WO2020169257A1 - Procédé et installation de décomposition d'air à basse température - Google Patents

Procédé et installation de décomposition d'air à basse température Download PDF

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Publication number
WO2020169257A1
WO2020169257A1 PCT/EP2020/025083 EP2020025083W WO2020169257A1 WO 2020169257 A1 WO2020169257 A1 WO 2020169257A1 EP 2020025083 W EP2020025083 W EP 2020025083W WO 2020169257 A1 WO2020169257 A1 WO 2020169257A1
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Prior art keywords
column
liquid
fed
bottom liquid
fluid
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PCT/EP2020/025083
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German (de)
English (en)
Inventor
Dimitri GOLUBEV
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Linde Gmbh
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Publication of WO2020169257A1 publication Critical patent/WO2020169257A1/fr

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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
    • F25J3/04006—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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/0403—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling 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
    • F25J3/04096—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 argon or argon enriched stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • F25J3/04145—Mechanically coupling of different compressors of the air fractionation process to the same driver(s)
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    • 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
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    • 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
    • F25J3/04181—Regenerating the adsorbents
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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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/0423—Subcooling of liquid process streams
    • 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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • 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
    • 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
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    • 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
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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
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low 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
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F25J3/04715—The auxiliary column system simultaneously produces oxygen
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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
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    • 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
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    • 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
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    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
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    • F25J2210/42—Nitrogen
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    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
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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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/50—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/52—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being oxygen enriched compared to air, e.g. "crude 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the 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
    • 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
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being 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
    • 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 method and a system for
  • Air separation plants have rectification column systems that
  • Multi-column systems can be formed.
  • rectification columns for obtaining nitrogen and / or oxygen in the liquid and / or gaseous state i.e. the rectification columns for nitrogen-oxygen separation
  • rectification columns can be provided for obtaining further air components, in particular the noble gases krypton, xenon and / or argon.
  • the terms “rectification” and “distillation” and “column” and “column” or terms composed of these are often used synonymously.
  • the rectification columns of the mentioned rectification column systems are operated at different pressure levels.
  • Known double column systems have a so-called high pressure column (also referred to as a pressure column, medium pressure column or lower column) and a so-called low pressure column (also referred to as an upper column).
  • the high pressure column is typically on a
  • the low-pressure column is operated at a pressure level of typically 1 to 2 bar, in particular about 1.4 bar. In certain cases, both
  • Rectification columns can also be used at higher pressure levels. With the here and The pressures given below are absolute pressures at the top of the columns given.
  • the third column comprises a first and a second condenser evaporator in an air separation process proposed in FR 3 011 916 A1 and nitrogen from a cold compressor is fed to one of the condenser evaporators.
  • liquid nitrogen is pressurized and a heat exchange with a
  • Heat exchange of non-evaporated liquid nitrogen is used as return.
  • an improvement in the separation performance is to be achieved by withdrawing part of the gas rising through the low-pressure column, increasing its temperature and pressure and then feeding it into the
  • EP 2 015 013 A2 proposes condensation and pseudocondensation of an air stream in the main heat exchanger with subsequent evaporation in an auxiliary condenser.
  • the evaporated air stream is heated, recompressed and fed back into the feed air.
  • raw argon are made from a second
  • DE 199 33 558 A1 proposes a method for the low-temperature separation of air in a three-column system with an additional column, whereby from the upper area the high pressure and / or additional column withdrawn a pressure nitrogen product and the pressure of at least part of at least one oxygen or
  • nitrogen-enriched liquid fraction is increased.
  • nitrogen is separated from air by cryogenic rectification and the nitrogen separated in this way is condensed at three or more pressures. In the separation, at least part of the condensed nitrogen is used as reflux.
  • liquid argon can be delivered or evaporated on site, or gaseous argon can be obtained on site.
  • the delivery of liquid argon not only brings economic disadvantages (transport costs, refueling losses, cold losses when evaporating against ambient air), but also makes high demands on the
  • the nitrogen produced should typically only contain about 1 ppb, a maximum of 1000 ppb, oxygen, be essentially free of particles, and be able to be supplied at a pressure level that is clearly above atmospheric.
  • Figures in ppb or ppm relate to the molar proportion.
  • Air separation plants are typically used to extract argon
  • Rectification columns are designed accordingly. Pure argon can then be withdrawn from the crude argon column or a comparable column typically somewhat further below than the fluid conventionally transferred into the pure argon column. Even if only comparatively small amounts of argon are in demand, conventionally a complete air separation plant with a double column and argon rectification has to be installed for the production of the gaseous argon, as explained above. The generation of nitrogen at a pressure level that is significantly above atmospheric and at the same time large
  • the present invention therefore sets itself the task of specifying a method and an air separation plant by means of which, in addition to larger amounts of high-purity, gaseous nitrogen on a clearly
  • argon can also be advantageously provided.
  • Liquids and gases can be rich or poor in one or more components in the parlance used here, with “rich” for a content of at least 75%, 90%, 95%, 99%, 99.5%, 99.9% or 99.99% and “poor” can mean a content of no more than 25%, 10%, 5%, 1%, 0.1% or 0.01% on a mole, weight or volume basis.
  • the term “predominantly” can match the definition of "rich”.
  • Liquids and gases can also be enriched or depleted in one or more components, these terms referring to a content in a starting liquid or a starting gas from which the liquid or the gas was obtained. Be the liquid or the gas
  • 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 to realize the inventive concept.
  • pressures and temperatures typically move in certain ranges, for example ⁇ 1%, 5% or 10% around a mean value.
  • pressure ranges and temperature ranges can be in disjoint areas or in areas that overlap one another.
