US20140013798A1 - Method for separating air by means of cryogenic distillation - Google Patents

Method for separating air by means of cryogenic distillation Download PDF

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US20140013798A1
US20140013798A1 US14/004,264 US201214004264A US2014013798A1 US 20140013798 A1 US20140013798 A1 US 20140013798A1 US 201214004264 A US201214004264 A US 201214004264A US 2014013798 A1 US2014013798 A1 US 2014013798A1
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air
during
sent
adsorber
phase
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Patrick Le Bot
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Assigned to L'AIR LIQUIDE SOCIETE ANONYME POUR L'ETUDE ET L'EXPLOITATION DES PROCEDES GEORGES CLAUDE reassignment L'AIR LIQUIDE SOCIETE ANONYME POUR L'ETUDE ET L'EXPLOITATION DES PROCEDES GEORGES CLAUDE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LE BOT, PATRICK
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048Providing 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
    • F25J3/04054Providing 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078Providing 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
    • F25J3/0409Providing 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163Hot end purification of the feed air
    • F25J3/04169Hot end purification of the feed air by adsorption of the impurities
    • F25J3/04175Hot end purification of the feed air by adsorption of the impurities at a pressure of substantially more than the highest pressure column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04151Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04163Hot end purification of the feed air
    • F25J3/04169Hot end purification of the feed air by adsorption of the impurities
    • F25J3/04181Regenerating the adsorbents
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation 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
    • F25J3/0429Generation 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation 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
    • F25J3/0429Generation 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
    • F25J3/04296Claude expansion, i.e. expanded into the main or high pressure column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04406Processes 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
    • F25J3/04412Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04472Processes 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
    • F25J3/04478Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00Processes or apparatus using other separation and/or other processing means
    • F25J2205/60Processes 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
    • F25J2205/66Regenerating the adsorption vessel, e.g. kind of reactivation gas
    • F25J2205/72Pressurising or depressurising the adsorption vessel
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/40Air or oxygen enriched air, i.e. generally less than 30mol% of O2

