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EP1357342A1 - Cryogenic triple column air separation system with argon recovery - Google Patents

Cryogenic triple column air separation system with argon recovery Download PDF

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Publication number
EP1357342A1
EP1357342A1 EP02011458A EP02011458A EP1357342A1 EP 1357342 A1 EP1357342 A1 EP 1357342A1 EP 02011458 A EP02011458 A EP 02011458A EP 02011458 A EP02011458 A EP 02011458A EP 1357342 A1 EP1357342 A1 EP 1357342A1
Authority
EP
European Patent Office
Prior art keywords
argon
column
pressure column
nitrogen
low
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP02011458A
Other languages
German (de)
French (fr)
Other versions
EP1357342B1 (en
Inventor
Dietrich Rottmann
Christian Kunz
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Linde GmbH
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Linde GmbH
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Publication date
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Publication of EP1357342A1 publication Critical patent/EP1357342A1/en
Application granted granted Critical
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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
    • F25J3/04151—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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another 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
    • F25J3/04078—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
    • F25J3/04187—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/04309—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 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
    • F25J3/04284—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
    • F25J3/04327—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 argon or argon enriched 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
    • 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
    • F25J3/04436—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 at least a triple pressure main column system
    • F25J3/04454—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 at least a triple pressure main column system a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
    • 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
    • F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/50—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/58—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams

Definitions

  • the invention relates to a method for low-temperature separation of air with the Features (a) to (d) of claim 1.
  • Methods and devices for the low-temperature separation of air are generally out Hausen / Linde, low-temperature technology, 2nd edition 1985, chapter 4 (pages 281 to 337) known.
  • a medium pressure column is used, which is operated under a pressure that lies between the operating pressures of the high pressure column and the low pressure column (see also Plank, Handbuch der Kältetechnik, Volume 8, 1957, page 194/195).
  • Insert fraction for the medium pressure column either serves at least part of one oxygen-enriched liquid from the high pressure column or a partial flow of Deployment air or both.
  • the medium pressure column can be used with a sump evaporator and / or be equipped with a top capacitor. Head and / or bottom products the medium pressure column is usually fed to the low pressure column and / or subtracted as a product under intermediate pressure.
  • a fraction is referred to as "argon enriched" if its argon content is higher than that of atmospheric air and for example 3 to 14 mol%, is preferably 5 to 14 mol%.
  • the invention has for its object to provide such a 3-pillar system, which enables particularly efficient argon production.
  • a relatively high level is also formed in the intermediate pressure column at an intermediate point Argon concentration (the "argon belly").
  • This argon enrichment is in the Framework of the invention used for argon production by at least a part of the Use of the crude argon column from approximately this intermediate point of the medium pressure column is subtracted.
  • This argon-enriched fraction is under higher pressure than that Low pressure column (approx. 5.5 bar if the low pressure column is below approx Atmospheric pressure is operated) and thus also contains a pressure potential that in Framework of the invention for the improvement of argon production is available.
  • the rectification system for nitrogen-oxygen separation can in the invention by any type of three or more pillar system can be formed, for example by a pure gas apparatus, an internal compression system or a liquid system (if necessary with a two or more turbine air or nitrogen circuit).
  • the usual compound can be used in the method according to the invention exist between the low pressure column and crude argon column, via which a second withdrawn argon-enriched stream from the low pressure column and into the Raw argon column is introduced.
  • argon enrichment Through the simultaneous use of argon enrichment The economy can be achieved in the medium pressure column and low pressure column the argon production further increase.
  • the sump liquid of the raw argon column is at least partially in the Medium pressure column returned. Since the raw argon column in the invention usually is operated under a pressure which is lower than the medium pressure column pressure (and for example approximately equal to the low pressure column pressure) is used for the return a liquid pump is generally used for the crude argon column bottom liquid.
  • the Condenser-evaporator is preferably the intermediate or bottom evaporator Raw argon column formed by removing part of a liquid from the Raw argon column, in particular a part of its bottom liquid, is evaporated.
  • the Pressure drop between the medium pressure column and crude argon column is thus used of the condenser evaporator.
  • the first argon-enriched stream is between condenser evaporator and feed into the medium pressure column and / or relaxed upstream of the condenser-evaporator.
  • the raw argon column is preferably fed in at an intermediate point, the for example 1 to 8 theoretical plates, preferably 2 to 6 theoretical plates Soils above the sump of the raw argon column, with a total of for example 45 to 200 theoretical plates, preferably 45 to 180 theoretical plates Soils in the raw argon column. If, in addition, a second argon-enriched stream is brought out of the low pressure column, it is fed into the Raw argon column lower, for example directly above the swamp.
  • the above-mentioned pressure potential can be used, by at least a portion of the first argon enriched stream upstream of the Introduction into the crude argon column relaxed work and thus for production of process cold can be used. Upstream of the workers The current is relaxed, preferably to an intermediate temperature in indirect heat exchange for feed air, for example in Main heat exchanger.
  • the invention also relates to a device for the low-temperature separation of air according to claim 7.
  • a first feed air stream 1 is compressed in a first air compressor 2 with aftercooler 3 to approximately the operating pressure of the high-pressure column described below (plus line losses).
  • the first air stream 4 then branches into a direct air stream 5 and a turbine air stream 6.
  • the direct air 5 is fed directly to the warm end of a main heat exchanger 7 and is cooled there to approximately dew point.
  • the cooled direct air 8 flows to the high-pressure column 9 without any further pressure-changing measures.
  • the high-pressure column 9 is part of a rectification system for nitrogen-oxygen separation, which also comprises a medium-pressure column 10 and a low-pressure column 11. Their operating pressures are (each at the head): High-pressure column owing 14.5 to 17 bar, for example about 15 bar Medium pressure column owing 5 to 6 bar, for example about 5.5 bar Low pressure column owing 1.2 to 1.5 bar, for example about 1.3 bar
  • the columns stand between the high pressure column via a first main condenser 12 and medium pressure column or a second main condenser 13 between Medium pressure column and low pressure column in a heat-exchanging connection.
  • Main condensers are head gas of the respective lower column in a known manner indirect heat exchange with evaporating sump liquid of the respective upper one Column condensed.
  • the turbine air flow 6, 16 is in a post-compressor 14 with an after-cooler 15 post-compressed, cooled to an intermediate temperature in the main heat exchanger 7 and via line 17 of work relaxation in a relaxation machine (Blowing turbine) 18, which is mechanically coupled to the post-compressor 14 is.
  • the relaxed turbine air 19 is finally fed directly into the low pressure column 11 blown.
  • the embodiment relates to an application in which limited Amount of air is already available under a superatmospheric pressure, for example, the medium pressure column pressure (plus line losses).
  • a superatmospheric pressure for example, the medium pressure column pressure (plus line losses).
  • Air flow - for example from a gas turbine-driven compressor or from other source - flows in the exemplary embodiment as a second feed air stream 20 towards the warm end of the main heat exchanger there will be about dew point cooled and finally fed directly to the medium pressure column 10.
