EP3290843A2 - Procédé et dispositif destiné à fabriquer de l'azote pressurisé et liquide par décomposition à basse température de l'air - Google Patents

Procédé et dispositif destiné à fabriquer de l'azote pressurisé et liquide par décomposition à basse température de l'air Download PDF

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Publication number
EP3290843A2
EP3290843A2 EP17020268.3A EP17020268A EP3290843A2 EP 3290843 A2 EP3290843 A2 EP 3290843A2 EP 17020268 A EP17020268 A EP 17020268A EP 3290843 A2 EP3290843 A2 EP 3290843A2
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Prior art keywords
nitrogen
pressure column
pressure
stream
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.)
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EP17020268.3A
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German (de)
English (en)
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EP3290843A3 (fr
Inventor
Dimitri GOLUBEV
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Linde GmbH
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Linde GmbH
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Publication date
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Publication of EP3290843A3 publication Critical patent/EP3290843A3/fr
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04436—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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/04024—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of purified feed air, so-called boosted air
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/0403—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of nitrogen
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    • 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
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04—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
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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
    • F25J3/04321—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 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
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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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.
    • F25J3/04381—Details relating to the work expansion, e.g. process parameter etc. using work extraction by mechanical coupling of compression and expansion so-called companders
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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    • F25J3/04375—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
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94—Details relating to the withdrawal point
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/40—Air or oxygen enriched air, i.e. generally less than 30mol% of 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/04—Recovery of liquid products
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • 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
    • F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop

Definitions

  • the invention relates to a process for the production of pressurized nitrogen and liquid nitrogen by cryogenic separation of air according to the preamble of patent claim 1.
  • the production of air products in the liquid or gaseous state by cryogenic separation of air in air separation plants is known.
  • Such air separation plants have distillation column systems which can be designed, for example, as two-column systems, in particular as classic Linde double-column systems, but also as three-column or multi-column systems.
  • devices for obtaining further air components in particular the noble gases krypton, xenon and / or argon, may be provided (cf., for example FG Kerry, Industrial Gas Handbook: Gas Separation and Purification, Boca Raton: CRC Press, 2006; Chapter 3: Air Separation Technology ).
  • the distillation column system of the invention may be designed as a classical double column system, but also as a three or more column system.
  • there may be other means for obtaining other air components for example, to obtain impure, pure or high purity oxygen or noble gases.
  • a “main heat exchanger” serves to cool feed air in indirect heat exchange with recycle streams from the distillation column system. It may be formed from a single or a plurality of parallel and / or serially connected and functionally connected heat exchanger sections, for example one or more plate heat exchanger blocks.
  • condenser-evaporator refers to a heat exchanger in which a first condensing fluid stream undergoes indirect heat exchange with a second evaporating fluid stream.
  • Each condenser-evaporator has a liquefaction space and an evaporation space, which consist of liquefaction passages or evaporation passages.
  • Liquefaction space the condensation (liquefaction) of the first fluid flow is performed, in the evaporation space, the evaporation of the second fluid stream.
  • Evaporation and liquefaction space are formed by groups of passages that are in heat exchange relationship with each other.
  • the evaporation space of a condenser-evaporator can be designed as a bath evaporator, falling-film evaporator or forced-flow evaporator.
  • a “relaxation machine” can have any design. Turbines (turboexpanders) are preferably used here.
  • the invention has for its object to provide a method of the type mentioned above and a corresponding device for a relatively high liquid production of 6 to 10 mol% of the nitrogen product amount or more with a relatively high nitrogen product yield in the process of approx. 60% are suitable and moreover efficient to operate. (The nitrogen yield depends on other parameters, for example product purity.)
  • a second pressure nitrogen stream is withdrawn from the top of the high pressure column and expanded in a second expansion machine to a pressure that still allows the withdrawal of this stream as a printed product, preferably at about the pressure of the first pressure nitrogen stream from the head of the low pressure column.
  • a part of the liquefied in the low-pressure column overhead condenser nitrogen withdrawn as liquid nitrogen product.