Definitions

  • This invention relates to a method for separating air by distillation of air, in particular intended for producing oxygen and/or nitrogen and/or argon, of the type wherein the air to be distilled is purified beforehand by means of at least two adsorbers which each follow, offset, a cycle wherein succeed an adsorption phase, at a pressure of the cycle, and a regeneration phase ending with a pressurisation of the adsorber.
  • the distillation of the air compressed beforehand by a compression apparatus, is carried out cryogenic temperatures and therefore requires that the air be purified in order to remove from therein the constituents of which the solidification temperatures are higher than the distillation temperature of the air, i.e. primarily water and carbon dioxide.
  • the main objective of the distillation of the air is to provide, in liquid and/or gaseous form, oxygen and/or nitrogen and/or argon. This production generates the coproduction of fluids with a low oxygen content, such as, for example, impure nitrogen, called residual nitrogen, and nitrogen of the highest purity, in liquid or gaseous form.
  • the purification of the air to be distilled is commonly carried out by adsorption of the disturbing constituents, by means in general of two bottles containing adsorbent substances arranged on a bed and operating in alternating cycles. While one bottle is in adsorption phase, (i.e., it is purifying the air that is to be distilled) the other bottle is in regeneration phase, (i.e., it is flushed with a dry regeneration gas, such as residual nitrogen) desorbing the impurities fixed on the adsorbent during its preceding adsorption phase.
  • a dry regeneration gas such as residual nitrogen
  • the regeneration of the adsorbent is increasingly effective when it is applied at a high temperature and at a low pressure in relation to that maintained during the adsorption, which requires that a bottle terminating its regeneration phase be pressurised, in order to restore a satisfactory condition of pressure for its upcoming adsorption phase.
  • the state of the art consists in sampling a fraction of purified air at the outlet of the bottle in adsorption phase and to decompress it to the bottle at the end of the regeneration phase, in order to increase the pressure of the latter.
  • it is however indispensable to maintain the air flow to be sent to the distillation constant in order to prevent any fluctuation in the supply of the distillation apparatus and in order to maintain the production of oxygen and/or nitrogen and/or argon.
  • the air compression apparatus must provide this surplus of air which is used for the pressurisation.
  • this additional air flow implies oversizing, and therefore an extra cost, of the compression apparatus. It is indeed asked to provide an additional compressed air flow of about 5% of the nominal air flow processed by the bottle in adsorption (according to the optimisation of the cycle), during a pressurisation duration of about 15 minutes for a bottle of common size.
  • the compression apparatus operations with nominal air flow (i.e., that which corresponds to the separation capacity of the device for separating air).
  • the normal flow rate for use will be 95 kNm 3 /hr sent to the cold box wherein takes place the distillation and 100 kNm 3 /hr solely for the single pressurisation phase at the end of regeneration wherein 5 kNm 3 /hr of air is sent in order to pressurise one of the bottles.
  • Certain methods for separating air use a lost air system wherein all of the purified air is not sent to the distillation columns. In this case there is generally an expansion turbine which will decompress to a pressure close to the atmospheric pressure the excess air in relation to the oxygen needs.
  • the purpose of certain embodiments of the invention is to avoid the oversizing of compressors by reducing, even by eliminating, the increase in the air flow to be compressed in order to provide the additional gas required for the pressurisation of the bottles of adsorbent.
  • an embodiment of the invention has for purpose a method for distilling air, in particular intended to produce oxygen and/or nitrogen and/or argon, of the type wherein the air to be distilled is compressed beforehand in a compressor, purified by means of at least two adsorbers which each follow, offset, a cycle wherein succeed an adsorption phase, at a high pressure of the cycle (P ads ) and a regeneration phase at a low pressure P atmos ending with a repressurisation phase of the adsorber, the purified air is cooled in an exchange line and then sent to a distillation column of a system of columns and oxygen-rich and nitrogen-rich fluids are withdrawn from a column of the system of columns, only during the repressurisation phase a purified air flow, constituting between 3 and 20% of the air compressed in the compressor, is used to pressurise, at least partially, the adsorber completing its regeneration phase and the air flow compressed in the compressor during the adsorption phase is substantially equal to the air flow compressed in the compressor
  • substantially equal covers the case wherein the air flow compressed in the compressor during the adsorption phase differs by at most 5%, more preferably by at most 3%, from the air flow compressed in the compressor during the pressurisation of the adsorber.
  • the two flows are more preferably strictly equal.
  • PSA Pressure swing adsorption
  • TSA Tempoture swing adsorption
  • TPSA Tempoture and pressure swing adsorption
  • FIG. 1 shows a diagrammatical view of an installation for a method according to an embodiment of the invention an embodiment of the present invention.
  • FIG. 1 shows an installation 1 for the distillation of air according to the invention.
  • This installation is for example intended to produce gaseous oxygen OG, as well as liquid oxygen OL.
  • the installation 1 substantially comprises:
