EP4619693A2 - Procédé de séparation cryogénique d'air et système de séparation d'air - Google Patents

Procédé de séparation cryogénique d'air et système de séparation d'air

Info

Publication number
EP4619693A2
EP4619693A2 EP23813562.8A EP23813562A EP4619693A2 EP 4619693 A2 EP4619693 A2 EP 4619693A2 EP 23813562 A EP23813562 A EP 23813562A EP 4619693 A2 EP4619693 A2 EP 4619693A2
Authority
EP
European Patent Office
Prior art keywords
liquid
pressure
column
low
gas
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.)
Pending
Application number
EP23813562.8A
Other languages
German (de)
English (en)
Inventor
Thomas Nohlen
Ralph Spöri
Dimitri GOLUBEV
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Linde GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PCT/EP2022/025517 external-priority patent/WO2023110142A1/fr
Application filed by Linde GmbH filed Critical Linde GmbH
Publication of EP4619693A2 publication Critical patent/EP4619693A2/fr
Pending legal-status Critical Current

Links

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
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/0406—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. 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
    • F25J3/04006—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
    • F25J3/04084—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 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
    • F25J3/04006—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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
    • F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
    • F25J3/04175—Hot end purification of the feed air by adsorption of the impurities at a pressure of substantially more than the highest pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
    • 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
    • F25J3/04721—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
    • F25J3/04763—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
    • 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
    • F25J3/04806—High purity argon purification
    • 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
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04884—Arrangement of reboiler-condensers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J5/00—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants
    • F25J5/002—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger
    • F25J5/005—Arrangements of cold exchangers or cold accumulators in separation or liquefaction plants for continuously recuperating cold, i.e. in a so-called recuperative heat exchanger in a reboiler-condenser, e.g. within a column
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    • 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
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
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    • 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
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/54—Oxygen production with multiple pressure O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • 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
    • F25J2240/46—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 oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • 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
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger

Definitions

  • the present invention relates to a process for the low-temperature separation of air and an air separation plant according to the respective preambles of the independent patent claims.
  • Air separation plants have rectification column arrangements that can be designed in different ways.
  • rectification columns for obtaining nitrogen and/or oxygen in liquid and/or gaseous state i.e. rectification columns for nitrogen-oxygen separation, which can be combined in a known double column
  • rectification columns can be provided for obtaining other air components, in particular noble gases, or pure oxygen.
  • the rectification columns of typical rectification column arrangements are operated at different pressure levels.
  • Known double columns have a so-called pressure column (also referred to as high-pressure column, medium-pressure column or lower column) and a so-called low-pressure column (upper column).
  • the high-pressure column is typically operated at a pressure level of 4 to 7 bar, in particular approx. 5.3 bar, while the low-pressure column is typically operated at a pressure level of 1 to 2 bar, in particular approx. 1.4 bar. In certain cases, higher pressure levels can also be used in these rectification columns.
  • the pressures specified here and below are absolute pressures at the top of the rectification columns specified in each case. Air separation plants with crude and pure argon columns can be used to produce argon.
  • the crude argon column essentially serves to separate the oxygen from the gas withdrawn from the crude argon column.
  • the oxygen separated in the crude argon column or a corresponding oxygen-rich fluid can be returned to the low-pressure column in liquid form.
  • a gaseous fraction remaining in the crude argon column during the separation, which essentially contains argon and nitrogen, can be further separated in a pure argon column to obtain pure argon.
  • the crude and optionally the pure argon column have top condensers which can be cooled in particular with a portion of a liquid (so-called "enriched liquid") withdrawn from the pressure column, enriched in oxygen and depleted in nitrogen, which partially evaporates during this cooling. This is also the case within the scope of the present invention.
  • the gas phase formed during the partial evaporation and the corresponding remaining liquid are also fed into the low-pressure column at different feed points, the selection of which will be explained below.
  • the pressure in the gas space of the top condenser is the same as at the point where the gas phase is fed into the low-pressure column.