  • the second turbine with a different inlet temperature from the first turbine also improves the temperature profile in the main heat exchanger (lower thermodynamic losses due to lower temperature differences).
  • the process according to the invention can be operated particularly favorably if the first pressure nitrogen stream is withdrawn from the top of the low-pressure column under a pressure of 8.0 to 9.0 bar, in particular 8.4 to 9.0 bar.
  • the second pressure nitrogen stream is expanded in the expansion machine to about the pressure of the first pressure nitrogen stream; Subsequently, the two pressure nitrogen streams are combined and withdrawn as a common pressure nitrogen product stream.
  • the merge is most easily done within the main heat exchanger; In principle, however, it can also be carried out in the warm, ie downstream of the main heat exchanger.
  • the two inlet temperatures of the expansion machines are preferably different, in particular the second intermediate temperature is at least 10 K higher than the first intermediate temperature.
  • the temperature difference is 90 to 30 K, preferably 70 to 50 K.
  • both expansion machines are coupled to a generator or a dissipative brake.
  • generator turbines are used. Although no energy is returned directly to the process here.
  • This variant is particularly flexible with regard to different load cases.
  • the two expansion machines each drive a compressor stage, and a process stream is compressed successively in the two compressor stages.
  • only one of the two turbines for example the pressurized nitrogen turbine (“second expansion machine"), may be coupled to a compressor stage and the other one (eg the residual gas turbine (“first expansion machine”) to a generator.
  • the two condenser-evaporator can be designed as a classic bath evaporator.
  • low-pressure column top condenser is designed on its evaporation side as a forced-flow evaporator. This results in no hydrostatic pressure loss on the evaporation side and also a comparatively low pressure on the liquefaction side.
  • the main condenser is formed on its evaporation side as a forced-flow evaporator. This results in comparison with a bath evaporator, a lower hydrostatic pressure loss on the evaporation side and also a comparatively low pressure on the liquefaction side.
  • the liquefied nitrogen in the first mode of operation, at least a portion of the liquefied nitrogen is vaporized under pressure and subsequently recovered as a pressurized nitrogen product.
  • the corresponding evaporation device is operated with external heat, that is, the heat source is in particular no process stream of the cryogenic separation.
  • no liquefied nitrogen or only a lesser amount than in the first mode of operation eg, less than 50%
  • the evaporation device has, in particular, an air-heated evaporator, a water bath evaporator and / or a solid-state cold storage.
  • the invention also relates to a device for generating pressurized nitrogen and liquid nitrogen by cryogenic separation of air according to claim 14.
  • the device according to the invention can be supplemented by device features which correspond to the characteristics of individual, several or all dependent method claims.
  • FIG. 1 is the total feed air (AIR) via a filter 1 of a main air compressor 2 with aftercooling 3 (and unillustrated intermediate cooling) on compressed a pressure of about 14.6 bar.
  • the subsequent pre-cooling system has a direct contact cooler 4.
  • the pre-cooled feed air 5 is fed to a cleaning device 6, preferably a switchable molecular sieve adsorber.
  • the entire purified feed air flows to the main heat exchanger 8. It is cooled down to the cold end.
  • the cold, completely or almost completely gaseous air 8 is introduced into the high-pressure column 9.
  • the high-pressure column 9 is part of a distillation column system, which also has a low-pressure column 10, a main condenser 11 and a low-pressure column top condenser 12.
  • the two condenser-evaporators 11, 12 are formed on the evaporation side as a forced-flow evaporator.
  • Liquid raw oxygen 13 from the bottom of the high pressure column 9 is cooled in a subcooling countercurrent 14 and fed via line 15 of the low pressure column 10 at an intermediate point.
  • the gaseous nitrogen head 16 of the high pressure column 9 is withdrawn to a first part 17 as the first pressure nitrogen stream and fed to the main heat exchanger 8.
  • a second part 20 of the gaseous top nitrogen 16 is at least partially liquefied in the liquefaction space of the main condenser 11.