  • Oxygenated liquid 22 is discharged from the sump of the high pressure column 9 withdrawn, cooled in a first subcooling countercurrent 23, via line 24 and throttle valve 25 inserted into the medium pressure column and there for the first part subjected to a further countercurrent rectification. To another part 26 he becomes passed through a second supercooling counterflow 27.
  • the hypothermic oxygen-enriched liquid 28 at intermediate pressure branches into two parts 29, 31, one of which is throttled via valve 30 into the low-pressure column 11.
  • On Part 33 of the gaseous top nitrogen of the high pressure column 9 is in the Main heat exchanger 7 warmed to about ambient temperature and below that High pressure column pressure obtained as product 34 (GAN).
  • Some of the nitrogen obtained in the first main condenser 12 is subcooled 35 (23) and given as return 36 on the head of the medium pressure column 10. Moreover generates the second main condenser 13 return 37 for the medium pressure column, as well if necessary liquid nitrogen product 38.
  • An oxygen with a purity of about 99.5 is obtained from the bottom of the medium pressure column mol% withdrawn liquid and introduced into a secondary condenser 40. There he is in indirect heat exchange with condensing top nitrogen 41 the High pressure column 9 partially evaporated. A first, somewhat impure oxygen product 42, 43 becomes from the steam formed under approximately the medium pressure column pressure won (GOX), possibly after compression in the second stage 44 one Oxygen compressor 56/44 with after-cooling 45. From the in the secondary condenser 40 portion 46 remaining in liquid form becomes a purer high-pressure oxygen product by means of internal compression 49 (GOX-IC) generated.
  • GOX-IC internal compression 49
  • the liquid 46 by means of a Pump 47 brought to a corresponding pressure, via a liquid line 48 led to the cold end of the main heat exchanger and evaporated there and warmed up.
  • a portion 82 of the gaseous nitrogen from the top of the medium pressure column becomes warmed in the main heat exchanger 7 and can via line 83 or - as shown -
  • line 86 after compression in a nitrogen compressor 84 with Post-compressor 85 can be obtained as a printed product (PGAN).
  • Return liquid 50, 51 for the head of the low pressure column 11 is from a Intermediate point of the medium pressure column 10 above the feed 24/25 oxygen-enriched liquid removed.
  • impure nitrogen 52 is removed as residual gas and after heating 27-23-7 removed from the system via line 53 (UN2).
  • the bottom product 54 of the Low-pressure column 11 is partially withdrawn in gaseous form, after heating 27-23-7 via line 55 of the first stage 56 (with intermediate cooling 57) of the Oxygen compressor 56/44 brought to about medium pressure column pressure and finally mixed with the medium pressure column oxygen 43. It can also be more fluid Oxygen 58 as a product or for flushing from the low pressure column sump subtracted from.
  • a first argon-enriched stream 59 is gaseous from an intermediate point in the Subtracted medium pressure column 10, the 24/25 below the feed oxygen-enriched liquid and below the air supply via line 21 is arranged.
  • the stream 59 is at least in a condenser-evaporator 60 partially, preferably completely condensed and finally via line 61 and Throttle valve 62 is introduced into a crude argon column 63, which is under approximately the same pressure how the low pressure column 11 is operated.
  • the entry point of the first argon-enriched electricity is, for example, 30 to 40 theoretical plates, preferably 33 to 38 theoretical plates above the swamp at one Total number of 70 to 90 theoretical plates, preferably 78 to 85 theoretical plates Soils in the crude argon column 63.
  • the condenser-evaporator 60 simultaneously represents the Bottom reboiler of the crude argon column 63.
  • Part 65 of the non-evaporated Bottom liquid 64 of the crude argon column 63 is opened again in a pump 65 Brought medium pressure column pressure and returned to the medium pressure column 10 (66).
  • the Rest 67 is introduced into the low pressure column 11.
  • Another use is a second argon-enriched stream 68 in gaseous form from the Low pressure column 11 of the crude argon column fed directly to the sump.
  • the top condenser 69 of the crude argon column 63 is enriched with oxygen Liquid 31 operated in a valve to a suitable pressure (about the same Low pressure column pressure) was released. Vapor formed in the top condenser 69 70 is introduced into the low pressure column at a suitable point.
  • the raw argon product (the "argon-rich fraction") 75 becomes gaseous from the top of the crude argon column 63 or withdrawn from the liquefaction space of the top condenser 69.
  • the first argon-enriched stream 259 is warmed to an intermediate temperature in the main heat exchanger 7, passed to a relaxation machine 272 via line 271, where it is relieved of work to about 0.2 bar above crude argon column pressure and finally led into the evaporation space of the condenser-evaporator 60 (274 ).
  • the expansion machine 272 is preferably designed as a turbine and coupled to a braking device 273, preferably a generator.
  • FIG. 3 largely corresponds to FIG. 2, but here a sump reboiler for the crude argon column 63 is dispensed with and the first argon-enriched stream 374, which is relaxed during the work, is introduced in gaseous form into the sump of the crude argon column.
  • the argon transfer turbine (272 in FIG. 2) is also dispensed with and the first argon-enriched stream 459 is throttled directly into the bottom of the crude argon column 63 (462).
  • FIGS. 5 to 9 show alternatives to the blowing in of FIG Turbine air 19 in the low pressure column. These different methods of Refrigeration can also be combined with any of the methods of Figures 2 to 4 become.
  • the air turbine 518 only relaxes to approximately the operating pressure of the medium pressure column 10. This variant is therefore particularly suitable when the cooling requirement is relatively low and increases the oxygen yield of the process.
  • the air 519 which has been relieved of work is fed into the medium-pressure column 10 together with the second feed air stream 20-21 via line 521.
  • FIG. 6 relates to a modification of FIG. 5, in which the turbine air 6 upstream of the turbine-driven post-compressor 14 is compressed in a further post-compressor 681 driven by external energy with post-cooling 682.
  • a higher pressure ratio can be achieved on the turbine 518 and thus produce more cold.
  • process cold can be obtained in a nitrogen turbine 718 according to FIG. 7 .
  • part 787 of the nitrogen 33 drawn off from the high-pressure column 9 is only heated to an intermediate temperature in the main heat exchanger 7 and expanded to approximately medium-pressure column pressure in a work-performing manner (718).
  • the expanded high-pressure column nitrogen is finally combined with the medium-pressure column nitrogen 82 upstream of the main heat exchanger 7.
  • the nitrogen turbine 718 is not coupled to a generator or to an oil brake as in FIG. 7, but is braked by means of a post-compressor 814, which increases the pressure in the turbine stream 887 and thus the inlet pressure of the turbine 718.
  • the corresponding part 887 of the high-pressure column nitrogen is previously warmed to approximately ambient temperature and cooled downstream of the post-compressor 814 by means of an after-cooler 815.
  • part 988 of the gaseous nitrogen 82 is made from the Medium pressure column 10 relaxed from an intermediate temperature from work.
  • the Relaxation machine is, for example, by an oil brake or a Generator braked.
  • the expanded nitrogen gas 989 is practically depressurized and will withdrawn below ambient temperature via line 990 (GAN).
  • FIG. 10 is based on FIG. 1, but shows a changed routing of the oxygen product from the low-pressure column 11.
  • the entire bottom product is removed from the low-pressure column in liquid form (line 1076).
  • the part that is not discharged via line 1058 as a liquid oxygen product or rinsing liquid flows through line 1077 to a pump 1078 and is brought to approximately medium-pressure column pressure there.
  • the pumped low-pressure column oxygen 1079 is warmed in the first supercooling countercurrent 27 and finally introduced into the medium-pressure column 10 via line 1080.
  • Line 39 now conveys all of the oxygen to be obtained in gaseous form, which was produced in medium pressure column 10 and low pressure column 11. This "pumping back" of the low-pressure column oxygen into the medium-pressure column can be applied in an analogous manner to the exemplary embodiments in FIGS. 2 to 9 and their variants.
  • the exemplary embodiments show a rectification system for nitrogen-oxygen separation, which is designed as a triple column in the narrower sense, that is High pressure column, medium pressure column and low pressure column are arranged one above the other and are in pairs over a main condenser 12, 13 in heat exchangers Connection.
  • the invention is also applicable to any other 3-pillar system applicable.
  • the medium pressure column next to a classic Linde double column be arranged, which comprises high pressure column and low pressure column; alternatively, all three pillars could be arranged side by side.
  • Others too Condenser configurations for the low pressure column, the medium pressure column and for the High pressure columns can be used in the context of the invention.