  • the same pressure is understood to mean a pressure range in which the two pressures do not differ by more than 25 mbar, preferably not more than 10 mbar.
  • the oxygen or oxygen-rich fluid from the crude argon column is typically fed several theoretical or practical plates below the Feed points for the liquid used in the cooling and partially evaporated from the pressure column are fed back into the low-pressure column.
  • the present invention has for its object to provide means for improving the operation of an air separation plant with an argon recovery system comprising a crude argon column and a pure argon column.
  • the present invention proposes a method for the low-temperature separation of air and an air separation plant with the features of the respective independent patent claims.
  • Embodiments are the subject of the dependent patent claims and the following description.
  • a "condenser-evaporator” is used here to describe a heat exchanger in which a first, condensing fluid stream enters into indirect heat exchange with a second, evaporating fluid stream.
  • Each condenser-evaporator has a condensation space and an evaporation space.
  • the condensation and evaporation spaces have condensation and evaporation passages, respectively.
  • the condensation (liquefaction) of the first fluid stream is carried out in the condensation space, and the evaporation of the second fluid stream is carried out in the evaporation space.
  • the evaporation and condensation spaces are formed by groups of passages that are in a heat exchange relationship with one another.
  • Condenser evaporators are also referred to as “head condensers” and “sump evaporators” depending on their function, whereby a head condenser is a
  • a condenser evaporator is one in which the top gas of a rectification column is condensed and a bottom evaporator is one in which the bottom liquid of a rectification column is evaporated.
  • bottom liquid can also be evaporated in a top condenser, for example as used in the present invention.
  • the so-called main condenser which connects a high-pressure column and a low-pressure column of an air separation plant in a heat-exchanging manner, is designed as a condenser-evaporator.
  • the main condenser or other condenser-evaporators can be designed as single- or multi-level bath evaporators, in particular as cascade evaporators (as described, for example, in EP 1 287 302 B1), or as falling-film evaporators.
  • a corresponding condenser-evaporator can be formed, for example, by a single heat exchanger block or by several heat exchanger blocks arranged in a common pressure vessel.
  • a liquid flow is pressed through the evaporation chamber by means of its own pressure and partially evaporated there.
  • Forced flow evaporators are sometimes also referred to as "once-through evaporators”
  • This pressure is generated, for example, by a liquid column in the supply line to the evaporation chamber, which results from the appropriate positioning of a liquid reservoir. The height of this liquid column corresponds at least to the pressure loss in the evaporation chamber.
  • the gas or gas-liquid mixture emerging from the evaporation chamber i.e.
  • liquids and gases may be rich or poor in one or more components, where "rich” may mean a content of at least 50%, 75%, 90%, 95%, 99%, 99.5%, 99.9% or 99.99% and “poor” may mean a content of at most 50%, 25%, 10%, 5%, 1%, 0.1% or 0.01% on a mole, weight or volume basis.
  • “predominantly” may correspond to the definition of "rich”.
  • Fluids may also be enriched or depleted in one or more components, where these terms refer to a content in a starting fluid from which the fluid was derived.
  • the fluid is "enriched” if it contains at least 1.1 times, 1.5 times, 2 times, 5 times, 10 times, 100 times or 1,000 times the content of a corresponding component, and “depleted” if it contains at most 0.9 times, 0.5 times, 0.1 times, 0.01 times or 0.001 times the content of the starting fluid. If, for example, “oxygen” or “nitrogen” is mentioned here, this also includes a fluid that is rich in oxygen or nitrogen, but does not necessarily have to consist exclusively of these.
  • pressure range and "temperature range” to characterize pressures and temperatures, which is intended to express that corresponding pressures and temperatures in a corresponding system do not have to be used in the form of exact pressure or temperature values in order to implement the inventive concept.
  • different pressures exist at different positions within the pressure and low pressure column, but these are within a certain pressure range, also referred to as the operating pressure range.
  • Corresponding pressure ranges and temperature ranges can be disjoint ranges or ranges that overlap one another.