  • the liquid nitrogen 21 produced in the process is used to a first part as reflux in the high-pressure column 9.
  • the remainder 22/23 is cooled in the subcooling countercurrent 14 and fed to the top of the low pressure column 10.
  • a liquid oxygen-rich fraction 24 from the bottom of the low-pressure column or from the evaporation space of the main condenser 11 is cooled in the subcooling countercurrent 14 and introduced via line 25 as a coolant flow in the evaporation chamber of the low-pressure column top condenser 12 and there at least partially evaporated.
  • the vapor generated in the evaporation chamber of the low-pressure column top condenser 12 is withdrawn as residual gas stream 26 and heated in the main heat exchanger 8 to a first intermediate temperature of, for example, 142 K.
  • the residual gas stream 27 is introduced at the first intermediate temperature in a first expansion machine 28, which is designed here as a generator turbine, where it works to just above Atmospheric pressure relaxes.
  • the work-performing relaxed residual gas stream 29 is in the main heat exchanger 8 completely, that is heated to approximately ambient temperature.
  • the warm residual gas 30 can be discharged via line 31 directly into the atmosphere (ATM). Alternatively or in part, it can be used as regeneration gas in the purification device 6 via line 32, optionally after heating in a regeneration gas heater 33. Used regeneration gas is discharged via line 34 into the atmosphere.
  • a first portion 44 of the gaseous overhead nitrogen of the low-pressure column 10 is taken as the first pressure nitrogen stream, warmed in the main heat exchanger 8 and withdrawn as the first pressure nitrogen product (PGAN) 18, 19.
  • a second part 45 of the gaseous nitrogen head of the low-pressure column 10 is in the liquefaction space low-pressure column top condenser 12th at least partially liquefied.
  • a portion 47 of the nitrogen 46 liquefied in the low-pressure column top condenser 12 is withdrawn as liquid nitrogen product (PLIN).
  • the second pressure nitrogen stream 17 from the high-pressure column 9 is heated in the main heat exchanger 8 to a second intermediate temperature of 207 K.
  • the second pressure nitrogen stream 40 is introduced under the second intermediate temperature in a second expansion machine 41 and there relaxes work to about the operating pressure at the top of the low-pressure column 10.
  • the second expansion machine 41 is also designed here as a generator turbine.
  • the working expanded second pressure nitrogen stream 42 is completely warmed in the main heat exchanger.
  • the warm second pressurized nitrogen stream 43 is combined with the warm first pressurized nitrogen stream 18 and withdrawn via line 19 together with the first pressurized nitrogen product as the second pressurized nitrogen product (PGAN).
  • FIG. 1 The procedures of the two Figures 2 and 3 differ from it by FIG. 1 in that they use the work done on the turbines to compress a process stream.
  • This is accomplished by two compressor stages (booster) 70, 72, which are coupled to the turbines 28 and 41 and connected to one another in series, and each having an aftercooler 71, 73.
  • boost 70, 72 can compressors and Instead of the illustrated configuration, turbines can also be connected in reverse, that is to say the first expansion machine 41 with the first compressor stage 70 and the second expansion machine 41 with the second compressor stage 72.
  • a portion 50 of the second pressurized nitrogen stream 17 may be passed from the high pressure column 9 to the warm end of the main heat exchanger 8 and discharged as a high pressure product HPGAN at a pressure of 13 to 14 bar (not shown).
  • part of the compression of the total air 7A, 7B is taken over by these turbine-driven compressor stages 70, 72.
  • the main air compressor for example, only has to compress this to 12.5 bar. Accordingly, a stage can be saved on the main air compressor.
  • FIG. 4 is identical to FIG. 1 with the exception of an additional subcooling countercurrent 414, in which the liquid nitrogen 47 withdrawn from the low pressure column 10 is subcooled against an evaporating nitrogen stream 415/416.
  • a small portion of the supercooled liquid nitrogen is branched off via a valve 417.
  • the vaporized nitrogen 416 is added to the exhaust 29 of the residual gas turbine 28 and heated together with this in the main heat exchanger 8.
