EP1189003A1 - Process and apparatus for air separation by cryogenic distillation - Google Patents

Process and apparatus for air separation by cryogenic distillation Download PDF

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Publication number
EP1189003A1
EP1189003A1 EP01402310A EP01402310A EP1189003A1 EP 1189003 A1 EP1189003 A1 EP 1189003A1 EP 01402310 A EP01402310 A EP 01402310A EP 01402310 A EP01402310 A EP 01402310A EP 1189003 A1 EP1189003 A1 EP 1189003A1
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EP
European Patent Office
Prior art keywords
pressure column
column
enriched
flow
oxygen
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EP01402310A
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German (de)
French (fr)
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EP1189003B1 (en
Inventor
Benoit Davidian
Francois De Bussy
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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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Publication of EP1189003A1 publication Critical patent/EP1189003A1/en
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04436—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • 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

Definitions

  • the present invention relates to a method and an installation for air separation by cryogenic distillation.
  • it relates to a process using three separation columns operating at high pressure, low pressure and an intermediate pressure between high and low pressures.
  • An object of the invention is to reduce the energy consumption of the process separation with respect to the methods of the prior art.
  • Another object of the invention is to produce oxygen with a purity of at least minus 95% mol., or even at least 98% mol. with improved performance.
  • Figure 1 shows a typical process with a low pressure column 103 operating at 1.3 bara making oxygen at 99.5% mol. with a 92% yield.
  • a flow of 1000 Nm 3 / h of air 1 at around 5 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara .
  • the flow 17 is sent to the tank of the high pressure column 101 and flow 3 liquefied in the exchanger 100 is expanded in a turbine 6 producing a flow at least partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the low pressure column 103.
  • a liquid air flow 12 is withdrawn from the high pressure column 101, cooled in the subcooler 83, expanded and sent to the low pressure column 103.
  • a residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow 31 of 193 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column 103, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.
  • a flow rate of 200 Nm 3 / h of nitrogen gas 33 is withdrawn from the head of the high pressure column 101 and is partially heated in the exchanger 100. At an intermediate temperature, part of the gas is expanded in a turbine 35 before d 'be mixed with waste gas 72.
  • a flow of 1000 Nm 3 / h of air 1 at around 14.3 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara.
  • the two flows 3.17 cool by passing through an exchanger 100.
  • the flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine 6 producing an at least partially liquid flow at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the sub-cooler 83 before being relaxed and sent to an intermediate level of the low pressure column 103.
  • a liquid air flow 12 is withdrawn from the high pressure column 101, cooled in the subcooler 83, expanded and sent to the low pressure column 103.
  • a residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow 31 of 164 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.
  • the inventors of the present application have discovered that even without using an argon separation column, the purification of oxygen in the bottom of the column low pressure remains satisfactory for the production of high purity oxygen.
  • a separation installation air by cryogenic distillation comprising a high pressure column, a column at intermediate pressure having a tank reboiler and a low pressure column, the high pressure column and the low pressure column being thermally connected between them, means for sending at least a mixture of oxygen, nitrogen and argon at least to the high pressure column, means for sending a flow enriched in oxygen from the high pressure column to the intermediate pressure column, means for sending an oxygen-enriched fluid and / or a nitrogen-enriched fluid from the intermediate pressure column to the low pressure column, means for send a fluid from the low pressure column to the column reboiler of the column to intermediate pressure, means for withdrawing a nitrogen-enriched fluid and a fluid enriched in oxygen from the low pressure column, characterized in that it does not includes no means for enriching argon with a fluid containing between 3 and 20% mol. argon other than high pressure, low pressure and pressure columns intermediate.
  • the fluid sent to the reboiler is withdrawn from the column low pressure at a level lower than the level of introduction of a fluid enriched in oxygen from the intermediate pressure column.
  • the intermediate pressure column has an overhead condenser.
  • Fluids called 'enriched in oxygen' or 'enriched in nitrogen' are enriched in these components compared to air.
  • the device operates with a low column pressure at 1.3 bara and in the case of Figure 4, the device operates with a low pressure column at 4.8 bara.
  • FIG. 3 The installation of Figure 3 includes a high pressure column 101 operating at 5 bara, an intermediate pressure column 102 operating at 2.7 bara and a low pressure column 103 operating at 1.3 bara. Part of the overhead nitrogen gas of the high pressure column is used to heat the bottom column reboiler pressure but other means of heating can be envisaged, such as double reboiler systems, one of which is heated by air.