  • Absolute and/or relative spatial specifications used below refer here in particular to the spatial alignment of the correspondingly designated elements of an air separation plant, for example rectification columns, sub-columns of multi-part rectification columns, or rectification areas of rectification columns in normal operation.
  • An arrangement of two elements "one above the other” is understood here in particular to mean that the upper end of the lower of the two elements is at a lower or equal geodetic height as the lower end of the upper of the two elements and the projections of the two elements on a horizontal plane overlap.
  • the two elements can be arranged exactly one above the other, ie the vertical center axes of the two elements run on the same vertical line.
  • An arrangement "side by side” is to be understood in particular to mean that the projections of the two elements on a horizontal plane do not overlap.
  • terms such as “functionally below” or “functionally above” refer to the arrangement of rectification areas or sub-columns that they would have if the rectification column were made up of one part.
  • the invention deviates from the usual operating method for forced-flow condensers, according to which in all operating modes the first evaporation gas is introduced into the low-pressure column with the lowest possible pressure loss, i.e. without any pressure-changing measures. This is fundamentally efficient.
  • the first evaporation gas is guided between the first top gas condensation arrangement and the low-pressure column through a first throttle valve.
  • the valve is preferably designed as an automatic valve; alternatively, a manual valve can be used. Overall, this results in particularly stable operation of the first top gas condensation arrangement and the crude argon column.
  • throttle valve is used here in the general sense of “throttling device” and includes, for example, throttle flaps.
  • the pressure drop across the first throttle valve can be between 300 and 50 mbar in at least one operating case, for example, and preferably between 250 and 80 mbar.
  • this throttling of the first evaporation gas is carried out in an underload case.
  • a lower or higher pressure drop and thus a lower or higher temperature is set.
  • the following values result for a composition of the ???? of approximately 57.4% nitrogen, 1.8% argon and 40.8% oxygen:
  • the first throttle valve is adjusted by means of the control device according to the invention so that the temperature of the first cooling liquid when entering the first top gas condensation arrangement is above the triple point temperature of argon.
  • This inlet temperature is preferably at least 0.1, in particular at least 0.25 K above the triple point of Argon.
  • the temperature difference is preferably between 0.1 and 2.0 K, most preferably between 0.2 and 1.0 K.
  • a throttle valve in place of the first throttle valve is known from the prior art (see also Figure 1), but only in systems with a bath evaporator at the top of the crude argon column.
  • the valve In a bath evaporator, however, the valve has a completely different function, namely a quantity control for the gas flow at the column inlet.
  • this quantity control is carried out by backing up the liquid at the outlet of the evaporator (on the condensation side); a valve between the condenser and the low-pressure column would only produce undesirable pressure loss and is unnecessary there for quantity control.
  • a throttle valve is used again, which is completely open in many operating cases, but in certain operating cases the stability of the operation of the
  • the condenser is usually designed and dimensioned for the design case (normal operation). In underload cases it offers a comparatively large heat exchange surface. Therefore it must be "braked” in underload cases in order to set the appropriate performance. In systems with bath evaporators, for example, this works by increasing the evaporation pressure (usual control of an evaporator). In systems with forced-flow evaporators, on the other hand, the performance (the load on the raw argon column) is regulated by backing up the liquid and covering part of the heat exchange surface, since there is no valve between the evaporation space of the condenser and the low-pressure column.
  • the operating pressure in the NDS in underload cases is noticeably lower than in the design case; therefore the pressure (or the temperature) in the evaporation space of the forced-flow evaporator is also lower and the argon can freeze. To counteract this, the pressure in the Low pressure column must be raised artificially. However, this costs energy. This energy loss is prevented by the method according to the invention.
  • the control device according to the invention can be analogue or digital and in particular can be integrated into an operating control system. It ensures, without human intervention, that the first throttle valve is partially closed in the corresponding operating cases in order to set the desired pressure difference. This measure is preferably integrated into an automatic load adjustment and thus ensures a consistently stable operation of the system, for example when changing from normal load operation to underload operation.