  • pressure ranges include, for example, unavoidable or expected pressure losses.
  • temperature ranges The values specified in bar for the pressure ranges are absolute pressures. If "expansion machines” are mentioned here, this is typically understood to mean known turboexpander. These expansion machines can in particular also be coupled to compressors. These compressors can in particular be turbo compressors. A corresponding combination of turbo expander and turbo compressor is typically also referred to as a "turbine booster".
  • turbo-expander and the turbo-compressor are mechanically coupled, the coupling being able to take place at the same speed (for example via a common shaft) or at different speeds (for example via a suitable transmission gear).
  • compressor is used here in general.
  • a “cold compressor” here denotes a compressor to which a fluid flow is fed in a temperature range well below 0 ° C, in particular below -50, -75 or -100 ° C and down to -150 or -200 ° C. A corresponding fluid flow is cooled to a temperature in this temperature range in particular by means of a main heat exchanger (see below).
  • a “main air compressor” is characterized by the fact that it compresses all of the air that is fed to the air separation plant and separated there. In contrast, in one or more optionally provided further compressors, for example booster compressors, only a portion of this air that has already been previously compressed in the main air compressor is further compressed.
  • the "main heat exchanger" of an air separation plant represents the heat exchanger in which at least the
  • a “heat exchanger” for use in the context of the present invention can be designed in a manner customary in the art. It serves for the indirect transfer of heat between at least two e.g. fluid flows guided in countercurrent to one another, for example a warm compressed air flow and one or more cold ones
  • Fluid flows or a cryogenic liquid air product and one or more warm or warmer, but possibly also cryogenic fluid flows.
  • Heat exchanger can be formed from a single or from several parallel and / or serially connected heat exchanger sections, for example from one or more Plate heat exchanger blocks. It is, for example, a plate heat exchanger (plate fin heat exchanger). Such a heat exchanger has "passages" which are separated from each other as fluid channels
  • Heat exchange surfaces are formed and connected in parallel and separated by other passages to form "passage groups". Characteristic of a
  • the heat exchanger is that in it heat is exchanged between two mobile media at a time, namely at least one fluid flow to be cooled and at least one fluid flow to be heated.
  • a “condenser evaporator” is a heat exchanger in which a first, condensing fluid flow enters into indirect heat exchange with a second, evaporating fluid flow.
  • Each condenser evaporator has one
  • Evaporation chambers have liquefaction or evaporation passages.
  • the condensation (liquefaction) of the first fluid flow is carried out in the liquefaction space, and the evaporation of the second fluid flow in the vaporization space.
  • the evaporation and the liquefaction space are formed by groups of passages which are in a heat exchange relationship with one another.
  • the gas-liquid mixture emerging from the evaporation chamber is separated according to phases in a "once through" condenser evaporator of this type directly to the next process step or to one
  • downstream device forwarded and in particular not in a
  • the axes of the two components do not have to be exactly perpendicular, but can also be offset from one another, especially if one of the two components, for example a rectification column or a column part with a smaller diameter, is to have the same distance from the sheet metal jacket of a coldbox as another with a larger one Diameter.
  • the present invention proposes a method for
  • the first to third columns in the air separation plant according to the invention result from the expansion of a classic double column system known from the prior art by an additional column operated at a higher pressure than the conventionally present high pressure column.
  • the first column can be provided in particular structurally separate from the second and third column, the second and third column in particular being part of a double column and by means of a corresponding one Condenser evaporator, the so-called main condenser, can be in heat-exchanging connection with one another.
  • the second and the third column which are part of a
  • Double columns are formed, can also be supplemented by an additional column in a corresponding multiple column system, or the second and third columns can be provided as separate columns.
  • the main capacitor can be provided as an internal or external main capacitor, as is basically known from the prior art.
  • an internal main condenser this is at least partially submerged in a bottom liquid in the bottom of the third column and an overhead gas to be condensed from the second column is passed through a
  • a first bottom liquid is formed in the first column
  • a second bottom liquid is formed in the second column
  • a third is formed in the third column
  • Bottom liquid is formed and a fourth bottom liquid is formed in the fourth column.
  • the fourth column in the context of the present invention is used in particular for argon production or
  • the fourth column can in particular be a conventional crude argon column of a known arrangement with crude and pure argon column, but it can also be a modified argon column from which argon is withdrawn in the pure state below the top without using an additional pure argon column.
  • Other variants are also possible within the scope of the present invention.
  • the first column is in a first
  • the second column is operated in a second pressure range below the first pressure range and the third column is operated in a third pressure range below the second (and thus also the first) pressure range.
  • the fourth column can in particular be operated in the third pressure range or in a pressure range which is slightly below this and which can result in particular from pressure losses via the lines connecting the third and fourth columns.
  • the first pressure range can in particular be 9 to 12 bar, for example approx. 10.5 bar, the first pressure range corresponding in particular to the pressure range in which nitrogen is also obtained within the scope of the present invention.
  • the second pressure range is within the scope of the present Invention advantageously at 4 to 6 bar, in particular at approx. 5.5 bar
  • the third pressure range is advantageously at 1 to 2 bar, in particular at approx. 1.4 bar.
  • the pressure specifications here denote absolute pressures at the head of corresponding columns.
  • the second and third columns are thus operated in the context of the present invention, as already mentioned above, in pressure ranges in which the high and low pressure columns conventionally used in air separation plants are also operated.
  • the first column is operated in a higher pressure range, in particular in order to be able to provide nitrogen in this pressure range without further compression, as is done by taking off from the first column.
  • Sump liquid is formed and the third sump liquid is formed with a higher oxygen content and a lower argon content than the second sump liquid.
