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EP1143216A1 - Process and apparatus for the production of oxygen enriched fluid by cryogenic distillation - Google Patents

Process and apparatus for the production of oxygen enriched fluid by cryogenic distillation Download PDF

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Publication number
EP1143216A1
EP1143216A1 EP01400749A EP01400749A EP1143216A1 EP 1143216 A1 EP1143216 A1 EP 1143216A1 EP 01400749 A EP01400749 A EP 01400749A EP 01400749 A EP01400749 A EP 01400749A EP 1143216 A1 EP1143216 A1 EP 1143216A1
Authority
EP
European Patent Office
Prior art keywords
argon
enriched
flow
column
oxygen
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
EP01400749A
Other languages
German (de)
French (fr)
Other versions
EP1143216B1 (en
Inventor
BenoĆ­t Davidian
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.)
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
LAir Liquide SA a Directoire et Conseil de Surveillance 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, LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP1143216A1 publication Critical patent/EP1143216A1/en
Application granted granted Critical
Publication of EP1143216B1 publication Critical patent/EP1143216B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • F25J3/04248—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.
    • F25J3/04387—Details relating to the work expansion, e.g. process parameter etc. using liquid or hydraulic turbine expansion
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—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
    • F25J3/04018—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 main feed 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
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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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    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • F25J3/04115—Arrangements of compressors and /or their drivers characterised by the type of prime driver, e.g. hot gas expander
    • F25J3/04127—Gas turbine as the prime mechanical driver
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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
    • F25J3/04315—Lowest pressure or impure nitrogen, so-called waste nitrogen expansion
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    • 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
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    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • 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
    • F25J3/04448—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 in a double column flowsheet with an intermediate pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
    • F25J3/04545—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels for the gasification of solid or heavy liquid fuels, e.g. integrated gasification combined cycle [IGCC]
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    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating
    • F25J3/04575—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating for a gas expansion plant, e.g. dilution of the combustion gas in a gas turbine
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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
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04593—The air gas consuming unit is also fed by an air stream
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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
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
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    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
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    • F25J2240/02—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream
    • F25J2240/10—Expansion of a process fluid in a work-extracting turbine (i.e. isentropic expansion), e.g. of the feed stream the fluid being air
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    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream being argon or crude argon

Definitions

  • the present invention relates to a production method and apparatus of a fluid enriched in oxygen by cryogenic distillation of a mixture containing nitrogen, oxygen and argon.
  • it relates to a method and an apparatus for separating air by cryogenic distillation allowing the production of pure oxygen, i.e. oxygen containing at least 95% mol. oxygen, preferably at least 98% mol. oxygen or even 99.5% mol. oxygen.
  • Patent application EP-A-0540900 describes a production process impure oxygen in which part of the impure argon containing at least 90% of argon from a column of mixture is mixed with the residual nitrogen from a simple column.
  • the mixing column operates at the same low pressure as the low column pressure, up to 1.75 bara.
  • EP-A-0384213 has a low pressure column operating at between 1.5 and 10 bara but the argon column operates at a lower pressure.
  • US-A-4932212 describes the case in which the low pressure column and the argon column operate at pressures between 1 and 2 bars.
  • EP-A-0518491 describes a process for the production of nitrogen gas under pressure and incidentally liquid nitrogen, liquid argon and liquid oxygen in which the low pressure column and the argon column operate at a pressure substantially identical above 2.5 bara. No argon gas flow is produced.
  • EP-A-0952415 describes an apparatus comprising a double column and a argon column operating with a yield lower than the optimal yield.
  • An object of the present invention is to increase the yield of pure oxygen an air separation device.
  • Another object of the invention is to provide an air separation device particularly well suited to the demands of large quantities of nitrogen under pressure (typically when integrated with an IGCC gas turbine).
  • the flow enriched in argon or the flow enriched in argon mixed with a gas enriched in nitrogen can be sent upstream of the expansion machine of a gas turbine.
  • the flow enriched in argon can contain between 10 and 95 mol%. argon (or between 40 and 95% mol. argon), between 2 and 40.% mol of oxygen and between 2 and 40% mol. nitrogen.
  • the flow enriched in argon which is released to the atmosphere and / or which is used to regenerate adsorbent beds or reversible exchangers and / or which is mixed with a gas enriched in nitrogen from the device and / or another device and / or which is sent upstream of the expansion machine of a gas turbine can constitute between 0.3 and 2% of the air, preferably between 0.5 and 1% of the air. For this reason, it is best to mix the flow enriched in argon with a gas enriched in nitrogen containing at least 90% mol.
  • the mixture formed comprises less than 2% mol. argon, preferably less than 1% mol. argon.
  • the low pressure column can operate between 2 and 10 bara, preferably above 2.5 bara.
  • the apparatus may include an auxiliary separation column a flow containing at least argon and oxygen and two other columns, of which a high pressure column and a low pressure column thermally connected between them, the auxiliary column being supplied from the low pressure column.
  • the apparatus may include an auxiliary separation column of a flow rate containing at least argon and oxygen and at least three others columns, including a high pressure column, an intermediate pressure column and a low pressure column thermally connected to each other, the auxiliary column being supplied from the low pressure column or the intermediate pressure column.
  • an integrated method of separation comprising a method according to one of claims 1 to 12 in which a nitrogen-enriched gas is sent from the operating column preferably at the lowest pressure at the gas turbine, after one step possible compression and, optionally, a fluid enriched with oxygen is sent from an appliance column to a gasifier.
  • the auxiliary column contains between 30 and 40 trays theoretical.
  • the separation of oxygen and argon in the low pressure column tank is facilitated.
  • the fluid enriched in argon withdrawn from the auxiliary column is not necessarily an end product of the device but can be used to cool flows re-entering the columns or supplying frigories by expansion.
  • Figure 1 is a diagram of an oxygen production apparatus according to the invention using a double column.
  • Figure 2 is a diagram of an oxygen production apparatus according to the invention using a triple column.
  • an air flow 1 of 1000Nm3 / h is purified by beds adsorbent 4 is divided into two.
  • the flow 2 is boosted at a higher pressure, sent to the heat exchanger 3 where it cools ensuring the vaporization of liquid oxygen and then to a hydraulic turbine 5 where it comes out at least partially liquid.
  • This liquid (or two-phase mixture) 7 is sent to the column high pressure 9 operating between 14 and 15 bar and possibly partly at the column low pressure 11 operating between 4 and 6 bar (or even between 2 and 10 bar), either sending part of the capacity liquid upstream of the medium pressure column either by withdrawing a flow having a composition similar to that of the liquid air of the high pressure column 9, as shown in Figure 1.
  • the device may include an insufflation turbine which serves during start-up or a low-pressure nitrogen turbine 55.
  • a flow of rich liquid 15 is withdrawn from the high pressure column and sent to the sub-cooler 17, divided in two and sent in part to the lower column pressure, after expansion in the valve 21 and in part at the head condenser 23 of the auxiliary column 25 after expansion in the valve 27. At least the rich liquid partially vaporized in the overhead condenser is sent to the lower column pressure 11. If the vaporization is partial, a liquid flow and a gas flow are sent from the condenser to the low pressure column.
  • a nitrogen gas flow 19 can optionally be withdrawn from the head of the high pressure column 9.
  • the auxiliary column is supplied by a gas flow 29 containing between 5 and 15% mol. argon, preferably around 7 mol%. argon.
  • the tank liquid 31 of the auxiliary column is returned to the low pressure column which operates substantially at the same pressure as the auxiliary column.
  • the auxiliary column 25 can alternatively be supplied with a liquid flow containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon.
  • column 25 will have a tank reboiler, heated by a gas flow such as air or nitrogen from the high pressure column 9.
  • a liquid air flow 33 and a lean liquid flow 35 are sent from the high pressure column 9 to low pressure column 11, after having been sub-cooled in the sub-cooler 17 and expanded in valves.
  • a liquid oxygen flow 37 containing 99.5% mol. oxygen is drawn in low pressure column tank, pressurized by a pump 39 and vaporized in the exchanger 3.
  • the mixture 53 heats up in the sub-cooler 17 then heats up in the exchanger 3.
  • the mixture can then be discharged into the atmosphere and / or can be used to regenerate the adsorbent beds 4 or reversible exchangers and / or sent in upstream of the expansion machine 51 of a gas turbine after a step of compression.
  • part of the mixture 53 can be expanded in a turbine 55 (dotted line).
  • a triple column is used in place of the double column of Figure 1.
  • An air flow 1 is purified by adsorbent beds 4 is divided into two.
  • Flow 2 is boosted to a higher pressure, sent to the heat exchanger heat 3 where it cools by ensuring the vaporization of liquid oxygen and then at a hydraulic turbine 5 where it exits in at least partially liquid form.
  • This liquid (or two-phase mixture) 7 is sent to the high pressure column 9 operating between 14 and 15 bar and possibly partly at the low pressure column 11 operating between 4 and 6 bar and / or possibly at the intermediate pressure column 40 operating between 7 and 9 bar, either by sending part of the liquid of a capacity upstream of the middle column pressure either by withdrawing a flow having a composition similar to that of liquid air of the high pressure column 9, as shown in FIG. 2.
  • the device may include an insufflation turbine which serves during start-up or a low-pressure nitrogen turbine 55.
  • a flow of rich liquid 15 is withdrawn from the high pressure column and sent to the sub-cooler 17, divided in two and sent partly to the middle of the column operating at intermediate pressure 40, after expansion in valve 21 and partly at head condenser 23 of the auxiliary column 25 after expansion in the valve 27.
  • the at least partially vaporized rich liquid in the overhead condenser is sent to the low pressure column 11. If the vaporization is partial, a liquid flow and a flow gases are sent from the condenser to the low pressure column.
  • a nitrogen gas flow 19 can optionally be withdrawn from the head of the high pressure column 9.
  • the auxiliary column is supplied with part of a gas flow 29 containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon.
  • the liquid tank 31 of the auxiliary column is returned to the low pressure column which operates at substantially the same pressure as the auxiliary column.
  • the auxiliary column 25 can alternatively be supplied with a liquid flow containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon.
  • column 25 will have a tank reboiler, heated by a gas flow such as air or nitrogen from the high pressure column 9.
  • the rest of the gas flow 29 is used to heat the tank reboiler 41 of the column 40 and after condensation is returned to the low pressure column with the flow rate 31.
  • the tank liquid 43 of the column 40 is partly sent directly to the low pressure column and partly to the condenser at the top of column 40 where it at least partially vaporizes before being sent to the low pressure column at its tower.
  • the overhead liquid 47 of the column 40 is sub-cooled in the exchanger 17, expanded, mixed with expanded flow 35 and sent to the top of the lower column pressure.
  • a liquid air flow 33 and a lean liquid flow 35 are sent from the high pressure column 9 to low pressure column 11, after having been sub-cooled in the sub-cooler 17 and expanded in valves.
  • a liquid oxygen flow 37 containing 99.5% mol. oxygen is drawn in low pressure column tank, pressurized by a pump 39 and vaporized in the exchanger 3.
  • the mixture 53 heats up in the sub-cooler 17 then heats up in the exchanger 3.
  • the mixture can then be discharged into the atmosphere and / or can be used to regenerate the adsorbent beds 4 or reversible exchangers and / or sent in upstream of the expansion machine 51 of a gas turbine after a step of possible compression.
  • part of the mixture 53 can be expanded in a turbine 55 (dotted line).
  • the method according to the invention is of particular interest in the case in which the nitrogen in the low pressure column is valued, for example by sending it to an expansion machine 51 of a gas turbine.
  • at least part of the air 1 can come from compressor 53 of the gas turbine and the oxygen produced by the device distillation can be used for the gasification necessary to produce the fuel for the gas turbine.

