem Kältekreis zirkuliert, wobei ein Stickstoffstrom aus dem Hochdruckteil des Kreises in einer zweiten Kolonne (7), umfassend einen Verdampfer (11) im Sumpf, der für die Kondensation dieses Stickstoffs vor dessen Einleitung in diese zweite Kolonne sorgt, und einen Kopfkondensator (10), der durch die Flüssigkeit im Sumpf der ersten Kolonne (6) gekühlt wird, von Wasserstoff gereinigt wird;
    - Flüssigkeit aus dem Sumpf der zweiten Kolonne (7) nach einer Entspannungsstufe in die erste Kolonne (6) eingeleitet wird;
    - der ultrareine Produktionsstickstoff der zweiten Kolonne (7) entnommen wird (bei 24) und zumindest ein Teil des durch Verdampfen von Flüssigkeit im Sumpf der ersten Kolonne (6) kondensierten Stickstoffs in der zweiten Kolonne (7) von Wasserstoff gereinigt wird,
    dadurch gekennzeichnet, daß ein zweiter Stickstoffstrom aus dem Hochdruckteil des Kreises durch Verdampfen von Flüssigkeit im Sumpf der ersten Kolonne (6) kondensiert wird (bei 10; 10A) und zumindest ein Teil des durch Verdampfen von Flüssigkeit im Sumpf der ersten Kolonne (6) kondensierten Stickstoffs als Rückfluß am Kopf der ersten Kolonne (6) eingeleitet wird.
  2. Verfahren nach Anspruch 1, bei dem zumindest ein Teil des durch Verdampfen von Flüssigkeit im Sumpf der ersten Kolonne (6) kondensierten Stickstoffs in die zweite Kolonne (7) eingeleitet wird.
  3. Verfahren nach Anspruch 1 oder 2, bei dem ein einstellbarer Teil der Luft einem Bypassventil (16) einer Luftentspannungsturbine (4) zugeführt wird.
  4. Vorrichtung zur Herstellung von ultrareinem Stickstoff durch Destillation von Luft, umfassend eine Doppel-Destillationskolonne (5), die selbst wiederum eine erste Kolonne (6) zur Zerlegung in Stickstoff/Sauerstoff, die durch die zu verarbeitende Luft gespeist wird, und eine zweite Kolonne (7) zur Zerlegung in Stickstoff/Wasserstoff umfaßt, deren Kopf mit dem Sumpf der ersten Kolonne über einen Verdampfer-Kondensator (10) verbunden ist und die einen Verdampfer (11) im Sumpf umfaßt, Mittel zum Entnehmen eines mit Wasserstoff angereicherten Gases und einen Stickstoffkältekreis (12), dessen Hochdruckteil den Verdampfer (11) im Sumpf der zweiten Kolonne (7) und dann diese zweite Kolonne selbst speist, Mittel (22) zum Entspannen von Flüssigkeit aus dem Sumpf der zweiten Kolonne und zum Einleiten derselben in die erste Kolonne, Mittel (24) zum Entnehmen des ultrareinen Produktionsstickstoffs aus der zweiten Kolonne (7), dadurch gekennzeichnet, daß sie außerdem Mittel (10; 10A) zum Kondensieren des Stickstoffs aus dem Hochdruckkreis durch Verdampfen von Flüssigkeit im Sumpf der ersten Kolonne (6) und Mittel zum Einleiten zumindest eines Teils des aus den genannten Kondensationsmitteln (10) stammenden flüssigen Stickstoffs als Rückfluß am Kopf der ersten Kolonne (6) umfaßt.
  5. Vorrichtung nach Anspruch 4, dadurch gekennzeichnet, daß die Kondensationsmittel in dem Verdampfer-Kondensator (10) vorgesehene Durchlässe für Stickstoff aus dem Hochdruckkreis umfassen.
  6. Vorrichtung nach Anspruch 4, dadurch gekennzeichnet, daß die Kondensationsmittel einen Hilfs-Verdampfer-Kondensator (10A), der parallel zu dem Verdampfer-Kondensator (10) der ersten Kolonne (6) angebracht ist, umfassen.
  7. Vorrichtung nach Anspruch 6, dadurch gekennzeichnet, daß der Hilfs-Verdampfer-Kondensator (10A) außerhalb der ersten Kolonne (6) angebracht ist.
  8. Vorrichtung nach einem der Ansprüche 4 bis 7, dadurch gekennzeichnet, daß sie Mittel zum Einleiten zumindest eines Teils des aus den Kondensationsvorrichtungen (10) stammenden flüssigen Stickstoffs in die zweite Kolonne (7) umfaßt.
EP94400257A 1993-02-09 1994-02-07 Verfahren und Anlage zur Herstellung von ultrareinem Stickstoff durch Luftdestillation Expired - Lifetime EP0611936B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9301403 1993-02-09
FR9301403A FR2701313B1 (fr) 1993-02-09 1993-02-09 Procédé et installation de production d'azote ultra-pur par distillation d'air.

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EP0611936A1 EP0611936A1 (de) 1994-08-24
EP0611936B1 true EP0611936B1 (de) 1997-05-14

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Country Link
US (1) US5440885A (de)
EP (1) EP0611936B1 (de)
JP (1) JPH06241651A (de)
CA (1) CA2115129A1 (de)
DE (1) DE69403103T2 (de)
FR (1) FR2701313B1 (de)

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US5208534A (en) * 1989-08-09 1993-05-04 Kabushiki Kaisha Toshiba Magnetic resonance imaging system
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US5611219A (en) * 1996-03-19 1997-03-18 Praxair Technology, Inc. Air boiling cryogenic rectification system with staged feed air condensation
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DE69403103D1 (de) 1997-06-19
JPH06241651A (ja) 1994-09-02
CA2115129A1 (fr) 1994-08-10
FR2701313B1 (fr) 1995-03-31
EP0611936A1 (de) 1994-08-24
US5440885A (en) 1995-08-15
FR2701313A1 (fr) 1994-08-12
DE69403103T2 (de) 1997-10-16

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