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Abstract

In a three-sage cryogenic air rectification process for the abstraction of air, the first argon-enriched flow (59, 61) is especially taken from a medium-pressure column (10). A cryogenic gas rectification system has three columns for the extraction of argon from air. The assembly has high (9), medium (10) and low-pressure (11) columns and is linked to a raw argon column (63). The system has an inlet for ambient air which is rectified to separate oxygen and nitrogen. Oxygen or nitrogen (52, 54, 58) is extracted from the low-pressure column. A first flow of argon-enriched gas (59, 61) is abstracted from the nitrogen/oxygen rectification system and surrendered to the raw argon column (63). An argon-rich fraction (75) is drawn from the column (63) and has an argon content greater than that of the first argon-enriched flow (59, 61). The first argon-enriched flow (59, 61) is taken from the medium-pressure column (10).

Description

Die Erfindung betrifft ein Verfahren zur Tieftemperatur-Zerlegung von Luft mit den Merkmalen (a) bis (d) des Patentanspruchs 1.The invention relates to a method for low-temperature separation of air with the Features (a) to (d) of claim 1.

Verfahren und Vorrichtungen zur Tieftemperaturzerlegung von Luft sind allgemein aus Hausen/Linde, Tieftemperaturtechnik, 2. Auflage 1985, Kapitel 4 (Seiten 281 bis 337) bekannt. Bei dem vorliegenden Verfahren wird zusätzlich zu der Hochdrucksäule und der Niederdrucksäule eines klassischen 2-Säulen-Systems zur Stickstoff-Sauerstoff-Trennung eine Mitteldrucksäule eingesetzt, die unter einem Druck betrieben wird, der zwischen den Betriebsdrücken von Hochdrucksäule und Niederdrucksäule liegt (siehe auch Plank, Handbuch der Kältetechnik, 8. Band, 1957, Seite 194/195). Als Einsatzfraktion für die Mitteldrucksäule dient entweder mindestens ein Teil einer sauerstoffangereicherten Flüssigkeit aus der Hochdrucksäule oder ein Teilstrom der Einsatzluft oder beides. Die Mitteldrucksäule kann mit einem Sumpfverdampfer und/oder mit einem Kopfkondensator ausgerüstet sein. Kopf- und/oder Sumpfprodukte der Mitteldrucksäule werden üblicherweise der Niederdrucksäule zugespeist und/oder als Produkt unter Zwischendruck abgezogen.Methods and devices for the low-temperature separation of air are generally out Hausen / Linde, low-temperature technology, 2nd edition 1985, chapter 4 (pages 281 to 337) known. In the present method, in addition to the high pressure column and the low pressure column of a classic 2-column system for nitrogen-oxygen separation a medium pressure column is used, which is operated under a pressure that lies between the operating pressures of the high pressure column and the low pressure column (see also Plank, Handbuch der Kältetechnik, Volume 8, 1957, page 194/195). As Insert fraction for the medium pressure column either serves at least part of one oxygen-enriched liquid from the high pressure column or a partial flow of Deployment air or both. The medium pressure column can be used with a sump evaporator and / or be equipped with a top capacitor. Head and / or bottom products the medium pressure column is usually fed to the low pressure column and / or subtracted as a product under intermediate pressure.

Drei-Säulen-Luftzerleger-Systeme sind außerdem bekannt aus DE 1041989 (=US 3091094), DE 1065867 (=US 3100696), US 3490246, DE 2903089 (=US 4356013), EP 768503 B1 (=US 5730004) und EP 949471 A1 (=US 6185960). Auch die noch zu veröffentlichenden Anmeldungen DE 10052180 A1 (und korrespondierende EP-Anmeldung 01103828.8), DE 10103968 A1 (und korrespondierende Anmeldungen), DE 10103957 A1 (und korrespondierende Anmeldungen) betreffen derartige Drei-Säulen-Verfahren.Three-column air separation systems are also known from DE 1041989 (= US 3091094), DE 1065867 (= US 3100696), US 3490246, DE 2903089 (= US 4356013), EP 768503 B1 (= US 5730004) and EP 949471 A1 (= US 6185960). Even that too published applications DE 10052180 A1 (and corresponding EP application 01103828.8), DE 10103968 A1 (and corresponding applications), DE 10103957 A1 (and corresponding applications) relate to such three-pillar processes.

Ein Drei-Säulen-Verfahren mit Argongewinnung der eingangs genannten Art ist aus DE 19609490 (=US 5669237), Figur 8 bekannt. Die Rohargonsäule ist hier - analog zu einem Zwei-Säulen-System mit Hochdrucksäule und Niederdrucksäule - als Seitenkolonne zu der Niederdrucksäule ausgebildet. Diese Verbindung zwischen Niederdrucksäule und Rohargonsäule ist auch bei den Drei-Säulen-Prozessen der nicht vorveröffentlichten Anmeldungen DE 10113791 A1 und DE 10113790 A1 realisiert.A three-column process with argon recovery of the type mentioned is over DE 19609490 (= US 5669237), Figure 8 is known. The raw argon column is here - analogous to a two-column system with high-pressure column and low-pressure column - as Side column formed to the low pressure column. This connection between Low pressure column and raw argon column is also the case with the three-column processes not previously published applications DE 10113791 A1 and DE 10113790 A1 realized.

Als "argonangereichert" wird hier eine Fraktion bezeichnet, wenn ihr Argongehalt höher als derjenige der atmosphärischen Luft ist und beispielsweise 3 bis 14 mol-%, vorzugsweise 5 bis 14 mol-% beträgt.A fraction is referred to as "argon enriched" if its argon content is higher than that of atmospheric air and for example 3 to 14 mol%, is preferably 5 to 14 mol%.

Der Erfindung liegt die Aufgabe zugrunde, ein derartiges 3-Säulen-System anzugeben, das eine besonders effiziente Argongewinnung ermöglicht.The invention has for its object to provide such a 3-pillar system, which enables particularly efficient argon production.

Diese Aufgabe wird dadurch gelöst, dass der erste argonangereicherte Strom, der als Einsatz für die Rohargonsäule dient, aus der Mitteldrucksäule entnommen wird.This problem is solved in that the first argon-enriched stream, the Use for the crude argon column, is taken from the medium pressure column.

Auch in der Mitteldrucksäule bildet sich an einer Zwischenstelle eine relativ hohe Argonkonzentration (der "Argonbauch") aus. Diese Argon-Anreicherung wird im Rahmen der Erfindung zur Argongewinnung genutzt, indem mindestens ein Teil des Einsatzes der Rohargonsäule von ungefähr dieser Zwischenstelle der Mitteldrucksäule abgezogen wird.A relatively high level is also formed in the intermediate pressure column at an intermediate point Argon concentration (the "argon belly"). This argon enrichment is in the Framework of the invention used for argon production by at least a part of the Use of the crude argon column from approximately this intermediate point of the medium pressure column is subtracted.

Diese argonangereicherte Fraktion steht unter einem höherem Druck als die Niederdrucksäule (etwa 5,5 bar, wenn die Niederdrucksäule unter etwa Atmosphärendruck betrieben wird) und enthält damit femer ein Druckpotential, das im Rahmen der Erfindung für die Verbesserung der Argongewinnung zu Verfügung steht.This argon-enriched fraction is under higher pressure than that Low pressure column (approx. 5.5 bar if the low pressure column is below approx Atmospheric pressure is operated) and thus also contains a pressure potential that in Framework of the invention for the improvement of argon production is available.

Das Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung kann bei der Erfindung durch jede Art von Drei- oder Mehr-Säulen-System gebildet werden, beispielsweise durch einen reinen Gasapparat, eine Innenverdichtungsanlage oder eine Flüssiganlage (gegebenenfalls mit Zwei- oder Mehr-Turbinen-Luft- oder -Stickstoff-Kreislauf).The rectification system for nitrogen-oxygen separation can in the invention by any type of three or more pillar system can be formed, for example by a pure gas apparatus, an internal compression system or a liquid system (if necessary with a two or more turbine air or nitrogen circuit).

Zusätzlich kann bei dem erfindungsgemäßen Verfahren die übliche Verbindung zwischen Niederdrucksäule und Rohargonsäule bestehen, über die ein zweiter argonangereicherter Strom aus der Niederdrucksäule abgezogen und in die Rohargonsäule eingeleitet wird. Durch die gleichzeitige Ausnutzung der Argon-Anreicherung in Mitteldrucksäule und Niederdrucksäule lässt sich die Wirtschaftlichkeit der Argongewinnung weiter erhöhen. In addition, the usual compound can be used in the method according to the invention exist between the low pressure column and crude argon column, via which a second withdrawn argon-enriched stream from the low pressure column and into the Raw argon column is introduced. Through the simultaneous use of argon enrichment The economy can be achieved in the medium pressure column and low pressure column the argon production further increase.

Die Sumpfflüssigkeit der Rohargonsäule wird mindestens teilweise in die Mitteldrucksäule zurückgeführt. Da die Rohargonsäule bei der Erfindung in der Regel unter einem Druck betrieben wird, der niedriger als der Mitteldrucksäulendruck (und beispielsweise etwa gleich dem Niederdrucksäulendruck) ist, wird für die Rückführung der Rohargonsäulen-Sumpfflüssigkeit im Allgemeinen eine Flüssigpumpe eingesetzt.The sump liquid of the raw argon column is at least partially in the Medium pressure column returned. Since the raw argon column in the invention usually is operated under a pressure which is lower than the medium pressure column pressure (and for example approximately equal to the low pressure column pressure) is used for the return a liquid pump is generally used for the crude argon column bottom liquid.

Ein Möglichkeit, das oben erwähnte Druckpotential einzusetzen, das im Rahmen der Erfindung zur Verfügung steht, besteht darin, dass mindestens ein Teil des ersten argonangereicherten Stroms stromaufwärts der Einleitung in die Rohargonsäule in einem Kondensator-Verdampfer mindestens teilweise kondensiert wird. Der Kondensator-Verdampfer ist vorzugsweise als Zwischen- oder Sumpfverdampfer der Rohargonsäule ausgebildet, indem dort ein Teil einer Flüssigkeit aus der Rohargonsäule, insbesondere ein Teil deren Sumpfflüssigkeit, verdampft wird. Das Druckgefälle zwischen Mitteldrucksäule und Rohargonsäule wird somit zum Betreiben des Kondensator-Verdampfers ausgenutzt. Der erste argonangereicherte Strom wird zwischen Kondensator-Verdampfer und Einspeisung in die Mitteldrucksäule und/oder stromaufwärts des Kondensator-Verdampfers entspannt.One way to use the pressure potential mentioned above, which in the context of Invention is available is that at least part of the first argon enriched stream upstream of the introduction into the crude argon column in a condenser-evaporator is at least partially condensed. The Condenser-evaporator is preferably the intermediate or bottom evaporator Raw argon column formed by removing part of a liquid from the Raw argon column, in particular a part of its bottom liquid, is evaporated. The Pressure drop between the medium pressure column and crude argon column is thus used of the condenser evaporator. The first argon-enriched stream is between condenser evaporator and feed into the medium pressure column and / or relaxed upstream of the condenser-evaporator.