  • a first liquid pressure stream is formed using a first portion of an oxygen-enriched liquid from the pressure column, which is expanded to obtain a first flash gas and to remain a first low-pressure liquid.
  • the crude argon column is operated using a first top gas condensation arrangement in which top gas of the crude argon column is subjected to condensation with partial evaporation of a first cooling liquid which is provided using the first low-pressure liquid or a part thereof.
  • the first top gas arrangement is also referred to below as the top condenser of the crude argon column.
  • the method and the plant can also provide a pure argon column which is operated using a second top gas condensation arrangement in which top gas of the pure argon column is subjected to condensation with partial evaporation of a second cooling liquid which is provided using the second low-pressure liquid or a part thereof.
  • the second top gas arrangement is also referred to below as the top condenser of the pure argon column.
  • a first evaporation gas or a part thereof formed during the partial evaporation of the first cooling liquid and a first excess liquid or a part thereof remaining during the partial evaporation of the first cooling liquid are fed into the low-pressure column.
  • a second evaporation gas or a part thereof formed during the partial evaporation of the second cooling liquid and a second excess liquid or a part thereof remaining during the partial evaporation of the second cooling liquid are fed into the low-pressure column.
  • evaporation gas refers to the vaporized portion which is formed by the heat transfer from the respective top gases of the crude and pure argon columns in the top gas condensation arrangements or the evaporated gas columns.
  • Condenser evaporators form therein. Any remaining liquid residue is referred to here as an "excess liquid”.
  • flash gas refers to the gas or vapor portion that is formed solely by expansion.
  • the liquid level on the evaporation side of the top gas condensation arrangement (13.10) is regulated by a second throttle valve (13V2), through which the first cooling liquid upstream of the top gas condensation arrangement (13.10) can be throttled.
  • the first evaporation gas is preferably withdrawn from the top gas condensation arrangement together with the first excess liquid as a first two-phase stream, without any part of the excess liquid being circulated via the evaporator.
  • one or more "forced flow" condenser evaporators of the type described can be used in the first top gas condensation arrangement. Reference is made to the above explanations.
  • the first low-pressure liquid or a part thereof is thus passed as the first cooling liquid through one or more condenser evaporators which are part of the first
  • Head gas condensation arrangement is or are designed, forcibly guided and thereby subjected to partial evaporation to the first evaporation gas and the first excess liquid.
  • "Forcibly guided” here means a feed into the evaporation space under pressure, for example by means of a pipeline
  • the throttle valve can be fully open at least temporarily during operation, in particular during normal operation (first operating mode). However, in at least one underload case (second operating mode), a pressure drop of at least 50 mbar is generated.
  • the first excess liquid is preferably also fed into the low-pressure column within the scope of the invention.
  • the gas and the liquid can be fed together as a first two-phase stream partially or completely into the low-pressure column, in particular in a first feed area.
  • the gas line is designed as a two-phase line and the first throttle valve as a two-phase valve and the two-phase stream or the part that flows into the low-pressure column is guided through the first throttle valve.
  • the first two-phase stream is fed into a phase separator.
  • the gas line between the phase separator and the low-pressure column is designed as a pure gas line and the first throttle valve as a pure gas valve.
  • the first excess liquid is fed between the top gas condensation arrangement and the first throttle valve through a phase separator in which the first evaporation gas and the first excess liquid are separated from one another.
  • the first evaporation gas is then introduced into the low-pressure column separately from the first excess liquid.
  • the pressure in the evaporation space is not controlled by the valve in the line for the first excess liquid, but by the first valve in the pure gas line, which connects the phase separator to the low-pressure column on the gas side.
  • the liquid level in the phase separator can be measured. Depending on the measured value, the amount of first cooling liquid that is introduced into the first top gas condensation arrangement is preferably adjusted. The amount of liquid accumulating in the phase separator is preferably volume-controlled.