  • the higher argon content of the second sump liquid compared to that of the first sump liquid results from the different
  • compositions of streams in the first and second column are Compositions of streams in the first and second column
  • the lower argon content in the third column results in particular from the fact that an argon-enriched gas is withdrawn from this third column, as will be explained below.
  • the oxygen content of the first sump liquid can be 28 to 40%, in particular about 34%
  • the oxygen content of the second sump liquid is approximately 45 to 65%, in particular approximately 55%, and the oxygen content of the third sump liquid is approximately 99.0 to 99.9%, in particular approximately 99.5%.
  • the respective percentages relate to the molar content of oxygen in a corresponding one
  • the third column is therefore used in the context of the present invention as a pure oxygen column and a corresponding pure oxygen product can be withdrawn from it.
  • the first and the second sump liquid are typically not used as a product, but are further processed in the plant.
  • fluid is generally fed from the first column into the second column and into the third column, and fluid from the second
  • Fluid from the third column is fed to the fourth column
  • fluid from the fourth column is fed to the third column. If it is said here that “fluid” is fed from one column into another, this is to be understood in particular as a direct or indirect transfer of a corresponding fluid flow. In particular, the transfer of the corresponding fluids can initially also be carried out in one feed
  • the transferred fluids can include overhead gases, bottom liquids and / or side streams of corresponding columns. Under a "side stream" is a
  • a sump liquid is discharged in particular in the form of a liquid material flow, and a top gas in particular in the form of a gaseous material flow.
  • liquid or gaseous material flows can also be withdrawn, for example, directly above the sump, but still below the lowest separating section or the lowest separating tray.
  • a liquid side stream can, for example, be removed from a liquid retention device or from a storage floor.
  • the fluid fed into the fourth column from the third column comprises at least part of a side stream which has a lower oxygen content and a higher argon content than the third Bottom liquid is withdrawn from the third column.
  • the side stream is withdrawn from the third column in particular in the area of the argon transition already explained above, but it can also be withdrawn below the argon transition.
  • a corresponding side stream represents a gas mixture in particular, which has a higher argon content than the bottom liquid and a lower argon content than the top gas.
  • An essential aspect of the present invention is that a reflux liquid is formed by condensing top gas of the second column, and that this reflux liquid is fed into the first column in liquid form by means of a pump.
  • the formation of the reflux liquid "using" the top gas can in particular include removing top gas in gaseous form from the second column, at least partially liquefying this in the main condenser, and at least partially returning a liquid portion to the first column.
  • Return flow can be withdrawn from the second column, for example, directly below the feed point for a corresponding liquefied substance flow, or withdrawn directly from the main condenser and conveyed back to the first column by means of a pump.
  • the pump By means of the pump, the one between the first column and the second column can be used
  • a corresponding reflux stream can be used in particular to cool part of the bottom liquid of the first column, as will also be explained in detail below.
  • the return of reflux liquid from the second column to the first column in the form of the mentioned reflux liquid enables an increased removal of gaseous nitrogen or a corresponding nitrogen-rich gas mixture at a correspondingly high pressure, i.e. in the pressure range in which the first column is operated.
  • a corresponding material flow does not have to be compressed in gaseous form, but can be returned to the first column in the form of the liquid reflux and further purified there if necessary.
  • second column present invention referred to as "second column" fed.
  • the bottom liquid of the second column becomes significantly more oxygen-containing and therefore significantly warmer than the bottom liquid of the first column through the use of the reflux liquid from the second column (i.e. the described "pumping back" of part of the liquid formed in the top condenser of the second column) , since nitrogen is discharged from the second column via the substream removed in this way. For this reason, this bottom liquid of the second column cannot be used to cool one
  • Condenser in the argon part for example, a top condenser of the fourth column, which can be designed as a crude argon column or modified crude argon column
  • the driving temperature difference in such a condenser would otherwise be negative.
  • the mixture provided in the prior art would also lead to a corresponding temperature reduction.
  • the nitrogen provided within the scope of the present invention at the initially mentioned pressure in the range from 9 to 12 bar (or in the first pressure) is advantageously provided with a residual oxygen content in the ppb range, i.e. in the range of 1 to 1,000 ppb. Its amount in standard cubic meters per hour is in particular in the range between 40 and 60%, further in particular between 45 and 55%, of the amount of air used, i.e. the total amount of air supplied to the column system, which is also specified here in standard cubic meters per hour.
  • the oxygen contents of the respective bottom liquids of the columns which can be used here have already been mentioned above.
  • the amount of reflux of the repeatedly mentioned reflux liquid from the second column into the first column can in this embodiment, based in each case on standard cubic meters per hour, for example between 15 and 25%, for example between 20 and 22%, of the feed air amount. Without a corresponding return flow rate, the aforementioned nitrogen cannot be provided in the stated amount. Furthermore, in this embodiment, further products in particular can be produced in specific product quantities, again expressed in standard cubic meters per hour and based on the amount of air used.
  • it can be internally compressed oxygen (0.5 to 5%, in particular 1 to 2% of the amount of air used), liquid nitrogen (0.1 to 0.5%, in particular 0.2 to 0.3% of the amount of air used), highly pure gaseous Oxygen (0.5 to 1%, in particular 0.6 to 0.8% of the feed air volume) and internally compressed argon (0.1 to 1%,
  • gas at the top of the fourth column is released by means of a first condenser evaporator condensed, in which a portion of the first bottom liquid is subjected to partial evaporation.