Die Einspeisung in die Rohargonsäule erfolgt vorzugsweise an einer Zwischenstelle, die beispielsweise 1 bis 8 theoretische Böden, vorzugsweise 2 bis 6 theoretische Böden oberhalb des Sumpfs der Rohargonsäule liegt, bei einer Gesamtzahl von beispielsweise 45 bis 200 theoretische Böden, vorzugsweise 45 bis 180 theoretischen Böden in der Rohargonsäule. Falls zusätzlich ein zweiter argonangereicherter Strom aus der Niederdrucksäule herangeführt wird, erfolgt dessen Zuspeisung in die Rohargonsäule tiefer, beispielsweise unmittelbar über dem Sumpf.The raw argon column is preferably fed in at an intermediate point, the for example 1 to 8 theoretical plates, preferably 2 to 6 theoretical plates Soils above the sump of the raw argon column, with a total of for example 45 to 200 theoretical plates, preferably 45 to 180 theoretical plates Soils in the raw argon column. If, in addition, a second argon-enriched stream is brought out of the low pressure column, it is fed into the Raw argon column lower, for example directly above the swamp.

Alternativ oder zusätzlich kann das oben erwähnte Druckpotential ausgenutzt werden, indem mindestens ein Teil des ersten argonangereicherten Stroms stromaufwärts der Einleitung in die Rohargonsäule arbeitsleistend entspannt und damit zur Erzeugung von Verfahrenskälte eingesetzt werden. Stromaufwärts der arbeitsleistenden Entspannung wird der Strom auf eine Zwischentemperatur angewärmt, vorzugsweise in indirektem Wärmeaustausch gegen Einsatzluft, beispielsweise im Hauptwärmetauscher. Alternatively or additionally, the above-mentioned pressure potential can be used, by at least a portion of the first argon enriched stream upstream of the Introduction into the crude argon column relaxed work and thus for production of process cold can be used. Upstream of the workers The current is relaxed, preferably to an intermediate temperature in indirect heat exchange for feed air, for example in Main heat exchanger.

Die Erfindung betrifft außerdem eine Vorrichtung zur Tieftemperaturzerlegung von Luft gemäß Patentanspruch 7.The invention also relates to a device for the low-temperature separation of air according to claim 7.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand von in den Zeichnungen schematisch dargestellten Ausführungsbeispielen näher erläutert. Hierbei zeigen:

Figur 1
ein erstes Ausführungsbeispiel der Erfindung mit Sumpfheizung der Rohargonsäule mit der Argonübergangs-Fraktion aus der Mitteldrucksäule,
Figur 2
ein zweites Verfahren, bei dem die Argonübergangs-Fraktion aus der Mitteldrucksäule außerdem arbeitsleistend entspannt wird,
Figur 3
ein drittes Beispiel ohne Sumpfheizung der Rohargonsäule,
Figur 4
ein Verfahren mit direkter Einleitung der Argonübergangs-Fraktion aus der Mitteldrucksäule in die Rohargonsäule,
Figuren 5 bis 9
verschiedene Varianten der Kältegewinnung bei einem Verfahren der Figur 1 (auch auf die Verfahren der Figuren 2 bis 4 anwendbar) und
Figur 10
ein Prozess mit Zurückpumpen von Sauerstoff aus der Niederdrucksäule in die Mitteldrucksäule.
The invention and further details of the invention are explained in more detail below on the basis of exemplary embodiments schematically illustrated in the drawings. Here show:
Figure 1
a first embodiment of the invention with bottom heating of the crude argon column with the argon transfer fraction from the medium pressure column,
Figure 2
a second method in which the argon transition fraction from the medium pressure column is also expanded to perform work,
Figure 3
a third example without sump heating of the crude argon column,
Figure 4
a method with direct introduction of the argon transition fraction from the medium pressure column into the crude argon column,
Figures 5 to 9
different variants of the cold generation in a method of Figure 1 (also applicable to the methods of Figures 2 to 4) and
Figure 10
a process of pumping back oxygen from the low pressure column to the medium pressure column.

Bei dem Verfahren von Figur 1 wird ein erster Einsatzluftstrom 1 in einem ersten Luftverdichter 2 mit Nachkühler 3 auf etwa den Betriebsdruck der unten beschriebenen Hochdrucksäule (plus Leitungsverluste) verdichtet. Der erste Luftstrom 4 verzweigt anschließend in einen Direktluftstrom 5 und einen Turbinenluftstrom 6. Die Direktluft 5 wird unmittelbar dem warmen Ende eines Hauptwärmetauschers 7 zugeführt und dort auf etwa Taupunkt abgekühlt. Die abgekühlte Direktluft 8 strömt ohne weitere druckverändernde Maßnahmen der Hochdrucksäule 9 zu.In the method of FIG. 1 , a first feed air stream 1 is compressed in a first air compressor 2 with aftercooler 3 to approximately the operating pressure of the high-pressure column described below (plus line losses). The first air stream 4 then branches into a direct air stream 5 and a turbine air stream 6. The direct air 5 is fed directly to the warm end of a main heat exchanger 7 and is cooled there to approximately dew point. The cooled direct air 8 flows to the high-pressure column 9 without any further pressure-changing measures.

Die Hochdrucksäule 9 ist Teil eines Rektifiziersystems zur Stickstoff-Sauerstoff-Trennung, das außerdem eine Mitteldrucksäule 10 und eine Niederdrucksäule 11 umfasst. Ihre Betriebsdrücke betragen (jeweils am Kopf): Hochdrucksäule..... 14,5 bis 17 bar, beispielsweise etwa 15 bar Mitteldrucksäule ..... 5 bis 6 bar, beispielsweise etwa 5,5 bar Niederdrucksäule ..... 1,2 bis 1,5 bar, beispielsweise etwa 1,3 bar The high-pressure column 9 is part of a rectification system for nitrogen-oxygen separation, which also comprises a medium-pressure column 10 and a low-pressure column 11. Their operating pressures are (each at the head): High-pressure column ..... 14.5 to 17 bar, for example about 15 bar Medium pressure column ..... 5 to 6 bar, for example about 5.5 bar Low pressure column ..... 1.2 to 1.5 bar, for example about 1.3 bar

Die Säulen stehen über einen ersten Hauptkondensator 12 zwischen Hochdrucksäule und Mitteldrucksäule beziehungsweise einen zweiten Hauptkondensator 13 zwischen Mitteldrucksäule und Niederdrucksäule in wärmetauschender Verbindung. In den Hauptkondensatoren wird auf bekannte Weise Kopfgas der jeweiligen unteren Säule in indirektem Wärmeaustausch mit verdampfender Sumpfflüssigkeit der jeweiligen oberen Säule kondensiert.The columns stand between the high pressure column via a first main condenser 12 and medium pressure column or a second main condenser 13 between Medium pressure column and low pressure column in a heat-exchanging connection. In the Main condensers are head gas of the respective lower column in a known manner indirect heat exchange with evaporating sump liquid of the respective upper one Column condensed.

Der Turbinenluftstrom 6, 16 wird in einem Nachverdichter 14 mit Nachkühler 15 nachverdichtet, im Hauptwärmetauscher 7 auf eine Zwischentemperatur abgekühlt und über Leitung 17 der arbeitsleistenden Entspannung in einer Entspannungsmaschine (Einblaseturbine) 18 zugeleitet, die mechanisch mit dem Nachverdichter 14 gekoppelt ist. Die entspannte Turbinenluft 19 wird schließlich direkt in die Niederdrucksäule 11 eingeblasen.The turbine air flow 6, 16 is in a post-compressor 14 with an after-cooler 15 post-compressed, cooled to an intermediate temperature in the main heat exchanger 7 and via line 17 of work relaxation in a relaxation machine (Blowing turbine) 18, which is mechanically coupled to the post-compressor 14 is. The relaxed turbine air 19 is finally fed directly into the low pressure column 11 blown.