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  • Physics & Mathematics (AREA)
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Abstract

Cryogenic distillation enables pure oxygen (95% minimum) to be obtained from a mixture containing nitrogen, oxygen and argon. The production of an oxygen (O2)-enriched flow in a cryogenic distillation unit comprises the following stages: (a) cooling of a supply (1) containing O2, nitrogen (N2) and argon (Ar) and introduction in a distillation unit comprising an auxiliary column (25) for the separation of a flow (29) containing Ar and O2, the unit comprising two other columns (9,18); (b) separation of the flow to form fluids enriched in O2 and N2 (15,33); (c) conveyance of the flow containing Ar and O2 from one of the columns (18) to the auxiliary column, both operating at 2-10 bars; (d) withdrawal of an O2-enriched flow (37) containing at least 95% mol of O2; and (e) withdrawal of an Ar-enriched flow (49) from the auxiliary column. Part of the Ar-enriched flow is rejected to atmosphere and/or acts as an adsorbent bed (4) regenerator and/or part may be mixed with an N2-enriched gas (47) from the unit, or from another unit. An Independent claim is also included for the apparatus for the above process.

Description

La prĆ©sente invention est relative Ć  un procĆ©dĆ© et Ć  un appareil de production d'un fluide enrichi en oxygĆØne par distillation cryogĆ©nique d'un mĆ©lange contenant de l'azote, de l'oxygĆØne et de l'argon.The present invention relates to a production method and apparatus of a fluid enriched in oxygen by cryogenic distillation of a mixture containing nitrogen, oxygen and argon.

En particulier il concerne un procĆ©dĆ© et Ć  un appareil de sĆ©paration d'air par distillation cryogĆ©nique permettant la production d'oxygĆØne pur, c'est Ć  dire de l'oxygĆØne contenant au moins 95% mol. oxygĆØne, de prĆ©fĆ©rence au moins 98% mol. d'oxygĆØne ou mĆŖme 99,5% mol. d'oxygĆØne.In particular, it relates to a method and an apparatus for separating air by cryogenic distillation allowing the production of pure oxygen, i.e. oxygen containing at least 95% mol. oxygen, preferably at least 98% mol. oxygen or even 99.5% mol. oxygen.

Lorsqu'on veut faire de l'oxygĆØne pur, on doit nĆ©cessairement sĆ©parer l'oxygĆØne de l'argon. Si les colonnes de l'appareil opĆØrent toutes Ć  une pression au-dessus de 2 bar, la distillation est difficile.When we want to make pure oxygen, we must necessarily separate the oxygen argon. If the columns of the device all operate at a pressure above 2 bar, distillation is difficult.

La production d'argon pur nƩcessite une colonne ayant plus que 100 plateaux thƩoriques.The production of pure argon requires a column with more than 100 trays theoretical.

La demande de brevet EP-A-0540900 dĆ©crit un procĆ©dĆ© de production d'oxygĆØne impur dans lequel une partie de l'argon impur contenant au moins 90% d'argon d'une colonne de mixture est mĆ©langĆ© avec l'azote rĆ©siduaire d'une simple colonne. La colonne de mixture opĆØre Ć  la mĆŖme pression basse que la colonne basse pression, jusqu'Ć  1,75 bara.Patent application EP-A-0540900 describes a production process impure oxygen in which part of the impure argon containing at least 90% of argon from a column of mixture is mixed with the residual nitrogen from a simple column. The mixing column operates at the same low pressure as the low column pressure, up to 1.75 bara.

EP-A-0384213 a une colonne basse pression opĆ©rant Ć  entre 1,5 et 10 bara mais la colonne argon opĆØre Ć  une pression plus basse.EP-A-0384213 has a low pressure column operating at between 1.5 and 10 bara but the argon column operates at a lower pressure.

US-A-4932212 dĆ©crit le cas dans lequel la colonne basse pression et la colonne argon opĆØrent Ć  des pressions entre 1 et 2 bars.US-A-4932212 describes the case in which the low pressure column and the argon column operate at pressures between 1 and 2 bars.