  • FIG. 5 contains in addition to FIG. 1 a pure oxygen column 550, in whose sump highly pure liquid oxygen is produced, which is withdrawn via line 551 and recovered as a high-purity liquid oxygen product HLOX. Via line 552, an oxygen fraction is withdrawn from the low-pressure column 10, which is free of less volatile constituents. It is undercooled in the bottom evaporator 553 of the pure oxygen column 550 and fed via line 554 and throttle valve 555 to the top of the pure oxygen column 550. There, the more volatile components are separated. The sump evaporator 553 is also from a part 556 of heated gaseous nitrogen head 16 of the high pressure column 9; Resulting liquid nitrogen 557 is applied to the low-pressure column 10. The impure gaseous oxygen 558 from the top of the pure oxygen column 550 is mixed with the residual gas 26 upstream of the residual gas turbine 28.
  • the air at the entrance to the high pressure column is already pre-liquefied (for example to about 1% or more).
  • the existing because of this Vorverminuteung liquid is deposited in the sump and can be discarded together with the rinsing liquid. As a result, the efficiency of the process is significantly reduced, as it is lost a lot of cold and nitrogen molecules.
  • the high pressure column has one to five practical trays as barrier bottoms 663.
  • the crude liquid oxygen 13 is withdrawn above the barrier bottoms, the high pressure column flushing liquid 661 below, namely directly from the sump; it contains both the return liquid from the high-pressure column or from the barrier floors, as well as the introduced via line 8 pre-liquefied air.
  • the stream 661 is fed to the top of the additional column 660 (possibly after subcooling), accumulates in the mass transfer within the column to gravitational and finally - withdrawn in much lesser amount from the bottom of the additional column 660 via line 662.
  • the deducted amount is for example, about 40 to 50 Nm 3 / h; Relatively, at 100,000 Nm 3 / h of total air quantity, the ratio of amounts of electricity 662 to 661 is for example between 1 and 10%.
  • the sump evaporator 664 of the additional column 660 is heated with gaseous air 665 from the high-pressure column 9.
  • the condensed in the bottom evaporator 664 666 air is supplied to the low pressure column 10.
  • the head gas 667 formed in the additional column 660 is likewise supplied to the low-pressure column 10 at a suitable point.
  • the C 3 H 8 from the partial air flow 665 to the condenser of the additional column 660 is retained in the system.
  • this amount of air is relatively small compared to the amount of feed air (about 1%), so that the reliability is not affected.
  • the flushing 662 being removed from the additional column 660, the return flow rate to the blocking section 663 in the high-pressure column can be increased.
  • more xenon is washed out and the actual purging 662 from the additional column can also be used and processed as a xenon concentrate;
  • the xenon yield can in a method according to FIG. 6 over 50%.
  • the high pressure column purge fluid 661 in the subcooler countercurrent 14 may be subcooled.
  • the liquid stream 666 from the sump evaporator 664 may be subcooled in the subcooling countercurrent 14 before being introduced into the low pressure column 10.
  • FIG. 7 is different from this FIG. 6 in that the purge stream 662 is not discarded in the liquid state. Rather, it is introduced via line 762 into the hot residual gas line 763, evaporates there abruptly and is then blown very dilute into the atmosphere.
  • the method described so far has only limited flexibility in operating cases with relatively low liquid production (ie deviating from the design case).
  • the pressure in the evaporation space of the upper condenser and thus also the inlet pressure of the residual gas turbine and the suction pressure in a downstream downstream compressor fall; for example, this refers to the use of blending natural gas to adjust the calorific value.
  • a significantly reduced intake pressure in the supercharger is heavily involved in the dimensioning of the machine and also means a limitation of the usual underload behavior.
  • FIG. 8 A relatively inexpensive and yet relatively efficient way out of this situation is with the in FIG. 8 shown interconnection possible.
  • a first mode of operation with reduced liquid delivery the liquid production in the plant is not significantly reduced, but a part of the applied separation or liquefaction energy is recovered from the liquid.