Das Ausführungsbeispiel bezieht sich auf einen Anwendungsfall, in dem in begrenztem Umfang Luft bereits unter einem überatmosphärischen Druck zur Verfügung steht, beispielsweise dem Mitteldrucksäulendruck (plus Leitungsverluste). Ein solcher Luftstrom - beispielsweise aus einem gasturbinengetriebenen Verdichter oder aus anderer Quelle - strömt bei dem Ausführungsbeispiel als zweiter Einsatzluftstrom 20 dem warmen Ende des Hauptwärmetauschers zu, wird dort auf etwa Taupunkt abgekühlt und schließlich direkt der Mitteldrucksäule 10 zugeführt.The embodiment relates to an application in which limited Amount of air is already available under a superatmospheric pressure, for example, the medium pressure column pressure (plus line losses). Such a Air flow - for example from a gas turbine-driven compressor or from other source - flows in the exemplary embodiment as a second feed air stream 20 towards the warm end of the main heat exchanger there will be about dew point cooled and finally fed directly to the medium pressure column 10.

Sauerstoffangereicherte Flüssigkeit 22 wird vom Sumpf der Hochdrucksäule 9 abgezogen, in einem ersten Unterkühlungs-Gegenströmer 23 abgekühlt, über Leitung 24 und Drosselventil 25 in die Mitteldrucksäule eingeführt und dort zum ersten Teil einer weiteren Gegenstrom-Rektifikation unterworfen. Zu einem anderen Teil 26 wird er durch einen zweiten Unterkühlungs-Gegenströmer 27 weitergeleitet. Die unterkühlte sauerstoffangereicherte Flüssigkeit 28 unter Zwischendruck verzweigt in zwei Teile 29, 31, von denen einer über Ventil 30 in die Niederdrucksäule 11 eingedrosselt wird. Ein Teil 33 des gasförmigen Kopf-Stickstoffs der Hochdrucksäule 9 wird im Hauptwärmetauscher 7 auf etwa Umgebungstemperatur angewärmt und unter dem Druck der Hochdrucksäule als Produkt 34 (GAN) gewonnen.Oxygenated liquid 22 is discharged from the sump of the high pressure column 9 withdrawn, cooled in a first subcooling countercurrent 23, via line 24 and throttle valve 25 inserted into the medium pressure column and there for the first part subjected to a further countercurrent rectification. To another part 26 he becomes passed through a second supercooling counterflow 27. The hypothermic oxygen-enriched liquid 28 at intermediate pressure branches into two parts 29, 31, one of which is throttled via valve 30 into the low-pressure column 11. On Part 33 of the gaseous top nitrogen of the high pressure column 9 is in the Main heat exchanger 7 warmed to about ambient temperature and below that High pressure column pressure obtained as product 34 (GAN).

Im ersten Hauptkondensator 12 gewonnener Stickstoff wird zum Teil 35 unterkühlt (23) und als Rücklauf 36 auf den Kopf der Mitteldrucksäule 10 aufgegeben. Außerdem erzeugt der zweite Hauptkondensator 13 Rücklauf 37 für die Mitteldrucksäule, sowie bei Bedarf flüssiges Stickstoffprodukt 38.Some of the nitrogen obtained in the first main condenser 12 is subcooled 35 (23) and given as return 36 on the head of the medium pressure column 10. Moreover generates the second main condenser 13 return 37 for the medium pressure column, as well if necessary liquid nitrogen product 38.

Vom Sumpf der Mitteldrucksäule wird ein Sauerstoff mit einer Reinheit von etwa 99,5 mol-% flüssig abgezogen und in einen Nebenkondensator 40 eingeleitet. Dort wird er in indirektem Wärmeaustausch mit kondensierendem Kopf-Stickstoff 41 der Hochdrucksäule 9 teilweise verdampft. Ein erstes, etwas unreineres Sauerstoffprodukt 42, 43 wird aus dem dabei gebildeten Dampf unter etwa dem Mitteldrucksäulendruck gewonnen (GOX), gegebenenfalls nach Verdichtung in der zweiten Stufe 44 eines Sauerstoffverdichters 56/44 mit Nachkühlung 45. Aus dem im Nebenkondensator 40 flüssig verbliebenen Anteil 46 wird per Innenverdichtung ein reineres Hochdruck-Sauerstoffprodukt 49 (GOX-IC) erzeugt. Dazu wird die Flüssigkeit 46 mittels einer Pumpe 47 auf einen entsprechenden Druck gebracht, über eine Flüssigkeitsleitung 48 zum kalten Ende des Hauptwärmetauschers geführt und dort verdampft und angewärmt. Ein Teil 82 des gasförmigen Stickstoffs vom Kopf der Mitteldrucksäule wird im Hauptwärmetauscher 7 angewärmt und kann über Leitung 83 oder - wie dargestellt - über Leitung 86 nach Verdichtung in einem Stickstoff-Verdichter 84 mit Nachverdichter 85 als Druckprodukt (PGAN) gewonnen werden.An oxygen with a purity of about 99.5 is obtained from the bottom of the medium pressure column mol% withdrawn liquid and introduced into a secondary condenser 40. There he is in indirect heat exchange with condensing top nitrogen 41 the High pressure column 9 partially evaporated. A first, somewhat impure oxygen product 42, 43 becomes from the steam formed under approximately the medium pressure column pressure won (GOX), possibly after compression in the second stage 44 one Oxygen compressor 56/44 with after-cooling 45. From the in the secondary condenser 40 portion 46 remaining in liquid form becomes a purer high-pressure oxygen product by means of internal compression 49 (GOX-IC) generated. For this purpose, the liquid 46 by means of a Pump 47 brought to a corresponding pressure, via a liquid line 48 led to the cold end of the main heat exchanger and evaporated there and warmed up. A portion 82 of the gaseous nitrogen from the top of the medium pressure column becomes warmed in the main heat exchanger 7 and can via line 83 or - as shown - With line 86 after compression in a nitrogen compressor 84 with Post-compressor 85 can be obtained as a printed product (PGAN).

Rücklaufflüssigkeit 50, 51 für den Kopf der Niederdrucksäule 11 wird von einer Zwischenstelle der Mitteldrucksäule 10 oberhalb der Zuspeisung 24/25 der sauerstoffangereicherten Flüssigkeit abgenommen. Vom Kopf der Niederdrucksäule wird unreiner Stickstoff 52 als Restgas entnommen und nach Anwärmung 27 - 23 - 7 über Leitung 53 aus der Anlage entfernt (UN2). Das Sumpfprodukt 54 der Niederdrucksäule 11 wird teilweise gasförmig abgezogen, nach Anwärmung 27 - 23 - 7 über Leitung 55 der ersten Stufe 56 (mit Zwischenkühlung 57) des Sauerstoffverdichters 56/44 auf etwa Mitteldrucksäulendruck gebracht und schließlich mit dem Mitteldrucksäulen-Sauerstoff 43 vermischt. Außerdem kann flüssiger Sauerstoff 58 als Produkt oder zur Spülung aus dem Niederdrucksäulensumpf abgezogen werden.Return liquid 50, 51 for the head of the low pressure column 11 is from a Intermediate point of the medium pressure column 10 above the feed 24/25 oxygen-enriched liquid removed. From the head of the low pressure column impure nitrogen 52 is removed as residual gas and after heating 27-23-7 removed from the system via line 53 (UN2). The bottom product 54 of the Low-pressure column 11 is partially withdrawn in gaseous form, after heating 27-23-7 via line 55 of the first stage 56 (with intermediate cooling 57) of the Oxygen compressor 56/44 brought to about medium pressure column pressure and finally mixed with the medium pressure column oxygen 43. It can also be more fluid Oxygen 58 as a product or for flushing from the low pressure column sump subtracted from.