  • a flow of 1000 Nm 3 / h of air 1 at around 5 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara .
  • the two flows 3.17 cool by passing through an exchanger 100.
  • the flow 17 is sent to the tank of the high pressure column 101 without having been expanded or compressed and the liquid flow 3 is expanded in a turbine 6 producing a flow at less partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured fillings of wavy-cross type. Liquid can be sent to another column level and the column can also receive a flow of gaseous air or liquid.
  • This liquid is separated into a second oxygen-enriched liquid 20 and a liquid enriched in nitrogen 25.
  • the liquid 25 cools in the subcooler 83, before to be relaxed and sent to the head of the low pressure column 103, after being mixed with a lean liquid flow 15 from the head of the high pressure column 101 which has also been cooled in the subcooler 83 and expanded in a valve.
  • the tank liquid 20 of the intermediate pressure column is divided into of them. A part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 22 of the intermediate pressure column where it vaporizes at least partially before to be sent to the low pressure column 103.
  • a liquid air flow 12 is withdrawn from the high pressure column, cooled in the subcooler 83, expanded and sent to the low pressure column 103.
  • the tank reboiler 24 of the intermediate pressure column 102 is heated by means of a gas flow enriched in argon 233 containing approximately 5 to 15% mol., preferably between 8 and 10% mol. argon from the lower column pressure 103. This flow condenses at least partially in the reboiler 24 before being returned to the low pressure column 103
  • a residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow 31 of 203 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column 103, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.
  • a flow 33 of 200 Nm 3 / h of nitrogen gas is drawn off at the head of the high pressure column 101 and is partially heated in the exchanger 100. At an intermediate temperature, part of the gas is expanded in a turbine 35 before be mixed with the waste gas 72. The rest of the nitrogen continues to heat up and constitutes a product of the apparatus.
  • Liquid products can be drawn from the appliance, but the appliance does not produces no argon-rich fluid.
  • FIG. 4 The installation of Figure 4 includes a high pressure column 101 operating at 14.3 bara, an intermediate pressure column 102 operating at 8.5 bara and a low pressure column 103 operating at 4.8 bara. All the nitrogen gas overhead high pressure column is used to heat the bottom column tank reboiler pressure but other means of heating can be envisaged, such as double reboiler systems, one of which is heated by air.
  • a flow of 1000 Nm 3 / h of air 1 at around 14.3 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara.
  • the two flows 3.17 cool by passing through an exchanger 100.
  • the flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine producing an at least partially liquid flow at its outlet, the fluid or mixture of fluids leaving the turbine being sent at least in part to the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured fillings of wavy-cross type. Liquid can be sent to another column level and the column can also receive a flow of gaseous air or liquid.
  • This liquid is separated into a second oxygen-enriched liquid 20 and a liquid enriched in nitrogen 25.
  • the liquid 25 cools in the subcooler 83, before to be relaxed and sent to the head of the low pressure column 103, after being mixed with a lean liquid flow 15 from the head of the high pressure column 101 which has also been cooled in the subcooler 83 and expanded in a valve.
  • the tank liquid 20 of the intermediate pressure column is divided into of them. A part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 22 of the intermediate pressure column where it vaporizes at least partially before to be sent to the low pressure column 103.
  • a liquid air flow 12 is withdrawn from the high pressure column, cooled in the subcooler 83, expanded and sent to the low pressure column.
  • the tank reboiler 24 of the intermediate pressure column 102 is heated by means of a gas flow enriched in argon 233 containing approximately 5 to 15% mol., preferably 8 to 10% mol. argon from the low pressure column 103. This flow condenses at least partially in the reboiler 24 before being returned to low pressure column 103.
  • a residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow 31 of 177 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.
  • the appliance can receive all or part of its supply air from a compressor of a gas turbine, the residual nitrogen from the appliance being returned to the gas turbine.
  • Figure 1 process Figure 3 process (invention) High pressure column pressure 5 bara 5 bara Low pressure column pressure 1.3 bara 1.3 bara Intermediate pressure column pressure 2.7 bara Total treated air flow 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.5% O2 99.5% O2 Oxygen production, counted pure 193 Nm 3 / h 203 Nm 3 / h High pressure nitrogen gas production 200 Nm 3 / h 200 Nm 3 / h Oxygen extraction efficiency 92% 97% Separation energy Base: 100 95 Figure 2 process Figure 4 process (invention) High pressure column pressure 14.3 bara 14.3 bara Low pressure column pressure 4.8 bara 4.8 bara Intermediate pressure column pressure 8.5 bara Total air flow 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
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  • Separation By Low-Temperature Treatments (AREA)