  • a head capacitor becomes one
  • the bottom liquid of the second column in the context of the present invention is significantly more oxygen-containing and therefore significantly warmer through the use of the reflux liquid from the second column (i.e. the described "pumping back" of part of the liquid formed in the top condenser of the second column), so that this is less suitable for cooling the top condenser.
  • evaporated and non-evaporated portions of the bottom liquid from the first column which were used in the top condenser or condensers of the fourth or fourth and fifth column, are then transferred to the third column, namely at a position which corresponds to the oxygen content and argon content of these fluids.
  • the feed of vaporized and non-vaporized parts can therefore be im
  • Streams can be combined or transferred separately from one another into the third column.
  • the fluid transferred from the first column to the third column thus comprises corresponding liquid, ie at least part of the first bottom liquid which was used to cool the top condenser or condensers of the fourth or fourth and fifth columns. If necessary, it is also possible to dispense with feeding vaporized fractions from the top condenser or condensers, and these vaporized fractions are removed from the process without being fed into the third column. In this case, too, part of the first bottom liquid is fed into the third column with the non-evaporated liquid.
  • the fluid fed from the second column into the third column comprises at least part of the second bottom liquid, which is transferred from the second column to the third column without using a pump.
  • corresponding bottom liquid can be transferred into the third column only on the basis of the pressure difference between the second and the third column. However, it can be subcooled beforehand or during the transfer against further currents using a subcooling countercurrent.
  • Overhead gas can be withdrawn from the first column at a defined withdrawal position and discharged from the air separation plant.
  • Removal position of the top gas from the first column are fed into the first column. However, it is also possible to feed in at essentially the same point as the overhead gas is withdrawn. Feeding the reflux liquid below the removal position of the top gas from the first column is particularly advantageous in order to achieve high product purities. A simpler pump can be used here than with a feed at the same height, which can result in less contamination.
  • thermodynamic potential a product purity of a nitrogen product can be achieved with a content of less than 1 ppb oxygen. With a feed at the same level, however, the entire thermodynamic potential can be used.
  • the reflux liquid is brought into a supercooled state by increasing the pressure by means of a pump, in particular the pump with which it is fed into the first column. Since it is not necessary to feed into the first column in the subcooled state, one or more liquid material flows can be cooled according to this embodiment of the invention by means of the reflux liquid, in particular in a subcooling countercurrent.
  • a first portion of the first bottom liquid can be subcooled in this context using the reflux stream and fed into the third column and a second portion can be fed into the second column without subcooling.
  • the supercooled first portion can in particular after the supercooling in the explained manner for cooling the top condenser of the fourth or, if present, the fourth and fifth columns are used.
  • the second fraction which is not supercooled, can be fed into the second column directly or, if necessary, after being used for cooling in a top condenser of the first column.
  • This enables the second and third columns to be advantageously fed with the fluids to be separated.
  • other fluids can also be correspondingly supercooled.
  • gas is advantageously withdrawn from the third column, heated, compressed, cooled and fed into the second column.
  • a feed circuit is created in which gas essentially withdrawn from the third column and having an oxygen content of approx. 15% to 40% is transferred back to the second column.
  • the gas for such a feed circuit does not necessarily have to be taken directly from the third column, but gas can also be taken from the
  • Evaporation space of a top condenser of the fourth column (as a partial amount or as a whole stream) can be used accordingly before this gas is fed into the third column.
  • bottom liquid of the second or first column which was used as a coolant in a top condenser of the first column and was partially evaporated in the process, can also be used in the evaporated portion to form a corresponding circulating flow can be used.
  • the corresponding gas can be heated, compressed and cooled as explained above for the gas withdrawn from the third column.
  • it is advantageously fed into the first column.
  • the oxygen content can be comparable to that explained above with regard to the gas from the third column or it can be slightly higher.
  • Top condenser of the first column unevaporated bottom liquid from the first column can advantageously be transferred to the third column and given up there as reflux in a middle position.
  • the fluid fed from the first column into the third column can, as already mentioned, at least a portion of a Gas phase, which is formed during partial evaporation in the first condenser evaporator, and at least a portion of a liquid phase which remains liquid during partial evaporation in the first condenser evaporator.
  • the condenser evaporator is only used for referencing reasons
  • top gas of the first column in particular can be condensed by means of a condenser evaporator, which is referred to here as a "second" condenser evaporator only for reference reasons, and in which a portion of the first and / or second bottom liquid, as also already mentioned, is a partial evaporation is subjected.
  • the fluid fed into the third column from the first column can comprise at least a portion of a liquid phase which remains liquid during the partial evaporation in the second condenser evaporator.
  • at least a portion of a gas phase that is formed during partial evaporation in the second condenser evaporator can be returned to the first column and in particular also be used partially in the form of the recycle stream already explained.
  • the fluid fed into the second column from the first column advantageously comprises a further portion of the first bottom liquid that has not been subjected to partial evaporation in the second condenser evaporator.
  • the corresponding bottom liquid can be transferred directly from the first column to the second column.
  • the present invention can be used in combination with a
  • Pure argon column can be used, that is to say a fifth column into which the fluid from the fourth column is transferred, the fluid transferred from the fourth column having an argon content which is higher than that from the third column
  • the fifth column is therefore used in the context of the present invention, as is fundamentally known from the field of air separation technology, to obtain a corresponding argon product.
  • the top gas of the fifth column is condensed by means of a further condenser evaporator, in which a further portion of the second
  • Partial evaporation in the further condenser evaporator remains liquid includes. Reference is expressly made to the above explanations.