EP-A-0518491 dĆ©crit un procĆ©dĆ© de production d'azote gazeux sous pression et accessoirement de l'azote liquide, de l'argon liquide et de l'oxygĆØne liquide dans lequel la colonne basse pression et la colonne argon opĆØrent Ć  une pression substantiellement identique au-dessus de 2,5 bara. Aucun dĆ©bit d'argon gazeux n'est produit.EP-A-0518491 describes a process for the production of nitrogen gas under pressure and incidentally liquid nitrogen, liquid argon and liquid oxygen in which the low pressure column and the argon column operate at a pressure substantially identical above 2.5 bara. No argon gas flow is produced.

EP-A-0952415 dƩcrit un appareil comprenant une double colonne et une colonne argon opƩrant avec un rendement infƩrieur au rendement optimal.EP-A-0952415 describes an apparatus comprising a double column and a argon column operating with a yield lower than the optimal yield.

Un but de la prĆ©sente invention est d'augmenter le rendement en oxygĆØne pur d'un appareil de sĆ©paration d'air.An object of the present invention is to increase the yield of pure oxygen an air separation device.

Un autre but de l'invention est de fournir un appareil de sĆ©paration d'air particuliĆØrement bien adaptĆ© aux demandes de grandes quantitĆ©s d'azote sous pression (typiquement en cas d'intĆ©gration avec une turbine Ć  gaz d'un IGCC). Another object of the invention is to provide an air separation device particularly well suited to the demands of large quantities of nitrogen under pressure (typically when integrated with an IGCC gas turbine).

Selon un objet de l'invention, il est prĆ©vu un procĆ©dĆ© de production d'un dĆ©bit enrichi en oxygĆØne dans un appareil de distillation cryogĆ©nique comprenant les Ć©tapes de:

  • a) refroidir un dĆ©bit d'alimentation comprenant de l'oxygĆØne, de l'azote et de l'argon et introduire ce dĆ©bit dans un appareil de distillation comprenant une colonne auxiliaire de sĆ©paration d'un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne et au moins deux autres colonnes ;
  • b) sĆ©parer ce dĆ©bit par distillation cryogĆ©nique dans l'appareil afin de former des fluides enrichis en oxygĆØne et en azote ;
  • c) envoyer le dĆ©bit contenant au moins de l'argon et de l'oxygĆØne d'une des autres colonnes Ć  la colonne auxiliaire, la colonne auxiliaire opĆ©rant substantiellement Ć  la mĆŖme pression que la colonne dont provient le dĆ©bit contenant au moins de l'argon et de l'oxygĆØne, cette pression Ć©tant entre 2 et 10 bars absolus ;
  • d) soutirer un dĆ©bit enrichi en oxygĆØne d'une colonne de l'appareil contenant au moins 95 % mol. d'oxygĆØne, Ć©ventuellement 98 % mol. d'oxygĆØne;
  • e) soutirer un dĆ©bit enrichi en argon de la colonne auxiliaire ;
    • ā€ƒā€ƒā€ƒcaractĆ©risĆ© en ce qu'au moins une partie du dĆ©bit enrichi en argon est rejetĆ©e Ć  l'atmosphĆØre et/ou sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants ou des Ć©changeurs rĆ©versibles et/ou au moins une partie du dĆ©bit enrichi en argon sert de produit, aprĆØs ĆŖtre mĆ©langĆ©e avec un gaz enrichi en azote de l'appareil et/ou un autre appareil.According to an object of the invention, a method is provided for producing a flow enriched in oxygen in a cryogenic distillation apparatus comprising the steps of:
  • a) cooling a feed flow comprising oxygen, nitrogen and argon and introducing this flow into a distillation apparatus comprising an auxiliary column for separating a flow containing at least argon, and oxygen and at least two other columns;
  • b) separating this flow rate by cryogenic distillation in the apparatus in order to form fluids enriched with oxygen and nitrogen;
  • c) send the flow containing at least argon and oxygen from one of the other columns to the auxiliary column, the auxiliary column operating at substantially the same pressure as the column from which the flow containing at least argon and oxygen, this pressure being between 2 and 10 bars absolute;
  • d) withdrawing a flow enriched in oxygen from a column of the apparatus containing at least 95% mol. oxygen, possibly 98% mol. oxygen;
  • e) withdrawing a flow enriched in argon from the auxiliary column;
    • characterized in that at least part of the flow enriched in argon is released to the atmosphere and / or is used to regenerate adsorbent beds or reversible exchangers and / or at least part of the flow enriched in argon is used as a product , after being mixed with a nitrogen-enriched gas from the device and / or another device.

    Par exemple le dĆ©bit enrichi en argon ou le dĆ©bit enrichi en argon mĆ©langĆ© avec un gaz enrichi en azote peut ĆŖtre envoyĆ© en amont de la machine de dĆ©tente d'une turbine Ć  gaz..For example the flow enriched in argon or the flow enriched in argon mixed with a gas enriched in nitrogen can be sent upstream of the expansion machine of a gas turbine..

    Le dĆ©bit enrichi en argon peut contenir entre 10 et 95 % mol. d'argon (ou entre 40 et 95% mol. d'argon) ,entre 2 et 40.% mol d'oxygĆØne et entre 2 et 40 % mol. d'azote.The flow enriched in argon can contain between 10 and 95 mol%. argon (or between 40 and 95% mol. argon), between 2 and 40.% mol of oxygen and between 2 and 40% mol. nitrogen.

    Optionnellement tout le dĆ©bit enrichi en argon est rejetĆ© Ć  l'atmosphĆØre et/ou sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants ou des Ć©changeurs rĆ©versibles et/ou est mĆ©langĆ© avec un gaz rĆ©siduaire de l'appareil et/ou un autre appareil et/ou envoyĆ© en amont de la machine de dĆ©tente d'une turbine Ć  gaz.Optionally all the flow enriched in argon is released to the atmosphere and / or used to regenerate adsorbent beds or reversible exchangers and / or is mixed with a waste gas from the appliance and / or another appliance and / or sent upstream of the gas turbine expansion machine.

    Dans ce cas, il peut tout de mĆŖme y avoir une production d'argon, par exemple en soutirant un dĆ©bit plus riche en argon de la colonne auxiliaire qui est le produit.In this case, there can still be a production of argon, for example by drawing off a richer flow of argon from the auxiliary column which is the product.

    Le dĆ©bit enrichi en argon qui est rejetĆ© Ć  l'atmosphĆØre et/ou qui sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants ou des Ć©changeurs rĆ©versibles et/ou qui est mĆ©langĆ© avec un gaz enrichi en azote de l'appareil et/ou un autre appareil et/ou qui est envoyĆ© en amont de la machine de dĆ©tente d'une turbine Ć  gaz peut constituer entre 0,3 et 2% de l'air, de prĆ©fĆ©rence entre 0,5 et 1% de l'air. Pour cette raison, il est prĆ©fĆ©rable de mĆ©langer le dĆ©bit enrichi en argon avec un gaz enrichi en azote contenant au moins 90 %mol. d'azote provenant par exemple de la colonne basse pression d'une double colonne et d'utiliser le mĆ©lange pour rĆ©gĆ©nĆ©rer des lits d'adsorbants ou des Ć©changeurs rĆ©versibles et/ou pour envoyer le mĆ©lange Ć  une turbine Ć  gaz et/ou de dĆ©tendre le mĆ©lange dans une turbine. Ainsi le mĆ©lange formĆ© comprend moins de 2 % mol. d'argon, de prĆ©fĆ©rence moins de 1% mol. d'argon.The flow enriched in argon which is released to the atmosphere and / or which is used to regenerate adsorbent beds or reversible exchangers and / or which is mixed with a gas enriched in nitrogen from the device and / or another device and / or which is sent upstream of the expansion machine of a gas turbine can constitute between 0.3 and 2% of the air, preferably between 0.5 and 1% of the air. For this reason, it is best to mix the flow enriched in argon with a gas enriched in nitrogen containing at least 90% mol. nitrogen coming for example from the low pressure column of a double column and use the mixture to regenerate adsorbent beds or reversible exchangers and / or to send the mixture to a gas turbine and / or to expand the mixture in a turbine. Thus the mixture formed comprises less than 2% mol. argon, preferably less than 1% mol. argon.

