EP2712419A2 - Verfahren zur trennung von luft durch kryogene destillation - Google Patents

Verfahren zur trennung von luft durch kryogene destillation

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Publication number
EP2712419A2
EP2712419A2 EP12714821.1A EP12714821A EP2712419A2 EP 2712419 A2 EP2712419 A2 EP 2712419A2 EP 12714821 A EP12714821 A EP 12714821A EP 2712419 A2 EP2712419 A2 EP 2712419A2
Authority
EP
European Patent Office
Prior art keywords
air
during
sent
adsorber
phase
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
EP12714821.1A
Other languages
English (en)
French (fr)
Other versions
EP2712419B1 (de
Inventor
Patrick Le Bot
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP2712419A2 publication Critical patent/EP2712419A2/de
Application granted granted Critical
Publication of EP2712419B1 publication Critical patent/EP2712419B1/de
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/04054—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
    • F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
    • F25J3/04175—Hot end purification of the feed air by adsorption of the impurities at a pressure of substantially more than the highest pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163—Hot end purification of the feed air
    • F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
    • F25J3/04181—Regenerating the adsorbents
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—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
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04472—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages
    • F25J3/04478—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 the cold from cryogenic liquids produced within the air fractionation unit and stored in internal or intermediate storages for controlling purposes, e.g. start-up or back-up procedures
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • F25J2205/72—Pressurising or depressurising the adsorption vessel
    • 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
    • F25J2215/40—Air or oxygen enriched air, i.e. generally less than 30mol% of O2