  • the operation of the installation 1 of FIG. 1 is as follows.
  • the air to be distilled, compressed beforehand by the compressor 4 is purified by one of the adsorbers 7 A, 7 B of the apparatus 6 , then cooled by the main thermal exchange line 8 to an intermediate temperature.
  • the adsorption can be of the TSA, PSA or TPSA type.
  • a portion 25 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 to be cooled.
  • Another portion 29 of the air is sent to the cold compressor 3 , sent back to the exchange line 8 .
  • a portion of the supercharged flow is expanded in a turbine 5 to the medium pressure in order to form the expanded flow 7 .
  • the expanded flow 7 in the vicinity of its dew point is introduced into the tank of the medium-pressure column 12 .
  • the rest of the supercharged air 9 continues to be cooled in the exchange line 8 , is expanded in a valve V then is sent to an intermediate level of the medium-pressure column 12 .
  • the vaporiser-condenser 16 vaporises liquid oxygen, for example having a purity of 99.5%, of the tank of the low-pressure column 14 , by condensation of gaseous nitrogen at the head of the medium-pressure column 12 .
  • “Rich liquid” LR oxygen-rich air
  • liquid nitrogen NL substantially pure
  • Impure or “residual” nitrogen NR withdrawn from the top of the low-pressure column 14 , is sent back to the main thermal exchange line 8 , where it causes the cooling of the air to be distilled.
  • Liquid oxygen OL is withdrawn from the tank of the low-pressure column 14 and supplies the storage reservoir 18 . After pressurisation in the pump P, it is vaporised in the main thermal exchange line 8 and distributed by a production pipe 32 in order to form pressurised gaseous oxygen.
  • An argon production column 26 is supplied from the low-pressure column 14 .
  • the cycle of FIG. 2 of which the period is, by way of example, equal to about 360 minutes for an adsorption pressure substantially equal to 20 bars, comprises 4 successive steps I to IV. These four steps shall now be described successively for the adsorber 7 A, with the understanding that the adsorber 7 B follows these same steps with a time delay of substantially
  • the adsorber 7 A is in adsorption phase under a high operating pressure noted as P ads , while the adsorber 7 B is in regeneration phase.
  • the air compressed by the compressor 4 supplies the adsorber 7 A, via an open valve 40 A.
  • the outlet of the adsorber 7 A is connected to the exchange line 8 , via an open valve 42 A.
  • the adsorber 7 A is in regeneration phase, while the adsorber 7 B is in adsorption phase. More precisely, during the step II, a valve 44 A for venting the adsorber 7 A to the air is open in such a way that the pressure inside the bottle of the adsorber 7 A is brought to a pressure substantially equal to the atmospheric pressure, noted as P atmos in FIG. 2 .
  • the valve 44 A remains open and residual nitrogen NR withdrawn at the head of the low-pressure column 14 then heated in the exchanger 8 supplies, via an open valve 46 A, the adsorber 7 A in order to circulate therein against the current. This is the effective phase of the regeneration during which the impurities are desorbed and the beds are regenerated.
  • the valves 44 A and 46 A are closed, in order to allow for the pressurisation of the adsorber.
  • the pressurisation of the adsorber is provided by a purified air flow, via the open valve 42 A, this purified air flow coming from the bottles 7 A, 7 B.
  • the sub-step IV′ is continued by the sub-step IV′′ until the pressure inside the adsorber 7 A is substantially equal to the high pressure P ads , by opening the valve 50 .
  • the pressurisation of each adsorber no longer requires, during the step IV, to increase the flow of the compressor 4 .
  • the compressor 4 is sized in an optimum manner, i.e. in such a way that its nominal flow is substantially constant. The investment and operating costs for this compression apparatus are reduced, in relation to those of installations concerning prior art.
  • the compressor 4 compresses 100 kNm 3 /hr of air and all of the purified air is sent to the exchange line 8. 30 kNm 3 /hr of air is sent to the lost air turbine 5. 70 kNm 3 /hr of air is sent to the system of distillation columns.
  • the compressor 4 compresses 100 kNm3/h of air, 95 kNm 3 /hr is sent to the exchange line 8 and 5 kNm 3 /hr is sent in order to pressurise an adsorption bottle. 25 kNm 3 /hr of air (therefore 5 kNm 3 /hr less) is sent to the lost air turbine 5 and 70 kNm 3 /hr of air is still sent to the system of distillation columns.
  • this invention applies to any method involving a lost air turbine, whether there is compression in a cold compressor or not, a double column or not, a production of argon or not, pressurisation and vaporisation of liquid oxygen or not.
  • “Comprising” in a claim is an open transitional term which means the subsequently identified claim elements are a nonexclusive listing (i.e., anything else may be additionally included and remain within the scope of “comprising”). “Comprising” as used herein may be replaced by the more limited transitional terms “consisting essentially of” and “consisting of” unless otherwise indicated herein.
  • Providing in a claim is defined to mean furnishing, supplying, making available, or preparing something. The step may be performed by any actor in the absence of express language in the claim to the contrary a range is expressed, it is to be understood that another embodiment is from the one.
  • Optional or optionally means that the subsequently described event or circumstances may or may not occur.
  • the description includes instances where the event or circumstance occurs and instances where it does not occur.
  • Ranges may be expressed herein as from about one particular value, and/or to about another particular value. When such particular value and/or to the other particular value, along with all combinations within said range.