    La colonne basse pression peut opƩrer entre 2 et 10 bara, de prƩfƩrence au-dessus de 2,5 bara.The low pressure column can operate between 2 and 10 bara, preferably above 2.5 bara.

    Par exemple, l'appareil peut comprendre une colonne auxiliaire de sĆ©paration d'un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne et deux autres colonnes, dont une colonne haute pression et une colonne basse pression reliĆ©es thermiquement entre elles, la colonne auxiliaire Ć©tant alimentĆ©e Ć  partir de la colonne basse pression.For example, the apparatus may include an auxiliary separation column a flow containing at least argon and oxygen and two other columns, of which a high pressure column and a low pressure column thermally connected between them, the auxiliary column being supplied from the low pressure column.

    Alternativement l'appareil peut comprendre une colonne auxiliaire de sĆ©paration d'un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne et au moins trois autres colonnes, dont une colonne haute pression, une colonne pression intermĆ©diaire et une colonne basse pression reliĆ©es thermiquement entre elles, la colonne auxiliaire Ć©tant alimentĆ©e Ć  partir de la colonne basse pression ou la colonne pression intermĆ©diaire.Alternatively the apparatus may include an auxiliary separation column of a flow rate containing at least argon and oxygen and at least three others columns, including a high pressure column, an intermediate pressure column and a low pressure column thermally connected to each other, the auxiliary column being supplied from the low pressure column or the intermediate pressure column.

    Selon un autre objet de l'invention, il est prĆ©vu un procĆ©dĆ© intĆ©grĆ© de sĆ©paration d'air et de production d'Ć©nergie comprenant un procĆ©dĆ© selon l'une des revendications 1 Ć  12 dans lequel on envoie un gaz enrichi en azote de la colonne opĆ©rant prĆ©fĆ©rablement Ć  la pression la plus basse Ć  la turbine Ć  gaz ,aprĆØs une Ć©tape Ć©ventuelle de compression et, Ć©ventuellement on envoie un fluide enrichi en oxygĆØne d'une colonne de l'appareil Ć  un gazĆ©ifieur.According to another object of the invention, an integrated method of separation is provided. of air and energy production comprising a method according to one of claims 1 to 12 in which a nitrogen-enriched gas is sent from the operating column preferably at the lowest pressure at the gas turbine, after one step possible compression and, optionally, a fluid enriched with oxygen is sent from an appliance column to a gasifier.

    Selon un autre objet de l'invention, il est prĆ©vu un appareil de production d'oxygĆØne par distillation cryogĆ©nique comprenant :

  • a) une colonne auxiliaire et au moins deux autres colonnes ;
  • b) des moyens pour envoyer un dĆ©bit contenant de l'oxygĆØne, de l'azote et de l'argon Ć  une des autres colonnes ;
  • c) des moyens pour soutirer un dĆ©bit enrichi en oxygĆØne d'une des autres colonnes ;
  • d) des moyens pour soutirer un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne d'une des autres colonnes et des moyens pour envoyer ce dĆ©bit comme alimentation Ć  la colonne auxiliaire ;
  • e) des moyens pour soutirer un fluide enrichi en argon de la colonne auxiliaire ;
    • ā€ƒā€ƒā€ƒcaractĆ©risĆ© en ce que la colonne auxiliaire contient entre 1 et 99 plateaux thĆ©oriques et en ce que l'appareil comprend une turbine de dĆ©tente, des moyens pour amener un gaz de la colonne opĆ©rant Ć  la pression la plus basse, Ć  part la colonne auxiliaire, Ć  la turbine de dĆ©tente, ces moyens ne comprenant pas de moyen de compression et des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  l'atmosphĆØre et/ou des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  des lits d'adsorbants ou des Ć©changeurs rĆ©versibles pour les rĆ©gĆ©nĆ©rer et/ou des moyens pour mĆ©langer au moins une partie du fluide enrichi en argon avec un gaz rĆ©siduaire de l'appareil ou un autre appareil et/ou des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  une turbine Ć  gaz.According to another object of the invention, there is provided an apparatus for producing oxygen by cryogenic distillation comprising:
  • a) an auxiliary column and at least two other columns;
  • b) means for sending a flow containing oxygen, nitrogen and argon to one of the other columns;
  • c) means for withdrawing a flow enriched in oxygen from one of the other columns;
  • d) means for withdrawing a flow containing at least argon and oxygen from one of the other columns and means for sending this flow as feed to the auxiliary column;
  • e) means for withdrawing a fluid enriched in argon from the auxiliary column;
    • characterized in that the auxiliary column contains between 1 and 99 theoretical plates and in that the apparatus comprises an expansion turbine, means for bringing a gas from the column operating at the lowest pressure, apart from the auxiliary column, to the expansion turbine, these means not comprising compression means and means for sending at least a part of the fluid enriched in argon to the atmosphere and / or means for sending at least a part of the fluid enriched in argon to adsorbent beds or reversible exchangers to regenerate them and / or means for mixing at least part of the argon-enriched fluid with a waste gas from the apparatus or another apparatus and / or means for sending at least one part of the fluid enriched in argon at a gas turbine.

    De prƩfƩrence il n'y a pas de moyen de dƩtente entre la colonne alimentant la colonne auxiliaire et la colonne auxiliaire.Preferably there is no means of expansion between the column supplying the auxiliary column and the auxiliary column.

    Optionnellement la colonne auxiliaire contient entre 30 et 40 plateaux thƩoriques.Optionally the auxiliary column contains between 30 and 40 trays theoretical.

    Ainsi avec une colonne auxiliaire opĆ©rant Ć  la mĆŖme pression que la colonne basse pression, et de prĆ©fĆ©rence opĆ©rant Ć  une pression au-dessus de 2 bar, la sĆ©paration d'oxygĆØne et argon en cuve de la colonne basse pression est facilitĆ©e. Dans ce cas le fluide enrichi en argon soutirĆ© de la colonne auxiliaire n'est pas nĆ©cessairement un produit final de l'appareil mais peut servir Ć  refroidir les dĆ©bits rentrant dans les colonnes ou Ć  fournir des frigories par dĆ©tente.So with an auxiliary column operating at the same pressure as the column low pressure, and preferably operating at a pressure above 2 bar, the separation of oxygen and argon in the low pressure column tank is facilitated. In in this case the fluid enriched in argon withdrawn from the auxiliary column is not necessarily an end product of the device but can be used to cool flows re-entering the columns or supplying frigories by expansion.

    L'invention sera dƩcrite en plus de dƩtail en se rƩfƩrant aux figures.The invention will be described in more detail with reference to the figures.

    La figure 1 est un schĆ©ma d'un appareil de production d'oxygĆØne selon l'invention utilisant une double colonne.Figure 1 is a diagram of an oxygen production apparatus according to the invention using a double column.

    La figure 2 est un schĆ©ma d'un appareil de production d'oxygĆØne selon l'invention utilisant une triple colonne.Figure 2 is a diagram of an oxygen production apparatus according to the invention using a triple column.