Definitions

  • the present invention relates to a process for air separation by air distillation, in particular for producing oxygen and / or nitrogen and / or argon, of the type in which the air to be distilled is previously purified by means of at least two adsorbers each of which, in offset, follow a cycle in which an adsorption phase is followed, at a pressure of the cycle, and a regeneration phase ending in a pressurization of the adsorber.
  • the pressures here are absolute pressures.
  • the distillation of the air is carried out cryogenically and therefore requires purifying the air in order to remove the constituents whose solidification temperatures are above the distillation temperature of the air, namely mainly water and carbon dioxide.
  • the main purpose of the distillation of air is to provide, in liquid and / or gaseous form, oxygen and / or nitrogen and / or argon. This production leads to the coproduction of fluids with low oxygen content, such as, for example, impure nitrogen, called residual nitrogen, and higher purity nitrogen, in liquid or gaseous form.
  • the purification of the air to be distilled is commonly carried out by adsorption of the troublesome constituents, generally by means of two bottles containing adsorbent substances arranged in a bed and operating in alternating cycles. While a bottle is in adsorption phase, ie it purifies the air to be distilled, the other bottle is in regeneration phase, that is to say that it is swept by a dry regeneration gas, such as residual nitrogen, desorbing the impurities fixed on the adsorbent during its previous adsorption phase.
  • a dry regeneration gas such as residual nitrogen
  • the regeneration of the adsorbent is all the more effective when it is applied at high temperature and at a low pressure compared with that maintained during the adsorption, which makes it necessary to pressurize a bottle ending its regeneration phase, in order to restore it to a satisfactory pressure condition for its future adsorption phase.
  • the state of the art consists in taking a fraction of purified air at the outlet of the bottle in the adsorption phase and relaxing it towards the bottle at the end of regeneration phase, in order to increase the pressure of the latter.
  • it is however essential to keep constant the flow of air to be sent to the distillation in order to avoid any fluctuation of supply of the distillation apparatus and to maintain the production of oxygen and / or nitrogen and / or argon.
  • the air compression device must provide the excess air that is used for pressurization
  • this additional air flow implies oversizing, and therefore an additional cost, of the compression device. It is indeed required to provide an additional compressed air flow of the order of 5% of the nominal air flow treated by the adsorption bottle (depending on the optimization of the cycle), during a period of pressurization of the 15 minutes for a standard size bottle.
  • the compression apparatus operates at the nominal air flow rate, that is to say that which corresponds to the separating capacity of the air separation apparatus.
  • the normal flow rate of use will be 95 kNm3 / h sent to the cold box where the distillation takes place and 100 kNm3 / h only for the only pressurization phase at the end of regeneration where 5 kNm3 / h of air is sent to pressurize one of the bottles.
  • Some air separation processes use a lost air system in which not all of the purified air is sent to the distillation columns.
  • an expansion turbine is generally found which will depressurise the excess air relative to the oxygen requirement to a pressure close to atmospheric pressure.
  • the object of the invention is to avoid over-sizing the compressors by reducing or even eliminating the increase in the air flow to be compressed in order to supply the additional gas necessary for the pressurization of the adsorbent bottles.
  • the subject of the invention is a process for the distillation of air, in particular intended to produce oxygen and / or nitrogen and / or argon, of the type in which the air to be distilled is compressed beforehand in a compressor, purified by means of at least two adsorbers which each follow, in offset, a cycle in which an adsorption phase is followed at a high pressure of the cycle (Pads), and a regeneration phase at a low pressure P a tmos ending with a repressurization phase of the adsorber, purified air is cooled in an exchange line and then sent to a distillation column d a system of columns and fluids enriched in oxygen and nitrogen are withdrawn from a column of the column system, only during the repressurization phase a flow of purified air, constituting between 3 and 20% of the compressed air in the compressor serves to pressurize, at least partially, the adsorber ending its regeneration phase and the compressed air flow in the compressor during the adsorption phase is substantially equal to the compressed air flow rate in the
  • substantially equal covers the case in which the flow rate of compressed air in the compressor during the adsorption phase differs by not more than 5%, preferably not more than 3%, from the compressed air flow rate. the compressor during the pressurization of the adsorber.
  • the two flows are preferably strictly equal.
  • the flow rate of compressed air in the compressor during the adsorption phase of an adsorber is equal to the compressed air flow rate in the compressor during the pressurization of the adsorber;
  • the reduction of the air flow sent to the turbine and then to the air during repressurization is equal to the air flow rate used during the repressurization to pressurize the adsorber ending its repressurization phase;
  • the compressed air flow rate in the compressor increases with respect to the flow rate sent during the remainder of the cycle and the quantity of air sent for distillation remains equal to that sent during the remainder of the cycle;
  • the column system consists of a double column comprising a medium pressure column and a low pressure column