Abstract

The plant, comprising a high-pressure column (101), an intermediate pressure column (102) with a boiler (24), and a low pressure column (103), has no means for argon enrichment of a fluid containing between 3 and 20 per cent/mol of argon other than the three aforementioned columns. During operation a mixture of at least oxygen, nitrogen and argon is fed into the high-pressure column, where it is separated into oxygen-rich and nitrogen-rich fractions. Part of both fractions is fed to the low-pressure column, which operates at preferably above 4 bars, and the gas from the lower part of this column is sent to the boiler in the intermediate column and at least partially condensed before being returned to the low-pressure column. Oxygen-rich and nitrogen-rich fluids (31, 72) are then drawn from the low-pressure column; at least part of the nitrogen-rich fluid is at least partly condensed in a vaporizer/condenser linked to the low-pressure column, and at least part of the partly condensed fluid is fed back to the high-pressure column, but no fluid containing 3-20 per cent/mol of argon is enriched with argon in any column apart from the high-pressure, low-pressure or intermediate-pressure columns. An Independent claim is also included for the instillation for the cryogenic air separating procedure.

Description

La présente invention est relative à un procédé et une installation de séparation d'air par distillation cryogénique. En particulier elle conceme un procédé utilisant trois colonnes de séparation opérant à une haute pression, une basse pression et une pression intermédiaire entre les haute et basse pressions.The present invention relates to a method and an installation for air separation by cryogenic distillation. In particular it relates to a process using three separation columns operating at high pressure, low pressure and an intermediate pressure between high and low pressures.

Il est connu de EP-A-0538118 d'utiliser un procédé de ce genre pour séparer de l'air, la colonne à pression intermédiaire ayant un rebouilleur de cuve chauffé par de l'azote de la colonne haute pression, réduisant ainsi le chauffage du rebouilleur de cuve de la colonne basse pression.It is known from EP-A-0538118 to use a process of this kind to separate air, the intermediate pressure column having a tank reboiler heated by nitrogen from the high pressure column, thereby reducing reboiler heating by low pressure column tank.

Un but de l'invention est de réduire la consommation en énergie du procédé de séparation par rapport aux procédés de l'art antérieur.An object of the invention is to reduce the energy consumption of the process separation with respect to the methods of the prior art.

Un autre but de l'invention est de produire de l'oxygène avec une pureté d'au moins 95 % mol., voire au moins 98 % mol. avec un rendement amélioré.Another object of the invention is to produce oxygen with a purity of at least minus 95% mol., or even at least 98% mol. with improved performance.

La Figure 1 montre un procédé classique avec une colonne basse pression 103 opérant à 1,3 bara permettant de faire de l'oxygène à 99,5 % mol. avec un rendement de 92 %.Figure 1 shows a typical process with a low pressure column 103 operating at 1.3 bara making oxygen at 99.5% mol. with a 92% yield.

Un débit de 1000 Nm3/h d'air 1 à environ 5 bara est divisé en deux pour former un premier débit 17 et un deuxième débit 3 qui est surpressé dans un surpresseur 5 à une pression plus élevée de l'ordre de 75 bara.A flow of 1000 Nm 3 / h of air 1 at around 5 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara .

Les deux débits 3,17 se refroidissent en traversant un échangeur 100. Le débit 17 est envoyé en cuve de la colonne haute pression 101 et le débit 3 liquéfié dans l'échangeur 100 est détendu dans une turbine 6 produisant un débit au moins partiellement liquide à sa sortie, le fluide ou mélange de fluides sortant de la turbine 6 étant envoyé au moins en partie à la colonne haute pression 101.The two flows 3.17 cool by passing through an exchanger 100. The flow 17 is sent to the tank of the high pressure column 101 and flow 3 liquefied in the exchanger 100 is expanded in a turbine 6 producing a flow at least partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.

Un débit de liquide riche 10 de la colonne haute pression 101 se refroidit dans le sousrefroidisseur 83 avant d'être détendu et envoyé à un niveau intermédiaire de la colonne basse pression 103.A flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the low pressure column 103.

Un débit d'air liquide 12 est soutiré de la colonne haute pression 101, refroidi dans le sousrefroidisseur 83, détendu et envoyé à la colonne basse pression 103.A liquid air flow 12 is withdrawn from the high pressure column 101, cooled in the subcooler 83, expanded and sent to the low pressure column 103.

Un débit d'azote résiduaire 72 est soutiré en tête de la colonne basse pression 103, envoyé au sousrefroidisseur 83 et ensuite à l'échangeur 100 où il se réchauffe. A residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.

Un débit 31 de 193 Nm3/h d'oxygène à 99,5 % mol. est soutiré sous forme liquide de la colonne basse pression 103, pompé dans la pompe 19 à 40 bara et se vaporise dans l'échangeur 100 pour former un débit gazeux sous pression.A flow 31 of 193 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column 103, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.

Un débit de 200 Nm3/h d'azote gazeux 33 est soutiré de la tête de la colonne haute pression 101 et se chauffe partiellement dans l'échangeur 100. A une température intermédiaire une partie du gaz est détendue dans une turbine 35 avant d'être mélangé avec le gaz résiduaire 72.A flow rate of 200 Nm 3 / h of nitrogen gas 33 is withdrawn from the head of the high pressure column 101 and is partially heated in the exchanger 100. At an intermediate temperature, part of the gas is expanded in a turbine 35 before d 'be mixed with waste gas 72.

Dans un autre schéma classique illustré à la Figure 2, la colonne basse pression opère à 4,8 bara et la colonne haute pression 101 opère à 14,3 bara. Ce procédé produit de l'oxygène à 99,5 % mol. avec un rendement de 78%.In another classic diagram illustrated in Figure 2, the lower column pressure operates at 4.8 bara and the high pressure column 101 operates at 14.3 bara. This process produces oxygen at 99.5 mol%. with a yield of 78%.

Un débit de 1000 Nm3/h d'air 1 à environ 14,3 bara est divisé en deux pour former un premier débit 17 et un deuxième débit 3 qui est surpressé dans un surpresseur 5 à une pression plus élevée de l'ordre de 75 bara.A flow of 1000 Nm 3 / h of air 1 at around 14.3 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara.

Les deux débits 3,17 se refroidissent en traversant un échangeur 100. Le débit 17 est envoyé en cuve de la colonne haute pression 101 et le débit liquide 3 est détendu dans une turbine 6 produisant un débit au moins partiellement liquide à sa sortie, le fluide ou mélange de fluides sortant de la turbine 6 étant envoyé au moins en partie à la colonne haute pression 101.The two flows 3.17 cool by passing through an exchanger 100. The flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine 6 producing an at least partially liquid flow at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.

Un débit de liquide riche 10 de la colonne haute pression 101 se refroidit dans le sousrefrodisseur 83 avant d'être détendu et envoyé à un niveau intermédiaire de la colonne basse pression 103.A flow of rich liquid 10 from the high pressure column 101 cools in the sub-cooler 83 before being relaxed and sent to an intermediate level of the low pressure column 103.

Un débit d'air liquide 12 est soutiré de la colonne haute pression 101, refroidi dans le sousrefroidisseur 83, détendu et envoyé à la colonne basse pression 103.A liquid air flow 12 is withdrawn from the high pressure column 101, cooled in the subcooler 83, expanded and sent to the low pressure column 103.

Un débit d'azote résiduaire 72 est soutiré en tête de la colonne basse pression 103, envoyé au sousrefroidisseur 83 et ensuite à l'échangeur 100 où il se réchauffe.A residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.