    Dans la figure 1, un dĆ©bit d'air 1 de 1000Nm3/h est Ć©purĆ© par des lits d'adsorbants 4 est divisĆ© en deux. Le dĆ©bit 2 est surpressĆ© Ć  une pression plus Ć©levĆ©e, envoyĆ© dans l'Ć©changeur de chaleur 3 oĆ¹ il se refroidit en assurant la vaporisation de l'oxygĆØne liquide et ensuite Ć  une turbine hydraulique 5 oĆ¹ il sort sous forme au moins partiellement liquide. Ce liquide (ou mĆ©lange diphasique) 7 est envoyĆ© Ć  la colonne haute pression 9 opĆ©rant entre 14 et 15 bar et Ć©ventuellement en partie Ć  la colonne basse pression 11 opĆ©rant entre 4 et 6 bar (ou mĆŖme entre 2 et 10 bar), soit en envoyant une partie du liquide d'une capacitĆ© en amont de la colonne moyenne pression soit en soutirant un dĆ©bit ayant une composition similaire Ć  celle de l'air liquide de la colonne haute pression 9, comme montrĆ© Ć  la figure 1.In figure 1, an air flow 1 of 1000Nm3 / h is purified by beds adsorbent 4 is divided into two. The flow 2 is boosted at a higher pressure, sent to the heat exchanger 3 where it cools ensuring the vaporization of liquid oxygen and then to a hydraulic turbine 5 where it comes out at least partially liquid. This liquid (or two-phase mixture) 7 is sent to the column high pressure 9 operating between 14 and 15 bar and possibly partly at the column low pressure 11 operating between 4 and 6 bar (or even between 2 and 10 bar), either sending part of the capacity liquid upstream of the medium pressure column either by withdrawing a flow having a composition similar to that of the liquid air of the high pressure column 9, as shown in Figure 1.

    Le reste de l'air 13 Ơ 14,4 bara est envoyƩ Ơ la colonne haute pression 9.The rest of the air 13 to 14.4 bara is sent to the high pressure column 9.

    Eventuellement l'appareil peut comporter une turbine d'insufflation qui sert pendant le dƩmarrage ou une turbine d'azote basse pression 55. Optionally the device may include an insufflation turbine which serves during start-up or a low-pressure nitrogen turbine 55.

    Un dĆ©bit de liquide riche 15 est soutirĆ© de la colonne haute pression et envoyĆ© au sous refroidisseur 17, divisĆ© en deux et envoyĆ© en partie Ć  la colonne basse pression, aprĆØs dĆ©tente dans la vanne 21 et en partie au condenseur de tĆŖte 23 de la colonne auxiliaire 25 aprĆØs dĆ©tente dans la vanne 27. Le liquide riche au moins partiellement vaporisĆ© dans le condenseur de tĆŖte est envoyĆ© Ć  la colonne basse pression 11. Si la vaporisation est partielle, un dĆ©bit liquide et un dĆ©bit gazeux sont envoyĆ©s du condenseur Ć  la colonne basse pression.A flow of rich liquid 15 is withdrawn from the high pressure column and sent to the sub-cooler 17, divided in two and sent in part to the lower column pressure, after expansion in the valve 21 and in part at the head condenser 23 of the auxiliary column 25 after expansion in the valve 27. At least the rich liquid partially vaporized in the overhead condenser is sent to the lower column pressure 11. If the vaporization is partial, a liquid flow and a gas flow are sent from the condenser to the low pressure column.

    Un dĆ©bit d'azote gazeux 19 peut Ć©ventuellement ĆŖtre soutirĆ© de la tĆŖte de la colonne haute pression 9.A nitrogen gas flow 19 can optionally be withdrawn from the head of the high pressure column 9.

    La colonne auxiliaire est alimentĆ©e par un dĆ©bit gazeux 29 contenant entre 5 et 15 % mol. d'argon, de prĆ©fĆ©rence vers 7 % mol. d'argon. Le liquide de cuve 31 de la colonne auxiliaire est renvoyĆ© Ć  la colonne basse pression qui opĆØre substantiellement Ć  la mĆŖme pression que la colonne auxiliaire.The auxiliary column is supplied by a gas flow 29 containing between 5 and 15% mol. argon, preferably around 7 mol%. argon. The tank liquid 31 of the auxiliary column is returned to the low pressure column which operates substantially at the same pressure as the auxiliary column.

    Le colonne auxiliaire 25 peut alternativement ĆŖtre alimentĆ©e par un dĆ©bit liquide contenant entre 5 et 15 % mol. d'argon, de prĆ©fĆ©rence vers 7 % mol. d'argon. Dans ce cas la colonne 25 aura un rebouilleur de cuve, chauffe par un dĆ©bit gazeux tel que l'air ou de l'azote de la colonne haute pression 9.The auxiliary column 25 can alternatively be supplied with a liquid flow containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon. In this case column 25 will have a tank reboiler, heated by a gas flow such as air or nitrogen from the high pressure column 9.

    Un dĆ©bit d'air liquide 33 et un dĆ©bit de liquide pauvre 35 sont envoyĆ©s de la colonne haute pression 9 Ć  la colonne basse pression 11, aprĆØs avoir Ć©tĆ© sous-refroidis dans le sous refroidisseur 17 et dĆ©tendus dans des vannes.A liquid air flow 33 and a lean liquid flow 35 are sent from the high pressure column 9 to low pressure column 11, after having been sub-cooled in the sub-cooler 17 and expanded in valves.

    Un dĆ©bit d'oxygĆØne liquide 37 contenant 99,5% mol. d'oxygĆØne est soutirĆ© en cuve de la colonne basse pression, pressurisĆ© par une pompe 39 et vaporisĆ© dans l'Ć©changeur 3.A liquid oxygen flow 37 containing 99.5% mol. oxygen is drawn in low pressure column tank, pressurized by a pump 39 and vaporized in the exchanger 3.

    Un gaz enrichi en argon 49 constituant entre 0,5 et 1% de l'air envoyĆ© Ć  l'appareil et contenant entre 40 et 95 % mol. d'argon soutirĆ© de la tĆŖte de la colonne auxiliaire 25 est mĆ©langĆ© avec de l'azote rĆ©siduaire 47 de la tĆŖte de la colonne basse pression. Le mĆ©lange 53 se rĆ©chauffe dans le sous refroidisseur 17 puis se rĆ©chauffe dans l'Ć©changeur 3. Le mĆ©lange peut ensuite ĆŖtre rejetĆ© Ć  l'atmosphĆØre et/ou peut servir Ć  rĆ©gĆ©nĆ©rer les lits d'adsorbants 4 ou des Ć©changeurs rĆ©versibles et/ou envoyĆ© en amont de la machine de dĆ©tente 51 d'une turbine Ć  gaz aprĆØs une Ć©tape de compression.A gas enriched in argon 49 constituting between 0.5 and 1% of the air sent to the device and containing between 40 and 95% mol. argon withdrawn from the column head auxiliary 25 is mixed with residual nitrogen 47 from the head of the lower column pressure. The mixture 53 heats up in the sub-cooler 17 then heats up in the exchanger 3. The mixture can then be discharged into the atmosphere and / or can be used to regenerate the adsorbent beds 4 or reversible exchangers and / or sent in upstream of the expansion machine 51 of a gas turbine after a step of compression.

    Eventuellement auparavant une partie du mĆ©lange 53 peut ĆŖtre dĆ©tendue dans une turbine 55 (en pointillĆ©s).Possibly beforehand, part of the mixture 53 can be expanded in a turbine 55 (dotted line).

    Par rapport Ć  un systĆØme classique avec une colonne haute pression Ć  14,3 bara et une colonne basse pression Ć  4,8 bara mais sans colonne auxiliaire, le procĆ©dĆ© de la Figure 1 permet d'augmenter le rendement en oxygĆØne de 78% Ć  90%. Compared to a conventional system with a high pressure column at 14.3 bara and a low pressure column at 4.8 bara but without an auxiliary column, the process in Figure 1 increases the oxygen yield from 78% to 90%.