  • the invention can in principle be used for all process cycle topologies with argon recovery, regardless of the type of cold generation or the type of product compression. These include in particular so-called MAC/BAC or HAP processes as described for example in paragraphs [0022] to [0025] of EP 3 196 573 A1, processes with nitrogen cycles as described in EP 2 235 460 A2 or in H. Hausen and H.
  • Figure 1 illustrates an air separation plant according to a non-inventive embodiment with bath evaporator in a simplified representation.
  • FIGS. 2 to 11 illustrate air separation plants according to embodiments of the invention in a simplified representation.
  • FIG. 1 an air separation plant according to a non-inventive embodiment of the present invention is illustrated in the form of a simplified process flow diagram and is designated overall by 90.
  • Air separation plants of the type shown are described in many other places, for example in (see above), Industrial Gases Processing, Wiley-VCH, 2006, in particular Section 2.2.5, "Cryogenic Rectification” and in connection with Figure 2.3A.
  • An air separation plant for use with the present invention can be designed in a wide variety of ways.
  • the present invention can in principle be used for all process circuit topologies with argon recovery, regardless of the type of refrigeration or the type of product compression.
  • the air separation plant 90 shown as an example in Figure 1 has, among other things, a main air compressor 1, a pre-cooling device 2, a cleaning system 3, a post-compressor arrangement 4, a first booster turbine 5, a second booster turbine 6, a main heat exchanger 7, pumps 8 and 9 and a rectification column system 10.
  • the rectification column system 10 comprises a classic double column arrangement consisting of a pressure column 11 and a low-pressure column 12 as well as a crude argon column 13 and a pure argon column 14.
  • the crude argon column 13 and the pure argon column 14 have a top gas condensation arrangement 13.10 and 14.10 referred to here as "first" and "second" top gas condensation arrangement, which here each comprise a reflux or bath condenser evaporator.
  • a feed air stream is sucked in and compressed by means of the main air compressor 1 via a filter (not designated).
  • the compressed feed air stream is fed to the pre-cooling device 2 operated with cooling water.
  • the pre-cooled feed air stream is cleaned in the cleaning system 3.
  • the cleaning system 3 which typically comprises a pair of In the adsorption tanks used in alternating operation, the pre-cooled feed air stream is largely freed of water and carbon dioxide.
  • the feed air flow Downstream of the cleaning system 3, the feed air flow is divided into partial flows.
  • the air of the feed air flow is cooled in the main heat exchanger 7 in a basically known manner.
  • two so-called turbine flows are formed in corresponding turbines.
  • the booster unit of the turbine booster 6 is designed as a so-called cold booster, i.e. it is fed with already cooled air from the main heat exchanger 7. Air that has been completely cooled in the main heat exchanger 7 is expanded in a liquefied state via throttle valves that are not specifically designated and fed into the rectification column system as so-called throttle flows.
  • an oxygen-enriched liquid bottom fraction and a nitrogen-enriched gaseous top fraction are formed in the pressure column 11.
  • the oxygen-enriched liquid bottom fraction is withdrawn from the pressure column 11 and fed in portions into the evaporation chambers of the reflux or
  • the operation of the air separation plant 90 illustrated here is standard practice, so reference is made to the specialist literature cited.
  • the crude argon column 13 is fed in the usual way from the low-pressure column 11, the pure argon column 14 in the usual way from the crude argon column 13.
  • an oxygen-enriched liquid withdrawn from the pressure column 11 is designated A.
  • a first liquid pressure stream B is formed, which is expanded in a valve (not separately designated) to obtain a first flash gas and to retain a first low-pressure liquid.
  • the first evaporation gas from the The top gas condensation arrangement 13.10 is introduced into the low-pressure column 12 via a gas line 13G, which contains a first throttle valve 13V1.
  • a second liquid pressure stream D is formed, which is expanded to obtain a second flash gas and to remain a second low-pressure liquid, the second flash gas being designated E in each case.