Ein erster argonangereicherter Strom 59 wird gasförmig von einer Zwischenstelle der Mitteldrucksäule 10 abgezogen, die unterhalb der Zuspeisung 24/25 sauerstoffangereicherter Flüssigkeit und unterhalb der Luftzuspeisung über Leitung 21 angeordnet ist. Der Strom 59 wird in einem Kondensator-Verdampfer 60 mindestens teilweise, vorzugsweise vollständig kondensiert und schließlich über Leitung 61 und Drosselventil 62 in eine Rohargonsäule 63 eingeleitet, die unter etwa demselben Druck wie die Niederdrucksäule 11 betrieben wird. Die Einspeisestelle des ersten argonangereicherten Stroms liegt beispielsweise 30 bis 40 theoretische Böden, vorzugsweise 33 bis 38 theoretische Böden oberhalb des Sumpfs bei einer Gesamtzahl von 70 bis 90 theoretische Böden, vorzugsweise 78 bis 85 theoretischen Böden in der Rohargonsäule 63. Der Kondensator-Verdampfer 60 stellt gleichzeitig der Sumpfaufkocher der Rohargonsäule 63 dar. Ein Teil 65 der nicht verdampften Sumpfflüssigkeit 64 der Rohargonsäule 63 wird in einer Pumpe 65 wieder auf Mitteldrucksäulendruck gebracht und in die Mitteldrucksäule 10 zurückgeführt (66). Der Rest 67 wird in die Niederdrucksäule 11 eingeleitet.A first argon-enriched stream 59 is gaseous from an intermediate point in the Subtracted medium pressure column 10, the 24/25 below the feed oxygen-enriched liquid and below the air supply via line 21 is arranged. The stream 59 is at least in a condenser-evaporator 60 partially, preferably completely condensed and finally via line 61 and Throttle valve 62 is introduced into a crude argon column 63, which is under approximately the same pressure how the low pressure column 11 is operated. The entry point of the first argon-enriched electricity is, for example, 30 to 40 theoretical plates, preferably 33 to 38 theoretical plates above the swamp at one Total number of 70 to 90 theoretical plates, preferably 78 to 85 theoretical plates Soils in the crude argon column 63. The condenser-evaporator 60 simultaneously represents the Bottom reboiler of the crude argon column 63. Part 65 of the non-evaporated Bottom liquid 64 of the crude argon column 63 is opened again in a pump 65 Brought medium pressure column pressure and returned to the medium pressure column 10 (66). The Rest 67 is introduced into the low pressure column 11.

Als weiterer Einsatz wird ein zweiter argonangereicherter Strom 68 in Gasform von der Niederdrucksäule 11 der Rohargonsäule direkt am Sumpf zugeführt.Another use is a second argon-enriched stream 68 in gaseous form from the Low pressure column 11 of the crude argon column fed directly to the sump.

Der Kopfkondensator 69 der Rohargonsäule 63 wird mit sauerstoffangereicherter Flüssigkeit 31 betrieben, die in einem Ventil auf einen geeigneten Druck (etwa gleich Niederdrucksäulendruck) entspannt wurde. Im Kopfkondensator 69 gebildeter Dampf 70 wird an geeigneter Stelle in die Niederdrucksäule eingeführt. Das Rohargonprodukt (die "argonreiche Fraktion") 75 wird gasförmig vom Kopf der Rohargonsäule 63 beziehungsweise aus dem Verflüssigungsraum des Kopfkondensators 69 abgezogen.The top condenser 69 of the crude argon column 63 is enriched with oxygen Liquid 31 operated in a valve to a suitable pressure (about the same Low pressure column pressure) was released. Vapor formed in the top condenser 69 70 is introduced into the low pressure column at a suitable point. The raw argon product (the "argon-rich fraction") 75 becomes gaseous from the top of the crude argon column 63 or withdrawn from the liquefaction space of the top condenser 69.

In Figur 2 wird der erste argonangereicherte Strom 259 im Hauptwärmetauscher 7 auf eine Zwischentemperatur angewärmt, über Leitung 271 zu einer Entspannungsmaschine 272 geleitet und dort arbeitsleistend auf etwa 0,2 bar über Rohargonsäulendruck entspannt und schließlich in den Verdampfungsraum des Kondensator-Verdampfers 60 geführt (274). Die Entspannungsmaschine 272 ist vorzugsweise als Turbine ausgebildet und mit einer Bremsvorrichtung 273 gekoppelt, vorzugsweise einem Generator.In FIG. 2 , the first argon-enriched stream 259 is warmed to an intermediate temperature in the main heat exchanger 7, passed to a relaxation machine 272 via line 271, where it is relieved of work to about 0.2 bar above crude argon column pressure and finally led into the evaporation space of the condenser-evaporator 60 (274 ). The expansion machine 272 is preferably designed as a turbine and coupled to a braking device 273, preferably a generator.

Figur 3 entspricht weit gehend Figur 2, allerdings wird hier auf einen Sumpfaufkocher für die Rohargonsäule 63 verzichtet und der arbeitsleistend entspannte erste argonangereicherte Strom 374 wird gasförmig in den Sumpf der Rohargonsäule eingeführt. FIG. 3 largely corresponds to FIG. 2, but here a sump reboiler for the crude argon column 63 is dispensed with and the first argon-enriched stream 374, which is relaxed during the work, is introduced in gaseous form into the sump of the crude argon column.

Bei dem Verfahren von Figur 4 wird auch auf die Argonübergangsturbine (272 in Figur 2) verzichtet und der erste argonangereicherte Strom 459 wird direkt in den Sumpf der Rohargonsäule 63 eingedrosselt (462).In the method of FIG. 4 , the argon transfer turbine (272 in FIG. 2) is also dispensed with and the first argon-enriched stream 459 is throttled directly into the bottom of the crude argon column 63 (462).

Die Figuren 5 bis 9 zeigen Alternativen zu der in Figur 1 dargestellten Einblasung von Turbinenluft 19 in die Niederdrucksäule. Diese abweichenden Methoden der Kälteerzeugung können auch mit jedem der Verfahren der Figuren 2 bis 4 kombiniert werden.FIGS. 5 to 9 show alternatives to the blowing in of FIG Turbine air 19 in the low pressure column. These different methods of Refrigeration can also be combined with any of the methods of Figures 2 to 4 become.

Die Luftturbine 518 entspannt in dem Verfahren der Figur 5 lediglich auf etwa den Betriebsdruck der Mitteldrucksäule 10. Diese Variante kommt also insbesondere bei relativ niedrigem Kältebedarf in Frage und erhöht die Sauerstoffausbeute des Prozesses. Die arbeitsleistend entspannte Luft 519 wird gemeinsam mit dem zweiten Einsatzluftstrom 20 - 21 über Leitung 521 in die Mitteldrucksäule 10 eingespeist.In the method of FIG. 5, the air turbine 518 only relaxes to approximately the operating pressure of the medium pressure column 10. This variant is therefore particularly suitable when the cooling requirement is relatively low and increases the oxygen yield of the process. The air 519 which has been relieved of work is fed into the medium-pressure column 10 together with the second feed air stream 20-21 via line 521.

Figur 6 betrifft eine Abwandlung von Figur 5, bei der die Turbinenluft 6 stromaufwärts des turbinengetriebenen Nachverdichters 14 in einem weiteren, mittels externer Energie angetriebenen Nachverdichter 681 mit Nachkühlung 682 verdichtet wird. Hierdurch lässt sich ein höheres Druckverhältnis an der Turbine 518 erreichen und damit mehr Kälte produzieren. FIG. 6 relates to a modification of FIG. 5, in which the turbine air 6 upstream of the turbine-driven post-compressor 14 is compressed in a further post-compressor 681 driven by external energy with post-cooling 682. As a result, a higher pressure ratio can be achieved on the turbine 518 and thus produce more cold.

Als Alternative zur bisher gezeigten arbeitsleistenden Entspannung von Einsatzluft kann Verfahrenskälte in einer Stickstoff-Turbine 718 gemäß Figur 7 gewonnen werden. Hierzu wird ein Teil 787 des aus der Hochdrucksäule 9 abgezogenen Stickstoffs 33 im Hauptwärmetauscher 7 nur auf eine Zwischentemperatur angewärmt und arbeitsleistend auf etwa Mitteldrucksäulendruck entspannt (718). Der entspannte Hochdrucksäulen-Stickstoff wird schließlich mit dem Mitteldrucksäulen-Stickstoff 82 stromaufwärts des Hauptwärmetauschers 7 vereinigt.As an alternative to the previously performed work-related relaxation of feed air, process cold can be obtained in a nitrogen turbine 718 according to FIG. 7 . For this purpose, part 787 of the nitrogen 33 drawn off from the high-pressure column 9 is only heated to an intermediate temperature in the main heat exchanger 7 and expanded to approximately medium-pressure column pressure in a work-performing manner (718). The expanded high-pressure column nitrogen is finally combined with the medium-pressure column nitrogen 82 upstream of the main heat exchanger 7.

Bei Figur 8 ist die Stickstoff-Turbine 718 nicht wie in Figur 7 an einen Generator oder an eine Ölbremse gekoppelt, sondern wird mittels eines Nachverdichters 814 gebremst, der den Druck im Turbinenstrom 887 und damit den Eintrittsdruck der Turbine 718 erhöht. Der entsprechende Teil 887 des Hochdrucksäulen-Stickstoffs wird vorher auf etwa Umgebungstemperatur angewärmt und stromabwärts es Nachverdichters 814 mittels eines Nachkühlers 815 abgekühlt. In FIG. 8 , the nitrogen turbine 718 is not coupled to a generator or to an oil brake as in FIG. 7, but is braked by means of a post-compressor 814, which increases the pressure in the turbine stream 887 and thus the inlet pressure of the turbine 718. The corresponding part 887 of the high-pressure column nitrogen is previously warmed to approximately ambient temperature and cooled downstream of the post-compressor 814 by means of an after-cooler 815.