Un débit 31 de 164 Nm3/h d'oxygène à 99,5 % mol. est soutiré sous forme liquide de la colonne basse pression, pompé dans la pompe 19 à 40 bara et se vaporise dans l'échangeur 100 pour former un débit gazeux sous pression.A flow 31 of 164 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.

Aucun débit d'azote gazeux n'est soutiré en tête de la colonne haute pression 101 (évidemment un débit d'azote gazeux haute pression se condense de manière classique dans un vaporiseur-condenseur associé à la colonne basse pression).No nitrogen gas flow is withdrawn at the top of the high pressure column 101 (obviously a flow of high pressure nitrogen gas condenses so conventional in a vaporizer-condenser associated with the low pressure column).

Il est connu de EP-A-0833118 et US-A-5657644 de chauffer une colonne à pression intermédiaire d'un système à triple colonne avec un gaz enrichi en argon qui sert également à alimenter une colonne de production d'argon. It is known from EP-A-0833118 and US-A-5657644 to heat a column to intermediate pressure of a triple column system with an argon enriched gas which also used to supply an argon production column.

Les inventeurs de la présente demande ont découvert que même sans utiliser une colonne de séparation d'argon, l'épuration de l'oxygène en cuve de la colonne basse pression reste satisfaisante pour la production d'oxygène à pureté élevée.The inventors of the present application have discovered that even without using an argon separation column, the purification of oxygen in the bottom of the column low pressure remains satisfactory for the production of high purity oxygen.

Selon un objet de l'invention, il est prévu un procédé de séparation d'air dans un appareil de séparation comprenant une colonne haute pression, une colonne à pression intermédiaire ayant un rebouilleur de cuve et une colonne basse pression dans lequel

  • a) on envoie au moins un mélange au moins d'oxygène, d'azote et d'argon au moins à la colonne haute pression où il se sépare en un premier débit enrichi en oxygène et un premier débit enrichi en azote
  • b) on envoie au moins une partie du premier débit enrichi en oxygène à la colonne opérant à pression intermédiaire où il se sépare en un deuxième débit enrichi en oxygène et un deuxième débit enrichi en azote
  • c) on envoie au moins une partie du deuxième débit enrichi en oxygène et/ou du deuxième débit enrichi en azote à la colonne basse pression
  • d) on envoie un gaz de la partie inférieure de la colonne basse pression au rebouilleur de cuve de la colonne à pression intermédiaire où il se condense au moins partiellement avant d'être renvoyé à la colonne basse pression
  • e) on soutire au moins un fluide enrichi en oxygène et au moins un fluide enrichi en azote de la colonne basse pression et
  • f) on condense au moins partiellement au moins une partie du premier fluide enrichi en azote dans un vaporiseur-condenseur associé à la colonne basse pression et on renvoie au moins une partie du fluide au moins partiellement condensé à la colonne haute pression
    •    caractérisé en ce qu'aucun fluide contenant entre 3 et 20 % mol. d'argon ne s'enrichit en argon dans une colonne de l'appareil autre que les colonnes haute pression, basse pression et pression intermédiaire.According to an object of the invention, there is provided a method for separating air in a separation apparatus comprising a high pressure column, an intermediate pressure column having a tank reboiler and a low pressure column in which
  • a) at least a mixture of at least oxygen, nitrogen and argon is sent to the high pressure column where it separates into a first flow enriched in oxygen and a first flow enriched in nitrogen
  • b) at least part of the first flow enriched in oxygen is sent to the column operating at intermediate pressure where it separates into a second flow enriched in oxygen and a second flow enriched in nitrogen
  • c) at least part of the second flow enriched in oxygen and / or the second flow enriched in nitrogen is sent to the low pressure column
  • d) a gas is sent from the lower part of the low pressure column to the tank reboiler of the intermediate pressure column where it at least partially condenses before being returned to the low pressure column
  • e) at least one fluid enriched in oxygen and at least one fluid enriched in nitrogen is withdrawn from the low pressure column, and
  • f) at least partially condensing at least a portion of the first nitrogen-enriched fluid in a vaporizer-condenser associated with the low pressure column and returning at least a portion of the fluid at least partially condensed to the high pressure column
    • characterized in that no fluid containing between 3 and 20% mol. argon is enriched in argon in a column of the device other than the high pressure, low pressure and intermediate pressure columns.