  • a high oxygen flow rate is withdrawn from the low pressure column and vaporized in the exchange line.
  • PSA pressure swing adsorption
  • TSA temperature swing adsorption
  • TPSA pressure swing adsorption
  • Figure 1 is a schematic view of an installation for operating the method according to the invention.
  • FIG. 1 is shown an installation 1 of air distillation according to the invention.
  • This installation is for example intended to produce oxygen gas OG, as well as liquid oxygen OL.
  • the installation 1 essentially comprises:
  • an apparatus 6 for adsorption air purification which apparatus comprises, on the one hand, two adsorbers 7A, 7B in the form of two bottles each containing adsorbent materials, for example molecular sieve with optionally alumina, capable of adsorbing water and carbon dioxide present in the air and, on the other hand, pipes and connecting valves whose arrangement will become clear when describing the process implemented in the installation 1 and which make it possible successively to subject each adsorber 7A, 7B to the flow of air to be distilled and to a regeneration gas of the adsorbent;
  • adsorbent materials for example molecular sieve with optionally alumina, capable of adsorbing water and carbon dioxide present in the air
  • pipes and connecting valves whose arrangement will become clear when describing the process implemented in the installation 1 and which make it possible successively to subject each adsorber 7A, 7B to the flow of air to be distilled and to a regeneration gas of the adsorbent
  • an air distillation apparatus in the form of a double column 10 comprising a medium pressure column 12, a low pressure column 14 and a vaporizer-condenser 16 coupling these two columns, as well as an argon separation column 26; and
  • a reservoir 18 for storing liquid oxygen for storing liquid oxygen.
  • the air to be distilled, previously compressed by the compressor 4, is purified by one of the adsorbers 7A, 7B of the apparatus 6, and then cooled by the main heat exchange line 8 to an intermediate temperature.
  • the adsorption may be of the TSA, PSA or TPSA type.
  • Part of the air is sent to a lost air turbine 27 and the expanded air is sent to the atmosphere after reheating in the exchanger 8. The rest of the air continues cooling.
  • Another part 29 of the air is sent to the cold compressor 3, returned to the exchange line 8.
  • a part of the supercharged flow is expanded in a turbine 5 to the medium pressure to form the expanded flow rate 7.
  • the expanded flow rate 7 in the vicinity of its dew point is introduced into the vat of the medium pressure column 12.
  • the rest of the compressed air 9 continues cooling in the exchange line 8, is expanded in a valve V and is sent to an intermediate level of the medium pressure column 12.
  • the vaporizer-condenser 16 vaporizes liquid oxygen, for example having a purity of 99.5%, of the tank of the low pressure column 14, by condensing nitrogen gas at the top of the medium pressure column 12.
  • Impure nitrogen or "waste" NR withdrawn from the top of the low pressure column 14, is returned to the main heat exchange line 8, where it causes cooling of the air to be distilled.
  • OL liquid oxygen is withdrawn from the tank of the low pressure column 14 and feeds the storage tank 18. After pressurization in the pump P, it vaporizes in the main heat exchange line 8 and distributed by a pipe of production 32 to form gaseous oxygen under pressure.
  • An argon production column 26 is fed from the low pressure column 14.
  • the cycle of FIG. 2, whose period is, for example, equal to approximately 360 minutes for an adsorption pressure substantially equal to 20 bars, comprises 4 successive stages I to IV.
  • the compressed air by the compressor 4 supplies the adsorber 7A via an open valve 40A.
  • the outlet of the adsorber 7A is connected to the exchange line 8 via an open valve 42A.
  • the adsorber 7A is in the regeneration phase, while the adsorber 7B is in the adsorption phase. More specifically, during stage II, a valve 44A for venting the adsorber 7A is opened so that the pressure inside the bottle of the adsorber 7A is reduced to a pressure substantially equal to atmospheric pressure, noted P a tmo in Figure 2.
  • step III the valve 44A remains open and residual nitrogen NR withdrawn at the top of the low pressure column 14 and then heated in the exchanger 8 feeds via an open valve 46A, the adsorber 7A to circulate there against a current. This is the actual phase of regeneration during which impurities are desorbed and the beds regenerated.
  • step IV the valves 44A and 46A are closed, to allow the pressurization of the adsorber.
  • the pressurization of the adsorber is provided by a stream of purified air, via the valve 42A open, this flow of clean air from the bottles 7A, 7B.
  • Sub-step IV continues with sub-step IV "until the pressure inside the adsorber 7A is substantially equal to the high pressure P a ds., By opening the valve 50.
  • the pressurization of each adsorber no longer requires, during step IV, to increase the flow rate of the compressor 4.
  • the compressor 4 is optimally sized, that is, - say so that its nominal flow is substantially constant. The investment and operating costs of this compression apparatus are reduced, compared with those of prior art installations.
  • the compressor 4 compresses 100 kNm3 / h of air and all the purified air is sent to the exchange line 8. 30 kNm3 / h of air are sent to the air turbine lost 5. 70 kNm3 / h of air are sent to the system of distillation columns.
  • the compressor 4 compresses 100 kNm3 / h of air, 95 kNm3 / h are sent to the discharge line 8 and 5 kNm3 / h are sent to pressurize an adsorption bottle. 25 kNm3 / h of air (thus 5 kNm3 / h less) are sent to the lost air turbine 5 and 70 kNm3 / h of air are always sent to the distillation column system. It will be understood that this invention applies to any process involving a lost air turbine, whether there is compression in a cold compressor or not, double column or not, argon production or not, pressurization and vaporization of liquid oxygen or not.