    Dans la Figure 2, une triple colonne est utilisĆ©e Ć  la place de la double colonne de la Figure 1. Un dĆ©bit d'air 1 est Ć©purĆ© par des lits d'adsorbants 4 est divisĆ© en deux. Le dĆ©bit 2 est surpressĆ© Ć  une pression plus Ć©levĆ©e, envoyĆ© dans l'Ć©changeur de chaleur 3 oĆ¹ il se refroidit en assurant la vaporisation de l'oxygĆØne liquide et ensuite Ć  une turbine hydraulique 5 oĆ¹ il sort sous forme au moins partiellement liquide. Ce liquide (ou mĆ©lange diphasique) 7 est envoyĆ© Ć  la colonne haute pression 9 opĆ©rant entre 14 et 15 bar et Ć©ventuellement en partie Ć  la colonne basse pression 11 opĆ©rant entre 4 et 6 bar et/ou Ć©ventuellement Ć  la colonne pression intermĆ©diaire 40 opĆ©rant entre 7 et 9 bar, soit en envoyant une partie du liquide d'une capacitĆ© en amont de la colonne moyenne pression soit en soutirant un dĆ©bit ayant une composition similaire Ć  celle de l'air liquide de la colonne haute pression 9, comme montrĆ© Ć  la figure 2.In Figure 2, a triple column is used in place of the double column of Figure 1. An air flow 1 is purified by adsorbent beds 4 is divided into two. Flow 2 is boosted to a higher pressure, sent to the heat exchanger heat 3 where it cools by ensuring the vaporization of liquid oxygen and then at a hydraulic turbine 5 where it exits in at least partially liquid form. This liquid (or two-phase mixture) 7 is sent to the high pressure column 9 operating between 14 and 15 bar and possibly partly at the low pressure column 11 operating between 4 and 6 bar and / or possibly at the intermediate pressure column 40 operating between 7 and 9 bar, either by sending part of the liquid of a capacity upstream of the middle column pressure either by withdrawing a flow having a composition similar to that of liquid air of the high pressure column 9, as shown in FIG. 2.

    Le reste de l'air 13 Ơ 14,4 bara est envoyƩ Ơ la colonne haute pression 9.The rest of the air 13 to 14.4 bara is sent to the high pressure column 9.

    Eventuellement l'appareil peut comporter une turbine d'insufflation qui sert pendant le dƩmarrage ou une turbine d'azote basse pression 55.Optionally the device may include an insufflation turbine which serves during start-up or a low-pressure nitrogen turbine 55.

    Un dĆ©bit de liquide riche 15 est soutirĆ© de la colonne haute pression et envoyĆ© au sous refroidisseur 17, divisĆ© en deux et envoyĆ© en partie au milieu de la colonne opĆ©rant Ć  pression intermĆ©diaire 40, aprĆØs dĆ©tente dans la vanne 21 et en partie au condenseur de tĆŖte 23 de la colonne auxiliaire 25 aprĆØs dĆ©tente dans la vanne 27. Le liquide riche au moins partiellement vaporisĆ© dans le condenseur de tĆŖte est envoyĆ© Ć  la colonne basse pression 11. Si la vaporisation est partielle, un dĆ©bit liquide et un dĆ©bit gazeux sont envoyĆ©s du condenseur Ć  la colonne basse pression.A flow of rich liquid 15 is withdrawn from the high pressure column and sent to the sub-cooler 17, divided in two and sent partly to the middle of the column operating at intermediate pressure 40, after expansion in valve 21 and partly at head condenser 23 of the auxiliary column 25 after expansion in the valve 27. The at least partially vaporized rich liquid in the overhead condenser is sent to the low pressure column 11. If the vaporization is partial, a liquid flow and a flow gases are sent from the condenser to the low pressure column.

    Un dĆ©bit d'azote gazeux 19 peut Ć©ventuellement ĆŖtre soutirĆ© de la tĆŖte de la colonne haute pression 9.A nitrogen gas flow 19 can optionally be withdrawn from the head of the high pressure column 9.

    La colonne auxiliaire est alimentĆ©e par une partie d'un dĆ©bit gazeux 29 contenant entre 5 et 15 % mol. d'argon, de prĆ©fĆ©rence vers 7 % mol. d'argon. Le liquide de cuve 31 de la colonne auxiliaire est renvoyĆ© Ć  la colonne basse pression qui opĆØre substantiellement Ć  la mĆŖme pression que la colonne auxiliaire.The auxiliary column is supplied with part of a gas flow 29 containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon. The liquid tank 31 of the auxiliary column is returned to the low pressure column which operates at substantially the same pressure as the auxiliary column.

    Le colonne auxiliaire 25 peut alternativement ĆŖtre alimentĆ©e par un dĆ©bit liquide contenant entre 5 et 15 % mol. d'argon, de prĆ©fĆ©rence vers 7 % mol. d'argon. Dans ce cas la colonne 25 aura un rebouilleur de cuve, chauffe par un dĆ©bit gazeux tel que l'air ou de l'azote de la colonne haute pression 9.The auxiliary column 25 can alternatively be supplied with a liquid flow containing between 5 and 15 mol%. argon, preferably around 7 mol%. argon. In this case column 25 will have a tank reboiler, heated by a gas flow such as air or nitrogen from the high pressure column 9.

    Le reste du dĆ©bit gazeux 29 sert Ć  chauffer le rebouilleur de cuve 41 de la colonne 40 et aprĆØs condensation est renvoyĆ© Ć  la colonne basse pression avec le dĆ©bit 31.The rest of the gas flow 29 is used to heat the tank reboiler 41 of the column 40 and after condensation is returned to the low pressure column with the flow rate 31.

    Le liquide de cuve 43 de la colonne 40 est envoyĆ© en partie directement Ć  la colonne basse pression et en partie au condenseur de tĆŖte de la colonne 40 oĆ¹ il se vaporise au moins partiellement avant d'ĆŖtre envoyĆ© Ć  la colonne basse pression Ć  son tour.The tank liquid 43 of the column 40 is partly sent directly to the low pressure column and partly to the condenser at the top of column 40 where it at least partially vaporizes before being sent to the low pressure column at its tower.

    Le liquide de tĆŖte 47 de la colonne 40 est sousrefroidi dans l'Ć©changeur 17, dĆ©tendu, mĆ©langĆ© avec le dĆ©bit dĆ©tendu 35 et envoyĆ© en tĆŖte de la colonne basse pression.The overhead liquid 47 of the column 40 is sub-cooled in the exchanger 17, expanded, mixed with expanded flow 35 and sent to the top of the lower column pressure.

    Un dĆ©bit d'air liquide 33 et un dĆ©bit de liquide pauvre 35 sont envoyĆ©s de la colonne haute pression 9 Ć  la colonne basse pression 11, aprĆØs avoir Ć©tĆ© sous-refroidis dans le sous refroidisseur 17 et dĆ©tendus dans des vannes.A liquid air flow 33 and a lean liquid flow 35 are sent from the high pressure column 9 to low pressure column 11, after having been sub-cooled in the sub-cooler 17 and expanded in valves.

    Un dĆ©bit d'oxygĆØne liquide 37 contenant 99,5% mol. d'oxygĆØne est soutirĆ© en cuve de la colonne basse pression, pressurisĆ© par une pompe 39 et vaporisĆ© dans l'Ć©changeur 3.A liquid oxygen flow 37 containing 99.5% mol. oxygen is drawn in low pressure column tank, pressurized by a pump 39 and vaporized in the exchanger 3.