    Selon d'autres objets facultatifs de l'invention, il est prévu que :

    • le fluide enrichi en oxygène soutiré de la colonne basse pression contient au moins 95 % mol. d'oxygène, éventuellement au moins 98 % mol. d'oxygène.
    • aucun débit gazeux enrichi en azote n'est soutiré en tête de la colonne haute pression ou un débit gazeux enrichi en azote est soutiré en tête de la colonne haute pression.
    • la colonne basse pression opère à au moins 1,3 bara, éventuellement au moins 2 bara, de préférence au moins 4 bara.
    • on envoie un (des) débit(s) d'air gazeux et/ou liquide à la colonne à pression intermédiaire et/ou à la colonne basse pression et/ou à la colonne haute pression.
    • le gaz provenant de la partie inférieure de la colonne basse pression envoyé au rebouilleur de cuve contient entre 1 et 20 % mol. d'argon, de préférence entre 5 et 15% mol . d'argon, encore plus préférablement entre 8 et 10 % mol. d'argon.
    • au moins une partie du deuxième débit enrichi en azote se condense, éventuellement dans un condenseur de tête de la colonne à pression intermédiaire.
    According to other optional objects of the invention, it is intended that:
    • the oxygen-enriched fluid withdrawn from the low-pressure column contains at least 95 mol%. oxygen, possibly at least 98% mol. oxygen.
    • no nitrogen-enriched gas flow is withdrawn at the top of the high pressure column or a nitrogen-enriched gas flow is withdrawn at the top of the high pressure column.
    • the low pressure column operates at at least 1.3 bara, possibly at least 2 bara, preferably at least 4 bara.
    • a flow (s) of gaseous and / or liquid air is sent to the intermediate pressure column and / or to the low pressure column and / or to the high pressure column.
    • the gas from the lower part of the low pressure column sent to the tank reboiler contains between 1 and 20% mol. argon, preferably between 5 and 15 mol%. argon, even more preferably between 8 and 10 mol%. argon.
    • at least part of the second nitrogen-enriched flow condenses, possibly in a condenser at the head of the column at intermediate pressure.

    Selon un autre objet de l'invention, il est prévu une installation de séparation d'air par distillation cryogénique comprenant une colonne haute pression, une colonne à pression intermédiaire ayant un rebouilleur de cuve et une colonne basse pression, la colonne haute pression et la colonne basse pression étant reliées thermiquement entre elles, des moyens pour envoyer un mélange au moins d'oxygène, d'azote et d'argon au moins à la colonne haute pression, des moyens pour envoyer un débit enrichi en oxygène de la colonne haute pression à la colonne à pression intermédiaire, des moyens pour envoyer un fluide enrichi en oxygène et/ou un fluide enrichi en azote de la colonne à pression intermédiaire à la colonne basse pression, des moyens pour envoyer un fluide de la colonne basse pression au rebouilleur de cuve de la colonne à pression intermédiaire, des moyens pour soutirer un fluide enrichi en azote et un fluide enrichi en oxygène de la colonne basse pression caractérisée en ce qu'elle ne comprend pas de moyens d'enrichissement en argon d'un fluide contenant entre 3 et 20 % mol. d'argon autre que les colonnes haute pression, basse pression et pression intermédiaire.According to another object of the invention, there is provided a separation installation air by cryogenic distillation comprising a high pressure column, a column at intermediate pressure having a tank reboiler and a low pressure column, the high pressure column and the low pressure column being thermally connected between them, means for sending at least a mixture of oxygen, nitrogen and argon at least to the high pressure column, means for sending a flow enriched in oxygen from the high pressure column to the intermediate pressure column, means for sending an oxygen-enriched fluid and / or a nitrogen-enriched fluid from the intermediate pressure column to the low pressure column, means for send a fluid from the low pressure column to the column reboiler of the column to intermediate pressure, means for withdrawing a nitrogen-enriched fluid and a fluid enriched in oxygen from the low pressure column, characterized in that it does not includes no means for enriching argon with a fluid containing between 3 and 20% mol. argon other than high pressure, low pressure and pressure columns intermediate.