  • the crude argon column 13 is therefore operated here using a first top gas condensation arrangement 13.10, in which top gas of the crude argon column 13 is subjected to condensation with partial evaporation of a first cooling liquid, which is provided using the first low-pressure liquid or a part thereof,
  • the pure argon column 14 is operated using a second top gas condensation arrangement 14.10 in which top gas of the pure argon column 14 is subjected to condensation with partial evaporation of a second cooling liquid which is provided using the second low-pressure liquid or a portion thereof.
  • a first evaporation gas formed during the partial evaporation of the first cooling liquid or a part thereof and a first excess liquid remaining during the partial evaporation of the first cooling liquid or a part thereof are in both embodiments 100, 200 according to Figures 2 to 4 fed into the low pressure column 12, as illustrated by F and G.
  • a second evaporation gas formed during the partial evaporation of the second cooling liquid or a part thereof and a second excess liquid remaining during the partial evaporation of the second cooling liquid or a part thereof are fed into the low-pressure column 12, as illustrated by H and I.
  • the first evaporation gas F or the part thereof fed into the low-pressure column 12 is always partially or completely fed into a first feed region into the low-pressure column 12, in particular at a common position with the first excess liquid G.
  • the second evaporation gas H or the part thereof fed into the low-pressure column 12 is, however, partially or completely fed into the low-pressure column 12 in a second feed region.
  • the second excess liquid I or the part thereof fed into the low-pressure column 12 is partially or completely fed into the low-pressure column 12 in the second feed region.
  • the first flash gas C or a part thereof is partially or completely fed into the low-pressure column 12 in the second feed region, separately from the first evaporation gas F.
  • a transfer stream from the crude argon column 13 into the pure argon column is additionally designated T in Figure 4 and is also present in the other embodiments.
  • Figure 5 shows very schematically the upper ends of the columns 10, 13 and 14.
  • the process is the same as in Figure 2 or Figure 3, but no separate separator is used as the phase separator of the first liquid pressure stream B, but simply the evaporation space of the second top gas condensation arrangement 14.10 (pure argon top condenser).
  • the gas line 13G is designed here as a two-phase line, the first throttle valve 13V1 as a two-phase valve.
  • the two liquid pressure streams B and H are jointly expanded in valve 601 downstream of the bottom evaporator 600 of the pure argon column 14 and via line 602 jointly into this evaporation chamber of the second Top gas condensation arrangement 14.10, which acts as a common phase separator.
  • the first flash gas C is withdrawn via line 603, together with the second evaporation gas E generated in the condenser evaporator 14.10.
  • the first cooling liquid K is withdrawn together with the second excess liquid I via line 604 from the evaporation space of the second top gas condensation arrangement 14.10 and separately introduced into the evaporation space of a first top gas condensation arrangement (13.10) for partial evaporation.
  • the first top gas condensation arrangement (13.10) is designed as a forced-flow evaporator on the evaporation side. The remaining fluids to and from the first top gas condensation arrangement (13.10) are guided as in Figures 2 and 3.
  • Figure 6 also shows, schematically, a further development based on Figure 5.
  • the further development can also be applied to Figures 2 to 4, in which the first top gas condensation arrangement (13.10) also has a forced-flow evaporator.
  • the gas line 13G is designed here as a two-phase line, the first throttle valve 13V1 as a two-phase valve.
  • the first throttle valve 13V1 is installed in the downpipe 702 of the two-phase flow 701.
  • the downpipe represents part of the gas line 13G.
  • the first throttle valve 13V1 is usually fully open during normal operation.
  • the two-phase flow can be throttled according to the invention in order to increase the pressure and thus the temperature in the first top gas condensation arrangement (13.10).
  • the valve can be designed to be pressure-controlled (or alternatively temperature-controlled).
  • the liquid 604 is divided into the streams K and I as in Figure 5; the corresponding proportions are set by the valve FIC1.
  • Figure 6 also shows the corresponding control elements.
  • FIC1 controls the supply of second excess liquid I into the low-pressure column 12, i.e. the division of the liquid flow 604.
  • FIC2 controls the supply of condensate from the first top gas condensation arrangement (13.10) depending on the amount used for the crude argon column.