    Un gaz enrichi en argon 49 constituant entre 0,5 et 1% de l'air envoyĆ© Ć  l'appareil et contenant entre 40 et 95 % mol. d'argon soutirĆ© de la tĆŖte de la colonne auxiliaire 25 est mĆ©langĆ© avec de l'azote rĆ©siduaire 47 de la tĆŖte de la colonne basse pression. Le mĆ©lange 53 se rĆ©chauffe dans le sous refroidisseur 17 puis se rĆ©chauffe dans l'Ć©changeur 3. Le mĆ©lange peut ensuite ĆŖtre rejetĆ© Ć  l'atmosphĆØre et/ou peut servir Ć  rĆ©gĆ©nĆ©rer les lits d'adsorbants 4 ou des Ć©changeurs rĆ©versibles et/ou envoyĆ© en amont de la machine de dĆ©tente 51 d'une turbine Ć  gaz aprĆØs une Ć©tape de compression Ć©ventuelle.A gas enriched in argon 49 constituting between 0.5 and 1% of the air sent to the device and containing between 40 and 95% mol. argon withdrawn from the column head auxiliary 25 is mixed with residual nitrogen 47 from the head of the lower column pressure. The mixture 53 heats up in the sub-cooler 17 then heats up in the exchanger 3. The mixture can then be discharged into the atmosphere and / or can be used to regenerate the adsorbent beds 4 or reversible exchangers and / or sent in upstream of the expansion machine 51 of a gas turbine after a step of possible compression.

    Eventuellement auparavant une partie du mĆ©lange 53 peut ĆŖtre dĆ©tendue dans une turbine 55 (en pointillĆ©s).Possibly beforehand, part of the mixture 53 can be expanded in a turbine 55 (dotted line).

    Le procĆ©dĆ© selon l'invention prĆ©sente un intĆ©rĆŖt particulier dans le cas dans lequel l'azote de la colonne basse pression est valorisĆ©, par exemple en l'envoyant Ć  une machine de dĆ©tente 51 d'une turbine Ć  gaz. Dans ce cas au moins une partie de l'air 1 peut provenir du compresseur 53 de la turbine Ć  gaz et l'oxygĆØne produit par l'appareil de distillation peut servir Ć  la gazĆ©ification nĆ©cessaire pour produire le carburant de la turbine Ć  gaz.The method according to the invention is of particular interest in the case in which the nitrogen in the low pressure column is valued, for example by sending it to an expansion machine 51 of a gas turbine. In this case at least part of the air 1 can come from compressor 53 of the gas turbine and the oxygen produced by the device distillation can be used for the gasification necessary to produce the fuel for the gas turbine.

    Claims (16)