    Selon d'autres objets facultatifs de l'invention, l'installation comprend :

    • une turbine de détente et des moyens pour amener un débit de la colonne basse pression à cette turbine sans le comprimer.
    • des moyens pour amener un débit d'air à la colonne à pression intermédiaire et/ou basse pression et/ou haute pression.
    According to other optional objects of the invention, the installation comprises:
    • an expansion turbine and means for bringing a flow rate from the low pressure column to this turbine without compressing it.
    • means for bringing an air flow to the column at intermediate pressure and / or low pressure and / or high pressure.

    Eventuellement, le fluide envoyé au rebouilleur est soutiré de la colonne basse pression à un niveau inférieur au niveau de l'introduction d'un fluide enrichi en oxygène provenant de la colonne à pression intermédiaire.Optionally, the fluid sent to the reboiler is withdrawn from the column low pressure at a level lower than the level of introduction of a fluid enriched in oxygen from the intermediate pressure column.

    De préférence, la colonne à pression intermédiaire a un condenseur de tête. Preferably, the intermediate pressure column has an overhead condenser.

    Les fluides dits 'enrichi en oxygène' ou 'enrichi en azote' sont enrichi en ces composants par rapport à de l'air.Fluids called 'enriched in oxygen' or 'enriched in nitrogen' are enriched in these components compared to air.

    Des exemples de mise en oeuvre de l'invention seront maintenant décrits par rapport aux Figures 3 et 4, qui montrent des dessins schématiques d'une installation selon l'invention.Examples of implementation of the invention will now be described by compared to Figures 3 and 4, which show schematic drawings of an installation according to the invention.

    Dans le cas de la Figure 3, l'appareil fonctionne avec une colonne basse pression à 1,3 bara et dans le cas de la Figure 4, l'appareil fonctionne avec une colonne basse pression à 4,8 bara.In the case of Figure 3, the device operates with a low column pressure at 1.3 bara and in the case of Figure 4, the device operates with a low pressure column at 4.8 bara.

    L'installation de la Figure 3 comprend une colonne haute pression 101 opérant à 5 bara, une colonne pression intermédiaire 102 opérant à 2,7 bara et une colonne basse pression 103 opérant à 1,3 bara. Une partie de l'azote gazeux de tête de la colonne haute pression sert à chauffer le rebouilleur de cuve de la colonne basse pression mais d'autres moyens de chauffage peuvent être envisagés, tel que des systèmes à doubles rebouilleurs, dont un chauffé par de l'air.The installation of Figure 3 includes a high pressure column 101 operating at 5 bara, an intermediate pressure column 102 operating at 2.7 bara and a low pressure column 103 operating at 1.3 bara. Part of the overhead nitrogen gas of the high pressure column is used to heat the bottom column reboiler pressure but other means of heating can be envisaged, such as double reboiler systems, one of which is heated by air.

    Un débit de 1000 Nm3/h d'air 1 à environ 5 bara est divisé en deux pour former un premier débit 17 et un deuxième débit 3 qui est surpressé dans un surpresseur 5 à une pression plus élevée de l'ordre de 75 bara.A flow of 1000 Nm 3 / h of air 1 at around 5 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara .

    Les deux débits 3,17 se refroidissent en traversant un échangeur 100. Le débit 17 est envoyé en cuve de la colonne haute pression 101 sans avoir été détendu ou comprimé et le débit liquide 3 est détendu dans une turbine 6 produisant un débit au moins partiellement liquide à sa sortie, le fluide ou mélange de fluides sortant de la turbine 6 étant envoyé au moins en partie à la colonne haute pression 101.The two flows 3.17 cool by passing through an exchanger 100. The flow 17 is sent to the tank of the high pressure column 101 without having been expanded or compressed and the liquid flow 3 is expanded in a turbine 6 producing a flow at less partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least in part to the high pressure column 101.

    Un débit de liquide riche 10 de la colonne haute pression 101 se refroidit dans le sousrefroidisseur 83 avant d'être détendu et envoyé à un niveau intermédiaire de la colonne à pression intermédiaire 102 entre deux sections, par exemple de garnissages structurés de type ondulé-croisé. Le liquide peut être envoyé à un autre niveau de la colonne et la colonne peut également recevoir un débit d'air gazeux ou liquide.A flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured fillings of wavy-cross type. Liquid can be sent to another column level and the column can also receive a flow of gaseous air or liquid.