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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)
US14/004,264 2011-03-31 2012-03-21 Method for separating air by means of cryogenic distillation Abandoned US20140013798A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR1152733 2011-03-31
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

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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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US20170276428A1 (en) * 2016-03-25 2017-09-28 L'air Liquide, Societe Anonyme Pour I'etude Et I'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
US20180008976A1 (en) * 2014-08-15 2018-01-11 Biomerieux, Inc. Methods, systems, and computer program products for verifying dispensing of a fluid from a pipette
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
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
US11612850B2 (en) 2019-11-08 2023-03-28 L'Air Liquide, Societe Anonyme Por L'Etude Et L'Exploitation Des Procedes Georges Claude Pressure equalizing system for air separation purification and control method

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WO2016146246A1 (de) * 2015-03-13 2016-09-22 Linde Aktiengesellschaft Anlage zur erzeugung von sauerstoff durch tieftemperaturzerlegung von luft
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

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US4261719A (en) * 1976-04-14 1981-04-14 Kobe Steel, Ltd. Method of and apparatus for controlling rate of material air supply to air separation plant
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
US6257020B1 (en) * 1998-12-22 2001-07-10 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for the cryogenic separation of gases from air
US20040055465A1 (en) * 2000-12-29 2004-03-25 Alain Guillard Method for treating a gas by adsorption and corresponding installation
WO2008084167A2 (fr) * 2006-12-22 2008-07-17 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation d'un melange gazeux par distillation cryogenique

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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
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

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4261719A (en) * 1976-04-14 1981-04-14 Kobe Steel, Ltd. Method of and apparatus for controlling rate of material air supply to air separation plant
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
US6257020B1 (en) * 1998-12-22 2001-07-10 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process for the cryogenic separation of gases from air
US20040055465A1 (en) * 2000-12-29 2004-03-25 Alain Guillard Method for treating a gas by adsorption and corresponding installation
WO2008084167A2 (fr) * 2006-12-22 2008-07-17 L'air Liquide Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation d'un melange gazeux par distillation cryogenique
US8713964B2 (en) * 2006-12-22 2014-05-06 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and device for separating a gas mixture by cryogenic distillation

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20180008976A1 (en) * 2014-08-15 2018-01-11 Biomerieux, Inc. Methods, systems, and computer program products for verifying dispensing of a fluid from a pipette
US20170276428A1 (en) * 2016-03-25 2017-09-28 L'air Liquide, Societe Anonyme Pour I'etude Et I'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
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
US11619443B2 (en) 2016-03-25 2023-04-04 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
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
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
US11612850B2 (en) 2019-11-08 2023-03-28 L'Air Liquide, Societe Anonyme Por L'Etude Et L'Exploitation Des Procedes Georges Claude Pressure equalizing system for air separation purification and control method

Also Published As

Publication number Publication date
WO2012131231A2 (fr) 2012-10-04
CN104246401B (zh) 2016-02-03
FR2973486A1 (fr) 2012-10-05
EP2712419A2 (de) 2014-04-02
FR2973486B1 (fr) 2013-05-03
CN104246401A (zh) 2014-12-24
EP2712419B1 (de) 2017-08-09
WO2012131231A3 (fr) 2015-08-20

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