  • the side stream which in the context of the present invention is formed with a lower oxygen content and a higher argon content than the third bottom liquid and is withdrawn from the third column, can, in particular, obtain a top gas and a bottom liquid in a further column
  • Substance exchange with a portion of the fourth bottom liquid are subjected, with at least a portion of the gas phase being able to be fed into the fourth column from the further column. In this way there is another
  • Depletion of a corresponding bottom liquid or an oxygen section of a corresponding fourth column is transferred to the further column.
  • a further proportion of the fourth bottom liquid can be depleted of higher-boiling components in the further column and returned to the fourth column, in particular a separate section of the further column being used.
  • Air separation plant for the features of which reference is expressly made to the corresponding independent patent claim.
  • such an air separation plant is set up to carry out a method, as has been explained above in different configurations, and this has means set up in each case for this purpose.
  • Air separation plant is expressly referred to the explanations relating to the method according to the invention.
  • FIGS. 1 and 3 relate to embodiments according to the invention. The latter is the case with regard to FIGS. 1 and 3.
  • the air separation plants according to FIGS. 1 to 19 are each designated as a whole with the reference symbols 1001 to 1019. Although the following explanations refer to the corresponding
  • All of the air separation plants 1001 to 1019 shown in FIGS. 1 to 19 are equipped with a column system which, regardless of the different configuration and possibly different number of columns, is each designated overall by 10.
  • the column systems 10 each have a first column 11, a second column 12, a third column 13 and a fourth column 14.
  • the second column 12 and the third column 13 are each part of one
  • Double column basically of a known type.
  • express reference is made to the technical literature on air separation plants cited at the beginning, in particular to the explanations on Figure 2.3A in Häring (see above), in which a corresponding double column is shown.
  • the first column 11 is formed separately from the second column 12 and the third column 13.
  • the first column 11 is equipped with an overhead condenser 111 which is used to condense overhead gas from the first column 11. Except for the air separation plants, in which this is explained differently (see there), bottom liquid from the second column 12, which is conveyed by means of a pump 17, is fed into the top condenser 111.
  • the second column 12 and the third column 13 are located above an internal condenser-evaporator 121, the so-called main condenser
  • the main condenser 121 serves on the one hand to condense an overhead gas of the second column 12 and on the other hand, for the evaporation of a bottom liquid of the third column 13.
  • the second column 12 and the third column 13 can also be formed separately.
  • the main capacitor 121 can alternatively also be formed on the outside. Different types of
  • Condenser evaporators can be used as the main condensers 121.
  • the fourth column 14 is used in all air separation plants 1001 to 1019 according to FIGS. 1 to 19 for the extraction of argon. Except for the air separation plant 1018 according to FIG. 18, the fourth column 14 is in each case designed as a crude argon column and a separate pure argon column is provided as the fifth column 15. In the
  • the fourth column 14 and the fifth column 15 are equipped with an overhead condenser 141 and 151, respectively, which in each case condenses overhead gas and, in all configurations, is cooled with a portion of the bottom liquid from the first column 11.
  • the bottom liquid used is subcooled beforehand by a subcooling countercurrent 18 and, apart from the cases in which this is explained differently below, is at least partially fed into the third column 13 in the evaporated and non-evaporated portions. If a fifth column 15 is present, bottom liquid is partially evaporated from this in a condenser evaporator 152, through which part of the bottom liquid from the first column 11 likewise flows.
  • a further further column 16 is provided in which a mass transfer between a portion of a bottom stream from the fourth column 14 and a side stream from the third column 13 and a portion of the bottom stream from the fourth column 14 is depleted in more volatile components.
  • the further column 16 has an upper and a lower area which are functionally completely separated from one another. Further details are explained below.
  • the further column 16 is designed with a condenser-evaporator 162 which is heated with top gas from the second column 12. As a component directly assigned to the column system 10, all
  • Air separation plants 1001 to 1019 according to FIGS. 1 to 19 have a pump 19 which conveys bottom liquid from the fourth column 14 back into the third column 13.
  • a second bottom liquid is correspondingly formed in the second column 12, a third bottom liquid in the third column 13 and a fourth bottom liquid in the fourth column 14.
  • the first column 11 is in a first pressure range, the second column 12 in a second
  • the second sump liquid will have a higher oxygen content and a higher one
  • fluid is fed from the first column 11 into the second column 12 and into the third column 13. Furthermore, fluid is fed from the second column 12 into the third column 13 and fluid is fed from the fourth column 14 into the third column 13.
  • the fluid fed from the third column 13 into the fourth column 14 comprises at least part of a side stream that has a lower oxygen content and a higher argon content than the second
  • the air separation plant 1001 according to FIG. 1 is first explained in more detail below. For the sake of clarity, the explanations relating to the air separation plants 1002 to 1019 according to FIGS. 2 to 19 relate only to the features that differ therefrom. In FIGS. 2 to 19, identical features are only partially provided with corresponding reference symbols.
  • a feed air stream a from the atmosphere generally designated here by A is sucked in by means of a main air compressor 1 through a filter, which is not separately designated and illustrated by hatching, aftercooled in an aftercooler, likewise not designated separately, and fed to a direct contact cooler 2, which is marked with Cooling water W is operated.
  • the feed air stream is freed from water and carbon dioxide in an adsorption device 3 in a manner which has been described many times in the literature.
  • the correspondingly treated and thus purified feed air flow, further designated with a, is then divided into two partial flows b and c, both of which are one on the warm side
  • Main heat exchanger 4 are supplied.
  • the partial flow c is previously subjected to a further pressure increase in a booster of a booster turbine arrangement 5 and is cooled in an aftercooler, which is not specifically designated.
  • the substream b is withdrawn from the main heat exchanger 4 on the cold side and fed into the first column 11.
  • the substream c is withdrawn from the main heat exchanger 4 at an intermediate temperature level, then expanded in a turbine of the booster turbine arrangement 5 and fed into the second column 12.