  • PIC1 controls the pressure on the evaporation side of the second top gas condensation arrangement (14.10).
  • LIC1 controls the amount of first cooling liquid that flows into the first top gas condensation arrangement (13.10).
  • LIC2 controls the total amount of cooling liquid via the bottom level measurement in the pressure column.
  • FIC2 controls the evaporator capacity (by backing up the liquid into block 13.10 and covering part of the condensing surface).
  • the liquid content in stream 701 is calculated and adjusted if necessary by FIC1.
  • phase separator 804 to separate the two-phase stream 701 into the first evaporation gas F and the first excess liquid G.
  • the gas line 13G is designed here as a pure gas line, extends from the phase separator 804 to the low-pressure column 12 and contains the throttle valve 13V1.
  • the first evaporation gas F separated in the phase separator 804 then flows according to the invention via this gas line 13G and through the first throttle valve 13V1 into the low-pressure column 12.
  • PIC1 and LIC2 have the same function as in Figure 7.
  • the pressure on the evaporation side of the second top gas condensation arrangement (14.10) can be controlled with PIC2.
  • a TIC controller Temporization Indication and Control
  • LIC3 regulates the amount of first cooling liquid that flows into the first top gas condensation arrangement (13.10), but here depending on the measured value of the filling level in the phase separator 804.
  • the amount of second excess liquid I that flows to the low-pressure column is set using LIC4 depending on the liquid level on the evaporation side of the pure argon condenser.
  • controllers FIC3 and FIC4 in the lines for the second excess liquid G and the raw argon that is passed on to the pure argon column 14.
  • the FIC3 controller is particularly important here. This allows the liquid portion in stream 701 to be regulated directly (and not calculated) and dry evaporation in the condenser to be avoided.
  • FIG 8 shows a simplified version of a particular apparatus embodiment of the invention according to Figure 7.
  • the heat exchanger block of the first top gas condensation arrangement 13.10 is arranged inside the phase separator 804, in which the first evaporation gas and the first excess liquid are separated from one another.
  • the first top gas condensation arrangement does not lose its character as a forced-flow evaporator. Rather, the liquid to be evaporated continues to flow in a forced-flow manner and through the line at LIC3 and the header on the heat exchanger block into the evaporation passages and is not sucked out of the liquid bath of the separator 804, as would be the case with a bath evaporator.
  • phase separator 804 can also be applied to the overall processes of Figures 2 to 5, both with a separate phase separator for the first liquid pressure stream and with one integrated into the overhead gas condensation arrangement, as shown in Figure 8.
  • Figure 10 differs from Figure 7 in a similar way.
  • the valve LIC4 and the corresponding line are omitted.
  • the vapor 901 from the separator 804 and the vapor 902 from the top condenser 14.10 of the pure argon column 14 are combined and fed into the low-pressure column via a common line 903, preferably at the same point as the liquid G from the separator 804.
  • the entire liquid stream 604 taken from the evaporation space of the top condenser 14.10 of the pure argon column 14 flows through the top condenser 13.10 of the crude argon column 13.
  • LIC1 like LIC2 in Figure 7, is responsible for level control in the bottom of the pressure column (not shown here).
  • the level in the evaporation chamber of the top condenser 14.10 of the pure argon column 14 is controlled by adjusting the amount of liquid drawn off by valve 13V2 (LIC2).
  • the valve FIC2 thus indirectly controls the amount of gas at the column inlet by backing up the liquid (and thus covering part of the heat exchange surface). This gives the top condenser 13.10 a higher cooling capacity (at a relatively low liquid level) or a lower one (at a relatively high liquid level).
  • valve 13V1 is pressure-controlled (PIC2) and thus sets the temperature of the head condenser 13.10 and thus its output.