Im Verfahren von Figur 9 wird ein Teil 988 des gasförmigen Stickstoffs 82 aus der Mitteldrucksäule 10 von einer Zwischentemperatur aus arbeitsleistend entspannt. Die Entspannungsmaschine wird beispielsweise durch eine Ölbremse oder einen Generator gebremst. Das entspannte Stickstoffgas 989 ist praktisch drucklos und wird unter Umgebungstemperatur über Leitung 990 abgezogen (GAN).In the process of FIG. 9, part 988 of the gaseous nitrogen 82 is made from the Medium pressure column 10 relaxed from an intermediate temperature from work. The Relaxation machine is, for example, by an oil brake or a Generator braked. The expanded nitrogen gas 989 is practically depressurized and will withdrawn below ambient temperature via line 990 (GAN).

Figur 10 basiert auf Figur 1, zeigt aber eine veränderte Führung des Sauerstoffprodukts aus der Niederdrucksäule 11. Hier wird das gesamte Sumpfprodukt der Niederdrucksäule flüssig entnommen (Leitung 1076). Derjenige Teil, der nicht über Leitung 1058 als flüssiges Sauerstoffprodukt beziehungsweise Spülflüssigkeit abgeführt wird, strömt über Leitung 1077 einer Pumpe 1078 zu und wird dort auf etwa Mitteldrucksäulendruck gebracht. Der gepumpte Niederdrucksäulen-Sauerstoff 1079 wird im ersten Unterkühlungs-Gegenströmer 27 angewärmt und schließlich über Leitung 1080 in die Mitteldrucksäule 10 eingeleitet. Leitung 39 fördert nun den gesamten gasförmig zu gewinnenden Sauerstoff, der in Mitteldrucksäule 10 und Niederdrucksäule 11 hergestellt wurde. Dieses "Zurückpumpen" des Niederdrucksäulen-Sauerstoffs in die Mitteldrucksäule kann in analoger Weise bei den Ausführungsbeispielen der Figuren 2 bis 9 und ihren Varianten angewendet werden. FIG. 10 is based on FIG. 1, but shows a changed routing of the oxygen product from the low-pressure column 11. Here, the entire bottom product is removed from the low-pressure column in liquid form (line 1076). The part that is not discharged via line 1058 as a liquid oxygen product or rinsing liquid flows through line 1077 to a pump 1078 and is brought to approximately medium-pressure column pressure there. The pumped low-pressure column oxygen 1079 is warmed in the first supercooling countercurrent 27 and finally introduced into the medium-pressure column 10 via line 1080. Line 39 now conveys all of the oxygen to be obtained in gaseous form, which was produced in medium pressure column 10 and low pressure column 11. This "pumping back" of the low-pressure column oxygen into the medium-pressure column can be applied in an analogous manner to the exemplary embodiments in FIGS. 2 to 9 and their variants.

Die Ausführungsbeispiele zeigen ein Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung, das als Dreifachsäule im engeren Sinne ausgeführt ist, das heißt Hochdrucksäule, Mitteldrucksäule und Niederdrucksäule sind übereinander angeordnet und stehen paarweise über je einen Hauptkondensator 12, 13 in wärmetauschender Verbindung. Die Erfindung ist aber auch bei jedem anderen 3-Säulen-System anwendbar. Beispielsweise kann die Mitteldrucksäule neben einer klassischen Linde-Doppelsäule angeordnet sein, die Hochdrucksäule und Niederdrucksäule umfasst; alternativ könnten alle drei Säulen nebeneinander angeordnet sein. Auch andere Kondensator-Konfigurationen für die Niederdrucksäule, die Mitteldrucksäule und für die Hochdrucksäule können im Rahmen der Erfindung eingesetzt werden.The exemplary embodiments show a rectification system for nitrogen-oxygen separation, which is designed as a triple column in the narrower sense, that is High pressure column, medium pressure column and low pressure column are arranged one above the other and are in pairs over a main condenser 12, 13 in heat exchangers Connection. However, the invention is also applicable to any other 3-pillar system applicable. For example, the medium pressure column next to a classic Linde double column be arranged, which comprises high pressure column and low pressure column; alternatively, all three pillars could be arranged side by side. Others too Condenser configurations for the low pressure column, the medium pressure column and for the High pressure columns can be used in the context of the invention.

Einige für die Erfindung nebensächliche Einzelheiten wie zum Beispiel die Reinigung der Einsatzluftströme ist in den Zeichnungen nicht dargestellt.Some details irrelevant to the invention, such as cleaning the input air flows are not shown in the drawings.

Claims (7)

Verfahren zur Tieftemperatur-Luftzerlegung von Luft in einem Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung, das eine Hochdrucksäule (9), eine Niederdrucksäule (11) und eine Mitteldrucksäule (10) aufweist, und in einer Rohargonsäule (63), wobei bei dem Verfahren (a)mindestens ein Einsatzluftstrom in das Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung eingeleitet (8, 19, 21, 521) wird, (b)der Niederdrucksäule (11) mindestens ein Sauerstoff- oder Stickstoff-Produktstrom (52, 54, 58, 1076) entnommen wird, (c) mindestens ein erster argonangereicherter Strom (59, 61, 259, 271, 274, 276, 374) aus dem Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung entnommen und der Rohargonsäule (63) zugeleitet wird und bei dem (d)der Rohargonsäule (63) eine argonreiche Fraktion 75 entnommen wird, deren Argongehalt größer als derjenige des ersten argonangereicherten Stroms (59, 61, 259, 271, 274, 276, 374) ist, dadurch gekennzeichnet, dass (e)der erste argonangereicherte Strom (59, 61, 259, 271, 274, 276, 374) aus der Mitteldrucksäule (10) entnommen wird. A method for low-temperature air separation of air in a rectification system for nitrogen-oxygen separation, which has a high-pressure column (9), a low-pressure column (11) and a medium-pressure column (10), and in a crude argon column (63), the method (a) at least one feed air stream is introduced (8, 19, 21, 521) into the rectification system for nitrogen-oxygen separation, (b) at least one oxygen or nitrogen product stream (52, 54, 58, 1076) is withdrawn from the low-pressure column (11), (c) at least one first argon-enriched stream (59, 61, 259, 271, 274, 276, 374) is removed from the rectification system for nitrogen-oxygen separation and fed to the crude argon column (63) and in which (d) an argon-rich fraction 75 is removed from the crude argon column (63), the argon content of which is greater than that of the first argon-enriched stream (59, 61, 259, 271, 274, 276, 374), characterized in that (e) the first argon-enriched stream (59, 61, 259, 271, 274, 276, 374) is withdrawn from the medium pressure column (10). Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass ein zweiter argonangereicherter Strom (68) aus der Niederdrucksäule abgezogen und in die Rohargonsäule (63) eingeleitet wird.A method according to claim 1, characterized in that a second argon-enriched stream (68) is withdrawn from the low pressure column and introduced into the crude argon column (63). Verfahren nach Anspruch 1 oder 5, dadurch gekennzeichnet, dass die Sumpfflüssigkeit (64) der Rohargonsäule (63) mindestens teilweise in die Mitteldrucksäule (10) zurückgeführt (65, 66) wird.Method according to claim 1 or 5, characterized in that the bottom liquid (64) of the crude argon column (63) is at least partially returned (65, 66) to the medium pressure column (10). Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass mindestens ein Teil des ersten argonangereicherten Stroms (59, 274) stromaufwärts der Einleitung (61, 276) in die Rohargonsäule (63) in einem Kondensator-Verdampfer (60) mindestens teilweise kondensiert wird. Method according to one of claims 1 to 3, characterized in that at least part of the first argon-enriched stream (59, 274) upstream of the introduction (61, 276) into the crude argon column (63) condenses at least partially in a condenser-evaporator (60) becomes. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass in dem Kondensator-Verdampfer (60) ein Teil einer Flüssigkeit, insbesondere der Sumpfflüssigkeit, aus der Rohargonsäule (63) verdampft wird.A method according to claim 4, characterized in that in the condenser-evaporator (60) a part of a liquid, in particular the bottom liquid, is evaporated from the crude argon column (63). Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass mindestens ein Teil des ersten argonangereicherten Stroms (259, 271) stromaufwärts der Einleitung (276, 374) in die Rohargonsäule (63) arbeitsleistend entspannt (272) wird.Method according to one of claims 1 to 5, characterized in that at least a portion of the first argon-enriched stream (259, 271) upstream of the introduction (276, 374) into the crude argon column (63) is expanded to perform work (272). Vorrichtung zur Tieftemperatur-Luftzerlegung von Luft mit einem Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung, das eine Hochdrucksäule (9), eine Niederdrucksäule (11) und eine Mitteldrucksäule (10) aufweist, mit einer Rohargonsäule (63) und mit (a)mindestens einer Einsatzluftleitung (8, 19, 21, 521) zum Einleiten mindestens eines Einsatzluftstroms in das Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung wird, (b)mindestens einer Produktleitung (52, 54, 58, 1076) zum Entnehmen mindestens eines Sauerstoff- oder Stickstoff-Produktstroms aus der Niederdrucksäule (11), (c) einer ersten Argonübergangs-Leitung (59, 61, 259, 271, 274, 276, 374) zur Einleitung eines argonangereicherten Stroms aus dem Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung in die Rohargonsäule (63) und mit (d)einer Rohargon-Produktleitung (75) zum Entnehmen einer argonreichen Fraktion, deren Argongehalt größer als derjenige des ersten argonangereicherten Stroms ist, aus der Rohargonsäule (63), dadurch gekennzeichnet, dass (e)die erste Argonübergangs-Leitung (59, 61, 259, 271, 274, 276, 374) mit der Mitteldrucksäule (10) verbunden ist. Device for low-temperature air separation of air with a rectification system for nitrogen-oxygen separation, which has a high-pressure column (9), a low-pressure column (11) and a medium-pressure column (10), with a crude argon column (63) and with (a) at least one feed air line (8, 19, 21, 521) for introducing at least one feed air stream into the rectification system for nitrogen-oxygen separation, (b) at least one product line (52, 54, 58, 1076) for removing at least one oxygen or nitrogen product stream from the low-pressure column (11), (c) a first argon transfer line (59, 61, 259, 271, 274, 276, 374) for introducing an argon-enriched stream from the rectification system for nitrogen-oxygen separation into the crude argon column (63) and with (d) a crude argon product line (75) for withdrawing an argon-rich fraction, the argon content of which is greater than that of the first argon-enriched stream, from the crude argon column (63), characterized in that (e) the first argon transfer line (59, 61, 259, 271, 274, 276, 374) is connected to the medium pressure column (10).
EP02011458A 2002-04-17 2002-05-24 Cryogenic triple column air separation system with argon recovery Expired - Lifetime EP1357342B1 (en)