  • the bottom liquid of the first column 11 is withdrawn from this and divided into two substreams d and e.
  • the substream d is into the second column 12
  • the substream e fed in, the substream e, however, passed through the subcooling countercurrent 18 and then through the condenser evaporator 152. Again in the form of two substreams, which, however, are no longer designated separately after the subdivision of the material flow e, are then fed into the substream e.
  • Evaporation chambers of the top condensers 141 and 151 The gas formed here and portions remaining in liquid form are fed into the third column 13 individually or separately, as illustrated here with material flows f.
  • the top gas of the first column 11 is partially passed through the condensation space of the top condenser 111 and returned to the first column 11 as liquid reflux. Another part is in the form of a stream g im
  • Main heat exchanger 4 heated and discharged as a gaseous nitrogen pressure product from the air separation plant 1001 or used in some other way.
  • the bottom liquid of the second column 12 is withdrawn from this in the form of a stream h and by means of the pump 17 into the evaporation chamber of the
  • the top gas of the second column 12 is partly passed through the condensation space of the main condenser 121, liquefied there and partly returned to the second column 12 as a liquid reflux.
  • a further portion is liquefied in the form of a material flow I in the condensation space of the condenser evaporator 162 and combined with the portion liquefied in the condensation space of the main condenser 121.
  • the portion liquefied in the form of the stream I in the condensation space of the condenser-evaporator 162 can also be fed back to the first column 11 by means of a pump.
  • liquefied overhead gas of the second column 12 is passed in the form of a stream m through the subcooling countercurrent 18 and fed into the third column 13.
  • Non-liquefied top gas of the second column 12 is heated in the form of a stream n in the main heat exchanger 4 and discharged as a gaseous nitrogen pressure product from the air separation plant 1001 or used in some other way.
  • the bottom liquid of the third column 13 is withdrawn from this in the form of a stream o, brought to liquid pressure by means of an internal compression pump 6, in the main heat exchanger 4 by heating in the gaseous or critical State transferred and discharged as a gaseous oxygen pressure product from the air separation plant 1001 or used otherwise.
  • Above the sump from the third column 13 in the form of a material flow p withdrawn gas is passed through the subcooling countercurrent 18 and combined with residual gas from the third column 13 (see below) to a collection flow q, which is then heated in the main heat exchanger 4 and as from
  • Air separation plant 1001 is diverted or used in some other way, in particular after further heating for the regeneration of the adsorption unit 3.
  • the top gas of the third column 12 is passed in the form of a stream r through the subcooling countercurrent 18, then heated in the main heat exchanger 4 and discharged from the air separation plant 1001 as a gaseous nitrogen product or used in some other way.
  • a stream s withdrawn from the third column 13 with a lower nitrogen content below the stream r is combined with the stream o, as mentioned, to form the collective stream q.
  • a side stream t is also withdrawn in gaseous form from the third column 13 and initially fed into an upper part of the further column 16.
  • a stream u is returned in liquid form to the third column 13.
  • In the upper part of the further column 16 is a
  • Substance exchange is carried out with bottom liquid from the fourth column 15, which is applied in liquid form in the form of a substance flow v into the upper and lower part of the further column 16.
  • the condenser evaporator 162 Gas is withdrawn from the upper and the lower part of the further column 16 and is fed into the fourth column 14 in the form of a material flow w.
  • part of the side stream t is fed into the fourth column 14 and from this part of the bottom liquid is returned to the third column 13.
  • the further column 16 can, for example, also be arranged above the top condenser 111 of the first column 11.
  • the tank system becomes a for the sake of clarity Also taken with x designated material flow, evaporated in the main heat exchanger 4 and executed as a highly pure, gaseous oxygen product.
  • Top gas of the fourth column 14 that is not liquefied in the condensation space of the top condenser 141 of the fourth column 14 is transferred into the fifth column 15 in the form of a stream y.
  • Top gas of the fifth column 15 that is not liquefied in the condensation space of the top condenser 151 of the fifth column 15 is released into the atmosphere.
  • the bottom liquid of the third column 13, if not evaporated in the condenser-evaporator 152, is brought to liquid pressure in the form of a stream z by means of an internal compression pump 7, in the
  • Main heat exchanger 4 converted into the gaseous or critical state by heating, and discharged as a gaseous argon pressure product from the air separation plant 1001 or used in some other way.
  • Liquid nitrogen, liquid oxygen (possibly also with different purities) and liquid argon can be provided as further products of the system 1001, as is generally known.
  • the air separation plant 1002 formed differs from the air separation plant shown in FIG. 1 essentially in that a liquid return flow R is carried out from an upper region of the second column 12 and fed into an upper region of the first column 11 by means of a pump 8.
  • An alternative feed position below the removal position of the top gas from the first column is illustrated by dashed lines.
  • An alternative embodiment, which represents a variant of the air separation plant 1002 according to FIG. 2, is illustrated in FIG. 19 in the form of the air separation plant 1019.
  • the air separation plant 1003 illustrated in FIG. 3 differs from the air separation plant 1001 shown in FIG. 1 essentially in that instead of dividing the feed air flow a into the two partial flows b and c and treating them separately, the entire input air flow a, as previously only the partial flow c , the further pressure increase in the booster
  • Booster turbine assembly 5 subjected, cooled in the not separately designated aftercooler, fed to the main heat exchanger 4 on the warm side, the Main heat exchanger 4 is taken at the intermediate temperature level, then expanded in the turbine of the booster turbine arrangement 5 and fed into the first column 11.