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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)
  • Separation Of Gases By Adsorption (AREA)
EP12714821.1A 2011-03-31 2012-03-21 Verfahren zur trennung von luft durch kryogene destillation Not-in-force EP2712419B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1152733A FR2973486B1 (fr) 2011-03-31 2011-03-31 Procede de separation d'air par distillation cryogenique
PCT/FR2012/050587 WO2012131231A2 (fr) 2011-03-31 2012-03-21 Procede de separation d'air par distillation cryogenique

Publications (2)

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EP2712419A2 true EP2712419A2 (de) 2014-04-02
EP2712419B1 EP2712419B1 (de) 2017-08-09

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US (1) US20140013798A1 (de)
EP (1) EP2712419B1 (de)
CN (1) CN104246401B (de)
FR (1) FR2973486B1 (de)
WO (1) WO2012131231A2 (de)

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CA2957421A1 (en) * 2014-08-15 2016-02-18 Biomerieux, Inc. Methods, systems, and computer program products for detecting pipette tip integrity
WO2016146246A1 (de) * 2015-03-13 2016-09-22 Linde Aktiengesellschaft Anlage zur erzeugung von sauerstoff durch tieftemperaturzerlegung von luft
US10895417B2 (en) 2016-03-25 2021-01-19 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method for the production of air gases by the cryogenic separation of air with improved front end purification and air compression
FR3074274B1 (fr) * 2017-11-29 2020-01-31 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation d'air par distillation cryogenique
US11137205B2 (en) * 2018-12-21 2021-10-05 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and apparatus for eliminating heat bumps following regeneration of adsorbers in an air separation unit
US11029086B2 (en) * 2018-12-21 2021-06-08 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and apparatus for reducing process disturbances during pressurization of an adsorber in an air separation unit
CN110787587A (zh) 2019-11-08 2020-02-14 乔治洛德方法研究和开发液化空气有限公司 一种空分纯化均压系统及控制方法

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US5419136A (en) * 1993-09-17 1995-05-30 The Boc Group, Inc. Distillation column utilizing structured packing having varying crimp angle
US6073463A (en) * 1998-10-09 2000-06-13 Air Products And Chemicals, Inc. Operation of a cryogenic air separation unit which intermittently uses air feed as the repressurization gas for a two bed PSA system
FR2787560B1 (fr) * 1998-12-22 2001-02-09 Air Liquide Procede de separation cryogenique des gaz de l'air
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WO2007033838A1 (de) * 2005-09-23 2007-03-29 Linde Aktiengesellschaft Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
FR2895069B1 (fr) * 2005-12-20 2014-01-31 Air Liquide Appareil de separation d'air par distillation cryogenique
FR2896860A1 (fr) * 2006-01-31 2007-08-03 Air Liquide Procede de separation d'air par distillation cryogenique et installation correspondante
FR2903483B1 (fr) * 2006-07-04 2014-07-04 Air Liquide Procede et appareil de separation d'air par distillation cryogenique
FR2910604B1 (fr) * 2006-12-22 2012-10-26 Air Liquide Procede et appareil de separation d'un melange gazeux par distillation cryogenique
FR2913759B1 (fr) * 2007-03-13 2013-08-16 Air Liquide Procede et appareil de production de gaz de l'air sous forme gazeuse et liquide a haute flexibilite par distillation cryogenique.
EP2185879A1 (de) * 2007-08-10 2010-05-19 L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Verfahren und vorrichtung zur trennung von luft durch kryogene destillation
EP2176610B1 (de) * 2007-08-10 2019-04-24 L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Verfahren zur trennung von luft durch kryogene destillation

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Also Published As

Publication number Publication date
WO2012131231A2 (fr) 2012-10-04
CN104246401B (zh) 2016-02-03
FR2973486A1 (fr) 2012-10-05
FR2973486B1 (fr) 2013-05-03
US20140013798A1 (en) 2014-01-16
CN104246401A (zh) 2014-12-24
EP2712419B1 (de) 2017-08-09
WO2012131231A3 (fr) 2015-08-20

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