Applications Claiming Priority (2)

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DE102007031765A1 (en) 2007-07-07 2009-01-08 Linde Ag Process for the cryogenic separation of air
DE102007031759A1 (en) 2007-07-07 2009-01-08 Linde Ag Method and apparatus for producing gaseous pressure product by cryogenic separation of air
DE102009034979A1 (en) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Method for producing pressurized oxygen by evaporating liquid oxygen using a copper and nickel heat exchanger block
EP2312248A1 (en) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Method and device for obtaining pressurised oxygen and krypton/xenon
EP2458311A1 (en) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Method and device for creating a gaseous, pressurised product by the cryogenic decomposition of air
DE102010052544A1 (en) 2010-11-25 2012-05-31 Linde Ag Process for obtaining a gaseous product by cryogenic separation of air
EP2520886A1 (en) 2011-05-05 2012-11-07 Linde AG Method and device for creating gaseous oxygen pressurised product by the cryogenic decomposition of air
EP2568242A1 (en) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Method and device for generating of steel
EP2600090A1 (en) 2011-12-01 2013-06-05 Linde Aktiengesellschaft Method and device for generating pressurised oxygen by cryogenic decomposition of air
DE102011121314A1 (en) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Method for producing gaseous oxygen product in main heat exchanger system in distillation column system, involves providing turbines, where one of turbines drives compressor, and other turbine drives generator
US20130340476A1 (en) * 2011-03-18 2013-12-26 L'air Liquide Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Apparatus and method for separating air by cryogenic distillation
DE102013017590A1 (en) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Method for recovering methane-poor fluids in liquid air separation system to manufacture air product, involves vaporizing oxygen, krypton and xenon containing sump liquid in low pressure column by using multi-storey bath vaporizer
DE102012017488A1 (en) 2012-09-04 2014-03-06 Linde Aktiengesellschaft Method for building air separation plant, involves selecting air separation modules on basis of product specification of module set with different air pressure requirements
EP2784420A1 (en) 2013-03-26 2014-10-01 Linde Aktiengesellschaft Method for air separation and air separation plant
WO2014154339A2 (en) 2013-03-26 2014-10-02 Linde Aktiengesellschaft Method for air separation and air separation plant
EP2801777A1 (en) 2013-05-08 2014-11-12 Linde Aktiengesellschaft Air separation plant with main compressor drive
EP2963367A1 (en) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Method and device for cryogenic air separation with variable power consumption
EP2963371A1 (en) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Method and device for creating a pressurised gas product by the cryogenic decomposition of air
EP2963369A1 (en) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Method and device for the cryogenic decomposition of air
EP2963370A1 (en) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Method and device for the cryogenic decomposition of air
CN105637311A (en) * 2013-10-15 2016-06-01 乔治洛德方法研究和开发液化空气有限公司 Method and device for separating air by cryogenic distillation
WO2018114052A2 (en) 2016-12-23 2018-06-28 Linde Aktiengesellschaft Cryogenic air separation method, and air separation plant
US10852061B2 (en) 2017-05-16 2020-12-01 Terrence J. Ebert Apparatus and process for liquefying gases
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DE102007031765A1 (en) 2007-07-07 2009-01-08 Linde Ag Process for the cryogenic separation of air
DE102007031759A1 (en) 2007-07-07 2009-01-08 Linde Ag Method and apparatus for producing gaseous pressure product by cryogenic separation of air
EP2015012A2 (en) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Process for the cryogenic separation of air
EP2015013A2 (en) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Process and device for producing a gaseous pressurised product by cryogenic separation of air
DE102009034979A1 (en) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Method for producing pressurized oxygen by evaporating liquid oxygen using a copper and nickel heat exchanger block
EP2312248A1 (en) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Method and device for obtaining pressurised oxygen and krypton/xenon
EP2458311A1 (en) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Method and device for creating a gaseous, pressurised product by the cryogenic decomposition of air
DE102010052545A1 (en) 2010-11-25 2012-05-31 Linde Aktiengesellschaft Method and apparatus for recovering a gaseous product by cryogenic separation of air
DE102010052544A1 (en) 2010-11-25 2012-05-31 Linde Ag Process for obtaining a gaseous product by cryogenic separation of air
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US20130340476A1 (en) * 2011-03-18 2013-12-26 L'air Liquide Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Apparatus and method for separating air by cryogenic distillation
EP2520886A1 (en) 2011-05-05 2012-11-07 Linde AG Method and device for creating gaseous oxygen pressurised product by the cryogenic decomposition of air
EP2568242A1 (en) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Method and device for generating of steel
DE102011112909A1 (en) 2011-09-08 2013-03-14 Linde Aktiengesellschaft Process and apparatus for recovering steel
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DE102011121314A1 (en) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Method for producing gaseous oxygen product in main heat exchanger system in distillation column system, involves providing turbines, where one of turbines drives compressor, and other turbine drives generator
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CN105637311A (en) * 2013-10-15 2016-06-01 乔治洛德方法研究和开发液化空气有限公司 Method and device for separating air by cryogenic distillation
CN105637311B (en) * 2013-10-15 2018-06-29 乔治洛德方法研究和开发液化空气有限公司 Pass through the method and apparatus of separating air by cryogenic distillation
DE102013017590A1 (en) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Method for recovering methane-poor fluids in liquid air separation system to manufacture air product, involves vaporizing oxygen, krypton and xenon containing sump liquid in low pressure column by using multi-storey bath vaporizer
EP2963369A1 (en) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Method and device for the cryogenic decomposition of air
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WO2018114052A2 (en) 2016-12-23 2018-06-28 Linde Aktiengesellschaft Cryogenic air separation method, and air separation plant
WO2018114052A3 (en) * 2016-12-23 2018-10-11 Linde Aktiengesellschaft Cryogenic air separation method, and air separation plant
US10852061B2 (en) 2017-05-16 2020-12-01 Terrence J. Ebert Apparatus and process for liquefying gases
EP3913310A1 (en) 2020-05-20 2021-11-24 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and device for air separation by cryogenic distilling
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ATE344428T1 (en) 2006-11-15

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