  • the entire feed air in the air separation plant 1003 illustrated in FIG. 3 is brought to a significantly higher pressure level. No feed air is fed into the second column 12.
  • the air separation plant 1004 illustrated in FIG. 4 differs from the air separation plant 1002 shown in FIG. 2 essentially in the features already explained for the air separation plant 1003 according to FIG.
  • the air separation plant 1004 illustrated in FIG. 4 differs from the air separation plant 1002 shown in FIG. 2 essentially in the features already explained for the air separation plant 1003 according to FIG.
  • Air separation plant 1004 is set up to carry out a high-air pressure process in which all of the feed air is in the booster
  • Booster turbine assembly 5 is compressed. As in the one in Figure 3
  • a turbine illustrated in the air separation plant 1003 can also be provided which is not coupled to a booster in a booster turbine arrangement 5, but, for example, to a generator or an oil brake.
  • the air separation plant 1005 illustrated in FIG. 5 differs from the air separation plant 1002 shown for example in FIG. 2 in that the material flow s, which is emphasized here for reasons of clarity, is not combined with the material flow p.
  • the material flow s is instead routed to the warm side of the heat exchanger 4, as before the material flow q.
  • a recycle stream designated here as S is branched off from the material stream s and fed back to the main heat exchanger 4 on the warm side by means of a circuit compressor 9 with a downstream but not separately designated aftercooler, removed from it on the cold side and fed into the second column 12. Gas is therefore taken from the third column 13, heated, compressed, cooled and fed into the second column 12.
  • the material flow p is heated separately in the main heat exchanger 4 and provided as a gaseous oxygen product or used in some other way.
  • the air separation plant 1006 illustrated in FIG. 6 differs from the air separation plant 1005 shown in, for example, FIG. 5 in that the third column 13 is designed without a section which is used to provide
  • Low-pressure nitrogen in the form of the material flow r is used. A withdrawal of a corresponding material flow is therefore dispensed with, as is the feeding in of a material flow corresponding to the material flow m.
  • the material flow n is here by means of a further compressor 91, which is advantageously provided in a common apparatus with the circulation compressor 9, is compressed.
  • the air separation plant 1007 illustrated in FIG. 7 differs from the air separation plant 1006 shown, for example, in FIG. 6 by the feed of external liquid nitrogen illustrated here in the form of a stream 11 into the second column 12 or optionally also the first column 11.
  • the air separation plant 1008 illustrated in FIG. 8 differs, for example, from the air separation plant 1005 shown in FIG. 5 in that the condenser evaporator 111 of the first column 11 is designed as a forced-flow condenser evaporator.
  • a stream i from the condenser-evaporator 111 which can be a pure gas stream or a two-phase stream, is fed into the second column 12 as before. Since no stream corresponding to stream k is formed, instead liquid is removed from the bottom of the second column and treated accordingly in the form of stream K.
  • the air separation plant 1009 illustrated in FIG. 9 differs, for example, from the air separation plant 1005 shown in FIG. 5 in the absence of the pump 17. Instead of the previously in the form of the material flow h in the
  • the bottom liquid fed into the top condenser 111 of the first column 11 is the stream e used here, which is formed from the bottom liquid of the first column 11.
  • the stream h is instead used as before the stream e, and the stream k is fed into the second column 12 instead of into the third column 13.
  • One of the streams previously designated with f, which is now designated with F and is formed from liquid from the top condenser 151 of the fifth column 15, is fed into the third column 13 as before, or this third column 13 is equipped with an additional separating section and the Material flow F is fed in there in a suitable manner.
  • the air separation plant 1010 illustrated in FIG. 10 differs, for example, from the air separation plant 1005 shown in FIG. 5 in that the partial flow c, which is also here the main heat exchanger 4, is on a
  • the air separation plant 1011 illustrated in FIG. 11 differs, for example, from the air separation plant 1005 shown in FIG. 5 in that, in order to form the material flow denoted here by J, which is generated by means of the
  • Circulation pump 9 is fed back to the main heat exchanger 4, a partial flow of the material flow i is used.
  • the stream J is returned here to the first column 11 instead of to the second column 12.
  • the air separation plant 1012 illustrated in FIG. 12 differs, for example, from the air separation plant 1005 shown in FIG. 5 in that, in addition to the material flow denoted by S in FIG. 12
  • Air separation plant 1011 according to FIG. 11 labeled J and explained there is formed. These material flows S and J are by means of two
  • Circuit compressors 9a and 9b are supplied to the main heat exchanger 4.
  • Circuit compressors 9a and 9b are preferably designed as part of a common machine.
  • a connecting flow denoted by SJ can be omitted if the material flow J is formed in the manner shown. Instead, however, the material flow J upstream of the cycle compressor 9b can also completely pass through the
  • Connection stream SJ can be replaced.
  • the air separation plant 1013 illustrated in FIG. 13 differs, for example, from the air separation plant 1005 shown in FIG Adsorption unit 3 can be used.
  • the air separation plant 1014 illustrated in FIG. 14 differs, for example, from the air separation plant 1005 shown in FIG. 5 in that the partial flow c is recompressed by means of a booster 5a and that the partial flow b is expanded by means of a generator turbine 5b.
  • the substreams present in particular at the same pressure are combined as shown and fed together into the first column 13.
  • the air separation plant 1015 illustrated in FIG. 15 differs, for example, from the air separation plant 1002 shown in FIG. 2 in that the top condenser 111 of the first column 11 is fed with bottom liquid from the first column 11. For better differentiation, a corresponding material flow is designated here with h '.
  • the bottom liquid of the second column 12, on the other hand, is only fed to the third column 13 here.
  • a corresponding material flow is designated with k 'for the sake of better distinguishability.