  • PIC2 pressure-controlled
  • FIG 11 A particularly preferred embodiment is shown in Figure 11, which is closely based on Figure 8, in particular the heat exchanger block of the top condenser 13.10 of the crude argon column 13 is installed in the separator 804. Otherwise, the entire liquid stream 604, which is taken from the evaporation space of the top condenser 14.10 of the pure argon column 14, is introduced into the evaporation space of the top condenser 13.10 of the crude argon column 13. Also analogous to Figure 10, the vapor 901 from the separator 804 and the vapor 902 from the top condenser 14.10 of the pure argon column 14 are combined and fed into the low-pressure column via the common line 903, preferably at the same point as the liquid G from the separator 804.
  • LIC1 is responsible for level control in the bottom of the pressure column (not shown here).
  • the level in the evaporation chamber of the top condenser 14.10 of the pure argon column 14 is set by adjusting the amount of liquid drawn off using valve 13V2 (LIC2).
  • the flow on the liquefaction side of the top condenser 13.10 of the crude argon column 13 is set as in Figure 10.
  • valve 13V1 is pressure-controlled (PIC2) and thus sets the temperature of the top condenser 13.10 and thus its output.
  • the liquid outflow from the separator 804 is set via LIC3 and thus the liquid level in the separator is regulated.
  • the pressure in the evaporation chamber of the top condenser 14.10 is set via PC1.

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Abstract

L'invention concerne un procédé de séparation cryogénique d'air faisant intervenir une installation de séparation d'air (100-300) comportant un ensemble colonne de rectification (10) qui comprend une colonne sous pression (11), une colonne basse pression (12) et une colonne d'argon brut (13). Un gaz d'évaporation provenant d'un dispositif de condensation de gaz de tête (13.10) associé à la colonne d'argon brut (13) est injecté partiellement ou totalement dans la colonne basse pression (12) par l'intermédiaire d'une conduite de gaz (13G). La conduite de gaz (13G) comprend une première vanne d'étranglement (13V1) qui est réglée au moyen d'un dispositif de régulation de manière à empêcher que l'argon ne gèle dans le premier dispositif de condensation de gaz de tête (13.10). Une chute de pression d'au moins 50 mbar est alors générée au moins temporairement par la soupape d'étranglement (13V1). Cette invention concerne en outre une installation de séparation d'air (100-200) correspondante.
EP23813562.8A 2022-11-17 2023-11-16 Procédé de séparation cryogénique d'air et système de séparation d'air Pending EP4619693A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
PCT/EP2022/025517 WO2023110142A1 (fr) 2021-12-13 2022-11-17 Procédé de séparation cryogénique de l'air et installation de séparation d'air
EP23020295 2023-06-16
PCT/EP2023/025485 WO2024104613A2 (fr) 2022-11-17 2023-11-16 Procédé de séparation cryogénique d'air et système de séparation d'air

Publications (1)

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Publication number Priority date Publication date Assignee Title
JPS6044586B2 (ja) * 1978-03-03 1985-10-04 株式会社日立製作所 空気の液化分離方法
JPS5546362A (en) * 1978-09-29 1980-04-01 Hitachi Ltd Method of controlling air separator equipped with argon catcher
GB2198513B (en) * 1986-11-24 1990-09-19 Boc Group Plc Air separation
DE10027139A1 (de) 2000-05-31 2001-12-06 Linde Ag Mehrstöckiger Badkondensator
EP2235460B1 (fr) 2008-01-28 2018-06-20 Linde Aktiengesellschaft Procédé et installation pour la séparation cryogénique d'air
EP3196573A1 (fr) 2016-01-21 2017-07-26 Linde Aktiengesellschaft Procede de production d'un produit pneumatique et installation de decomposition d'air
EP3423170B1 (fr) * 2016-03-01 2021-05-26 Praxair Technology, Inc. Procédé et appareil de récupération d'argon dans une unité de séparation d'air cryogénique intégrée à un système d'adsorption par inversion de pression

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WO2024104613A3 (fr) 2024-08-29
TW202434845A (zh) 2024-09-01
CN120129811A (zh) 2025-06-10
WO2024104613A2 (fr) 2024-05-23

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