    ProcĆ©dĆ© de production d'un dĆ©bit enrichi en oxygĆØne dans un appareil de distillation cryogĆ©nique comprenant les Ć©tapes de : a) refroidir un dĆ©bit d'alimentation (1) comprenant de l'oxygĆØne, de l'azote et de l'argon et introduire ce dĆ©bit dans un appareil de distillation comprenant une colonne auxiliaire (25) de sĆ©paration d'un dĆ©bit (29) contenant au moins de l'argon et de l'oxygĆØne et au moins deux autres colonnes (9,11) ; b) sĆ©parer ce dĆ©bit par distillation cryogĆ©nique dans l'appareil afin de former des fluides enrichis en oxygĆØne et en azote (15,33,35) ; c) envoyer le dĆ©bit contenant au moins de l'argon et de l'oxygĆØne d'une des autres colonnes Ć  la colonne auxiliaire, la colonne auxiliaire opĆ©rant substantiellement Ć  la mĆŖme pression que la colonne (11) dont provient le dĆ©bit contenant au moins de l'argon et de l'oxygĆØne, cette pression Ć©tant entre 2 et 10 bars absolus ; d) soutirer un dĆ©bit enrichi en oxygĆØne (37), contenant au moins 95 %mol. d'oxygĆØne d'une colonne de l'appareil ; e) soutirer un dĆ©bit enrichi en argon (49)de la colonne auxiliaire ; ā€ƒā€ƒā€ƒcaractĆ©risĆ© en ce qu'au moins une partie du dĆ©bit enrichi en argon (49) est rejetĆ©e Ć  l'atmosphĆØre et/ou sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants (4) ou des Ć©changeurs rĆ©versibles et/ou au moins une partie du dĆ©bit enrichi en argon sert de produit aprĆØs s'ĆŖtre mĆ©langĆ©e avec un gaz enrichi en azote (47) de l'appareil et/ou un autre appareil.Method for producing a flow enriched with oxygen in a cryogenic distillation apparatus comprising the steps of: a) cooling a feed flow (1) comprising oxygen, nitrogen and argon and introducing this flow into a distillation apparatus comprising an auxiliary column (25) for separating a flow (29 ) containing at least argon and oxygen and at least two other columns (9,11); b) separating this flow rate by cryogenic distillation in the apparatus in order to form fluids enriched with oxygen and nitrogen (15,33,35); c) sending the flow containing at least argon and oxygen from one of the other columns to the auxiliary column, the auxiliary column operating at substantially the same pressure as the column (11) from which the flow containing at least argon and oxygen, this pressure being between 2 and 10 bars absolute; d) withdrawing a flow enriched in oxygen (37), containing at least 95 mol%. oxygen from an apparatus column; e) withdrawing a flow enriched in argon (49) from the auxiliary column; characterized in that at least part of the flow enriched in argon (49) is released to the atmosphere and / or is used to regenerate adsorbent beds (4) or reversible exchangers and / or at least part of the flow enriched in argon serves as a product after mixing with a nitrogen-enriched gas (47) from the apparatus and / or another apparatus. ProcĆ©dĆ© selon la revendication 1 dans lequel le dĆ©bit enrichi en argon (49) contient entre 10 et 95 % mol. d'argon.The method of claim 1 wherein the flow enriched in argon (49) contains between 10 and 95% mol. argon. ProcĆ©dĆ© selon la revendication 2 dans lequel le dĆ©bit enrichi en argon (49)contient entre 40 et 95 % mol. d'argon.The method of claim 2 wherein the flow enriched in argon (49) contains between 40 and 95% mol. argon. ProcĆ©dĆ© selon la revendication 1 ou 2 dans lequel le dĆ©bit enrichi en argon (49) contient entre 2 et 40 % mol. d'oxygĆØne.The method of claim 1 or 2 wherein the flow enriched in argon (49) contains between 2 and 40% mol. oxygen. ProcĆ©dĆ© selon l'une des revendications prĆ©cĆ©dentes dans lequel au moins une partie du dĆ©bit enrichi en argon (49) est rejetĆ©e Ć  l'atmosphĆØre, Ć©ventuellement aprĆØs l'avoir mĆ©langĆ© avec un gaz enrichi en azote de l'appareil.Method according to one of the preceding claims, in which at least one part of the flow enriched in argon (49) is released to the atmosphere, possibly after having mixed it with a nitrogen-enriched gas from the appliance. ProcĆ©dĆ© selon l'une des revendications prĆ©cĆ©dentes dans lequel au moins une partie du dĆ©bit enrichi en argon (49) sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants (4) ou des Ć©changeurs rĆ©versibles, Ć©ventuellement aprĆØs l'avoir mĆ©langĆ© avec un gaz enrichi en azote de l'appareil. Method according to one of the preceding claims, in which at least one part of the flow enriched in argon (49) is used to regenerate adsorbent beds (4) or reversible exchangers, possibly after having mixed it with a gas enriched in device nitrogen. ProcĆ©dĆ© selon l'une des revendications prĆ©cĆ©dentes dans lequel au moins une partie du dĆ©bit enrichi en argon (49) envoyĆ©e en amont de la machine de dĆ©tente (51) d'une turbine Ć  gaz,. Ć©ventuellement aprĆØs l'avoir mĆ©langĆ© avec un gaz enrichi en azote de l'appareil.Method according to one of the preceding claims, in which at least one part of the flow enriched with argon (49) sent upstream of the expansion machine (51) of a gas turbine ,. possibly after mixing it with a nitrogen-enriched gas of the device. ProcĆ©dĆ© selon l'une des revendications 1 Ć  7 dans lequel tout le dĆ©bit enrichi en argon (49) est rejetĆ© Ć  l'atmosphĆØre et/ou sert Ć  rĆ©gĆ©nĆ©rer des lits d'adsorbants ou des Ć©changeurs rĆ©versibles et/ou sert de produit final Ć©ventuellement aprĆØs s'ĆŖtre mĆ©langĆ© avec un gaz enrichi en azote de l'appareil.Method according to one of Claims 1 to 7, in which all the flow enriched in argon (49) is released to the atmosphere and / or is used to regenerate adsorbent beds or reversible exchangers and / or serves as final product possibly after mixing with a nitrogen-enriched gas from the device. ProcĆ©dĆ© selon l'une des revendications 1 Ć  8 dans lequel il y a production d'un fluide enrichi en argon comme produit final.Method according to one of claims 1 to 8 wherein there is production of a fluid enriched with argon as final product. ProcĆ©dĆ© selon l'une des revendications prĆ©cĆ©dentes dans lequel au moins une partie du dĆ©bit (49) enrichi en argon est envoyĆ©e Ć  une turbine de dĆ©tente (53) ou une vanne de dĆ©tente, Ć©ventuellement aprĆØs avoir Ć©tĆ© mĆ©langĆ© avec un dĆ©bit gazeux enrichi en azote.Method according to one of the preceding claims, in which at least one part of the flow (49) enriched in argon is sent to an expansion turbine (53) or a expansion valve, possibly after being mixed with an enriched gas flow in nitrogen. ProcĆ©dĆ© selon l'une des revendications prĆ©cĆ©dentes dans lequel l'appareil comprend une colonne auxiliaire (25) de sĆ©paration d'un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne et deux autres colonnes, dont une colonne haute pression (9) et une colonne basse pression (11) reliĆ©es thermiquement entre elles, la colonne auxiliaire Ć©tant alimentĆ©e Ć  partir de la colonne basse pression.Method according to one of the preceding claims, in which the apparatus comprises an auxiliary column (25) for separating a flow containing at least argon and oxygen and two other columns, including a high pressure column (9) and a low pressure column (11) thermally connected to each other, the auxiliary column being supplied from the low pressure column. ProcĆ©dĆ© selon l'une des revendications 1 Ć  10 dans lequel l'appareil comprend une colonne auxiliaire (25) de sĆ©paration d'un dĆ©bit contenant au moins de l'argon et de l'oxygĆØne et au moins trois autres colonnes, dont une colonne haute pression (9), une colonne pression intermĆ©diaire (40) et une colonne basse pression (11) reliĆ©es thermiquement entre elles, la colonne auxiliaire Ć©tant alimentĆ©e Ć  partir de la colonne basse pression ou la colonne pression intermĆ©diaire.Method according to one of claims 1 to 10 wherein the apparatus comprises an auxiliary column (25) for separating a flow containing at least argon and oxygen and at least three other columns, including a high pressure column (9), a intermediate pressure column (40) and a low pressure column (11) connected thermally between them, the auxiliary column being supplied from the column low pressure or the intermediate pressure column. ProcĆ©dĆ© intĆ©grĆ© de sĆ©paration d'air et de production d'Ć©nergie comprenant un procĆ©dĆ© selon la revendication 7 dans lequel on envoie un fluide enrichi en oxygĆØne d'une colonne de l'appareil Ć  un gazĆ©ifieur ou au moins une partie de l'air destinĆ© Ć  l'appareil de distillation provient d'un compresseur (53) de la turbine Ć  gaz.Integrated method of air separation and energy production comprising a process according to claim 7, in which an oxygen-enriched fluid is sent from an appliance column to a gasifier or at least part of the air intended for the distillation apparatus comes from a compressor (53) of the gas turbine. Appareil de production d'oxygĆØne par distillation cryogĆ©nique comprenant : a) une colonne auxiliaire (25) et au moins deux autres colonnes(9,11); b) des moyens pour envoyer un dĆ©bit (1) contenant de l'oxygĆØne, de l'azote et de l'argon Ć  une des autres colonnes ; c) des moyens pour soutirer un dĆ©bit enrichi en oxygĆØne (37) d'une des autres colonnes ; d) des moyens pour soutirer un dĆ©bit (29)contenant au moins de l'argon et de l'oxygĆØne d'une des autres colonnes et des moyens pour envoyer ce dĆ©bit comme alimentation Ć  la colonne auxiliaire (25) ; e) des moyens pour soutirer un fluide enrichi en argon de la colonne auxiliaire ; caractĆ©risĆ© en ce que la colonne auxiliaire contient entre 1 et 99 plateaux thĆ©oriques et il y a une turbine de dĆ©tente (53), des moyens pour amener .un gaz (53) de la colonne opĆ©rant Ć  la pression la plus basse (11), Ć  part la colonne auxiliaire,Ć  la turbine de dĆ©tente, ces moyens ne comprenant pas de moyen de compression et des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  l'atmosphĆØre et/ou des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  des lits d'adsorbants ou des Ć©changeurs rĆ©versibles pour les rĆ©gĆ©nĆ©rer et/ou des moyens pour mĆ©langer au moins une partie du fluide enrichi en argon avec un gaz enrichi en azote (47) de l'appareil ou d'un autre appareil et/ou des moyens pour envoyer au moins une partie du fluide enrichi en argon Ć  une turbine Ć  gaz.Apparatus for producing oxygen by cryogenic distillation comprising: a) an auxiliary column (25) and at least two other columns (9,11); b) means for sending a flow (1) containing oxygen, nitrogen and argon to one of the other columns; c) means for withdrawing a flow enriched in oxygen (37) from one of the other columns; d) means for withdrawing a flow (29) containing at least argon and oxygen from one of the other columns and means for sending this flow as feed to the auxiliary column (25); e) means for withdrawing a fluid enriched in argon from the auxiliary column; characterized in that the auxiliary column contains between 1 and 99 theoretical plates and there is an expansion turbine (53), means for bringing a gas (53) from the column operating at the lowest pressure (11), apart from the auxiliary column, to the expansion turbine, these means not comprising compression means and means for sending at least part of the fluid enriched in argon to the atmosphere and / or means for sending at least part fluid enriched in argon with adsorbent beds or reversible exchangers to regenerate them and / or means for mixing at least part of the fluid enriched in argon with a nitrogen enriched gas (47) of the apparatus or another device and / or means for sending at least part of the fluid enriched in argon to a gas turbine. Appareil selon la revendication 14 dans lequel il n'y a pas de moyen de dĆ©tente entre la colonne (11) alimentant la colonne auxiliaire et la colonne auxiliaire (25).Apparatus according to claim 14 in which there is no expansion means between the column (11) supplying the auxiliary column and the auxiliary column (25). Appareil selon la revendication 14 ou 15 comprenant des moyens pour envoyer tout le fluide enrichi en argon Ć  l'atmosphĆØre ou des moyens pour mĆ©langer tout le fluide enrichi en argon avec un gaz enrichi de l'appareil ou un autre appareil.Apparatus according to claim 14 or 15 comprising means for sending any fluid enriched with argon to the atmosphere or means for mixing all the fluid enriched in argon with a gas enriched with the device or another device.
    EP01400749A 2000-04-04 2001-03-22 Process and apparatus for the production of oxygen enriched fluid by cryogenic distillation Expired - Lifetime EP1143216B1 (en)

    Applications Claiming Priority (2)

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    FR0004284 2000-04-04
    FR0004284A FR2807150B1 (en) 2000-04-04 2000-04-04 PROCESS AND APPARATUS FOR PRODUCING OXYGEN ENRICHED FLUID BY CRYOGENIC DISTILLATION

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    JP2001349669A (en) 2001-12-21
    ATE548619T1 (en) 2012-03-15
    ES2382453T3 (en) 2012-06-08
    FR2807150A1 (en) 2001-10-05
    FR2807150B1 (en) 2002-10-18
    EP1143216B1 (en) 2012-03-07
    US20010052243A1 (en) 2001-12-20
    US6434973B2 (en) 2002-08-20

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