  • This can be realized either by the use of an air- or steam-heated emergency supply evaporator or by incorporating one or more cold storage. In the latter case, the cold of the liquefaction process is also partially stored - for example, to increase the liquid production in other operating cases.
  • an air partial flow can also be liquefied.
  • a second mode less or no liquid product is vaporized.
  • the additional process steps that are used in the first mode of operation are shut down.
  • FIG. 8 a portion 830 of the relaxed stream in the residual gas turbine 28 is warmed separately before being vented to the atmosphere (ATM).
  • the nitrogen product 44, 18 from the low pressure column 10 is further densified by two two-stage (820, 821) nitrogen product compressors before being discharged via line 819 as a pressurized product.
  • the product compressor 820, 821 as a whole thus has four stages. (Alternatively, one or three nitrogen product compressors with one, three, or more stages may be used.)
  • the compressed stream may be either fully pressurized to final pressure; alternatively, a part between the two nitrogen product compressors 820 and 821 are taken on an intermediate pressure (not shown).
  • liquid nitrogen 871 is pressurized by a pump 872 (eg, approximately the pressure between the two nitrogen product compressors 820, 821); alternatively, the pump delivers to the pressure before the first nitrogen product compressor 820 or to the pressure behind the second nitrogen product compressor 821 (not shown).
  • the high pressure nitrogen is vaporized in an atmospheric evaporator 873; Alternatively, a steam-heated water bath evaporator can be used.
  • the gaseous high pressure nitrogen is mixed via one of the lines 875a, 875b, 875c with the hot gaseous nitrogen 18 from the low pressure column 10.
  • the atmospheric evaporator 873 is shut down and all liquid production PLIN is delivered as an end product or stored in the liquid nitrogen tank 870.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP17020268.3A 2016-07-12 2017-06-23 Procédé et dispositif destiné à fabriquer de l'azote pressurisé et liquide par décomposition à basse température de l'air Withdrawn EP3290843A3 (fr)

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EP3757493A1 (fr) 2019-06-25 2020-12-30 Linde GmbH Procédé et installation d'obtention d'un produit dérivé de l'air riche en azote et riche en oxygène au moyen d'un fractionnement à basse température de l'air
WO2021190784A1 (fr) * 2020-03-23 2021-09-30 Linde Gmbh Procédé et installation de séparation d'air à basse température
EP4450910A1 (fr) * 2023-04-18 2024-10-23 Linde GmbH Procédé de séparation d'air à basse température et installation de séparation d'air
WO2024217721A1 (fr) * 2023-04-18 2024-10-24 Linde Gmbh Procédé de fractionnement cryogénique d'air et installation de fractionnement d'air
EP4567360A3 (fr) * 2023-12-06 2025-09-17 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé de production d'oxygène de haute pureté, et dispositif de séparation d'air pour la production d'oxygène de haute pureté

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EP3757493A1 (fr) 2019-06-25 2020-12-30 Linde GmbH Procédé et installation d'obtention d'un produit dérivé de l'air riche en azote et riche en oxygène au moyen d'un fractionnement à basse température de l'air
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CN115151771A (zh) * 2020-03-23 2022-10-04 林德有限责任公司 用于低温分离空气的方法和设备
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EP4450910A1 (fr) * 2023-04-18 2024-10-23 Linde GmbH Procédé de séparation d'air à basse température et installation de séparation d'air
WO2024217721A1 (fr) * 2023-04-18 2024-10-24 Linde Gmbh Procédé de fractionnement cryogénique d'air et installation de fractionnement d'air
EP4567360A3 (fr) * 2023-12-06 2025-09-17 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé de production d'oxygène de haute pureté, et dispositif de séparation d'air pour la production d'oxygène de haute pureté

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TWI737770B (zh) 2021-09-01
US10488106B2 (en) 2019-11-26
CN107606875A (zh) 2018-01-19
EP3290843A3 (fr) 2018-06-13
TW201809563A (zh) 2018-03-16

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