  • fluid evaporated in the form of a material flow f from the top condenser 141 of the fourth column 14 is partially combined with the material flow s.
  • a production ratio between gaseous low-pressure nitrogen and gaseous pressure nitrogen can in particular be 0 to approx. 15 to 20%.
  • the air separation plant 1016 illustrated in FIG. 16 represents a variant of the air separation plant 1015 illustrated in FIG. 15, in which a (small) pump 17 'is present, by means of which part of the bottom liquid from the second column 12 in the form of a material flow h ′′ for compensation a possibly existing
  • Liquid deficit is pumped into the top condenser 111 of the first column 11 or into its evaporation chamber.
  • a production ratio between gaseous low-pressure nitrogen to gaseous pressure nitrogen cf. material flow g and material flow r
  • gaseous low-pressure nitrogen to gaseous pressure nitrogen can in particular be more than 15 to 20%.
  • the air separation plant 1017 illustrated in FIG. 17 represents a variant of the air separation plant 1016 illustrated in FIG. 16, in which in the
  • Top condenser 111 of the first column 11 or an additional separating section 112 is provided in its evaporation chamber. This functionally represents the lowermost separating section of the second column 12, which is present in the air separation plant 1016 illustrated in FIG. 16.
  • Air separation plant 1017 according to FIG. 17 therefore no longer has this separation section.
  • a corresponding configuration is also possible in systems without the production of gaseous low-pressure nitrogen.
  • the air separation plant 1018 illustrated in FIG. 18 differs from the air separation plants 1001 to 1017 previously shown in FIGS. 1 to 17 in that the fifth column 15 is not provided and that the third column 13, which is accordingly designed with one fewer separating section, does not the material flow corresponding to the material flow r is taken.
  • Liquid nitrogen can be implemented here in the form of a material flow L.
  • the air separation plant 1019 illustrated in FIG. 19 represents in particular a variant of the air separation plant 1002 according to FIG. 2.
  • part of the bottom liquid from the second column 12 is denoted by k 'as in FIGS Material flow in the third column 13 and a further part by means of a pump 17 'in the form of a
  • Material flow h ′′ is fed into the evaporation space of the top condenser 111. Liquid from the evaporation space of the top condenser 111 is combined with the material flow i and fed into the second column 12 with this.

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Abstract

La présente invention concerne un procédé de décomposition d'air à basse température avec production d'azote à une pression dans une plage de pressions de 9 à 12 bars et avec production d'argon. Ledit procédé emploie une installation d'air (1001-1019) munie d'un système de colonnes (10) qui comprend une première colonne (11), une deuxième colonne (12), une troisième colonne (13) et une quatrième colonne (14). Un premier liquide de décantation est formé dans la première colonne (11), un deuxième liquide de décantation est formé dans la deuxième colonne (12), un troisième liquide de décantation est formé dans la troisième colonne (13), un quatrième liquide de décantation est formé dans la quatrième colonne (14). La première colonne (11) est exploitée dans une première plage de pressions, la deuxième colonne (12) est exploitée dans une deuxième plage de pressions en dessous de la première plage de pressions et la troisième colonne (13) est exploitée dans une troisième plage de pressions en dessous de la deuxième plage de pressions. Le deuxième liquide de décantation est formé avec une teneur en oxygène et une teneur en argon qui sont supérieures à celles du premier liquide de décantation, et le troisième liquide de décantation est formé avec une teneur en oxygène supérieure à celle du second liquide de décantation et avec une teneur en argon inférieure à celle du second liquide de décantation. Le fluide provenant de la première colonne (11) est introduit dans la seconde colonne (12) et dans la troisième colonne (13), le fluide provenant de la deuxième colonne (12) est introduit dans la troisième colonne (13), le fluide provenant de la troisième colonne (13) est introduit dans la quatrième colonne (14) et le fluide provenant de la quatrième colonne (14) est introduit dans la troisième colonne (13). Le fluide provenant de la troisième colonne (13) introduit dans la quatrième colonne (14) comporte au moins une part d'un flux latéral qui, avec une teneur en oxygène inférieure à celle du troisième liquide de décantation et une teneur en argon supérieure à celle du troisième liquide de décantation, est prélevé de la troisième colonne (13). Selon la présente invention, une condensation du gaz de tête de la deuxième colonne (12) forme un liquide de retour et le liquide de retour est introduit au moyen d'une pompe (8) sous forme liquide dans la première colonne (11). La présente invention a en outre pour objet une installation correspondante (1001-1019).
PCT/EP2020/025083 2019-02-22 2020-02-21 Procédé et installation de décomposition d'air à basse température WO2020169257A1 (fr)

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JP7329714B1 (ja) * 2023-04-28 2023-08-18 大陽日酸株式会社 窒素製造方法及び装置
EP4317877A1 (fr) 2022-08-01 2024-02-07 Air Products and Chemicals, Inc. Procédé et dispositif pour la récupération d'au moins de l'azote et de l'argon
EP4357708A2 (fr) 2022-10-18 2024-04-24 Air Products and Chemicals, Inc. Procédé et dispositif pour la récupération améliorée d'argon

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EP4317877A1 (fr) 2022-08-01 2024-02-07 Air Products and Chemicals, Inc. Procédé et dispositif pour la récupération d'au moins de l'azote et de l'argon
EP4357708A2 (fr) 2022-10-18 2024-04-24 Air Products and Chemicals, Inc. Procédé et dispositif pour la récupération améliorée d'argon
JP7329714B1 (ja) * 2023-04-28 2023-08-18 大陽日酸株式会社 窒素製造方法及び装置

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