    Ce liquide est séparé en un deuxième liquide enrichi en oxygène 20 et un liquide enrichi en azote 25. Le liquide 25 se refroidit dans le sousrefroidisseur 83, avant d'être détendu et envoyé en tête de la colonne basse pression 103, après être mélangé avec un débit de liquide pauvre 15 de la tête de la colonne haute pression 101 qui a également été refroidi dans le sousrefroidisseur 83 et détendu dans une vanne. This liquid is separated into a second oxygen-enriched liquid 20 and a liquid enriched in nitrogen 25. The liquid 25 cools in the subcooler 83, before to be relaxed and sent to the head of the low pressure column 103, after being mixed with a lean liquid flow 15 from the head of the high pressure column 101 which has also been cooled in the subcooler 83 and expanded in a valve.

    Le liquide de cuve 20 de la colonne à pression intermédiaire est divisé en deux. Une partie est détendue et envoyée à la colonne basse pression directement tandis que le reste est détendu dans une vanne, envoyé au condenseur de tête 22 de la colonne à pression intermédiaire où il se vaporise au moins partiellement avant d'être envoyé à la colonne basse pression 103.The tank liquid 20 of the intermediate pressure column is divided into of them. A part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 22 of the intermediate pressure column where it vaporizes at least partially before to be sent to the low pressure column 103.

    Un débit d'air liquide 12 est soutiré de la colonne haute pression, refroidi dans le sousrefroidisseur 83, détendu et envoyé à la colonne basse pression 103.A liquid air flow 12 is withdrawn from the high pressure column, cooled in the subcooler 83, expanded and sent to the low pressure column 103.

    Le rebouilleur de cuve 24 de la colonne à pression intermédiaire 102 est chauffé au moyen d'un débit gazeux enrichi en argon 233 contenant environ 5 à 15 % mol., préférablement entre 8 et 10 % mol. d'argon provenant de la colonne basse pression 103. Ce débit se condense au moins partiellement dans le rebouilleur 24 avant d'être renvoyé à la colonne basse pression 103The tank reboiler 24 of the intermediate pressure column 102 is heated by means of a gas flow enriched in argon 233 containing approximately 5 to 15% mol., preferably between 8 and 10% mol. argon from the lower column pressure 103. This flow condenses at least partially in the reboiler 24 before being returned to the low pressure column 103

    Un débit d'azote résiduaire 72 est soutiré en tête de la colonne basse pression 103, envoyé au sousrefroidisseur 83 et ensuite à l'échangeur 100 où il se réchauffe.A residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.

    Un débit 31 de 203 Nm3/h d'oxygène à 99,5 % mol. est soutiré sous forme liquide de la colonne basse pression 103, pompé dans la pompe 19 à 40 bara et se vaporise dans l'échangeur 100 pour former un débit gazeux sous pression.A flow 31 of 203 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column 103, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.

    Un débit 33 de 200 Nm3/h d'azote gazeux est soutiré en tête de la colonne haute pression 101 et se chauffe partiellement dans l'échangeur 100. A une température intermédiaire une partie du gaz est détendue dans une turbine 35 avant d'être mélangé avec le gaz résiduaire 72. Le reste de l'azote poursuit son réchauffement et constitue un produit de l'appareil.A flow 33 of 200 Nm 3 / h of nitrogen gas is drawn off at the head of the high pressure column 101 and is partially heated in the exchanger 100. At an intermediate temperature, part of the gas is expanded in a turbine 35 before be mixed with the waste gas 72. The rest of the nitrogen continues to heat up and constitutes a product of the apparatus.

    Il est possible de soutirer des produits liquides de l'appareil mais l'appareil ne produit aucun fluide riche en argon.Liquid products can be drawn from the appliance, but the appliance does not produces no argon-rich fluid.

    L'installation de la Figure 4 comprend une colonne haute pression 101 opérant à 14,3 bara, une colonne pression intermédiaire 102 opérant à 8,5 bara et une colonne basse pression 103 opérant à 4,8 bara. Tout l'azote gazeux de tête de la colonne haute pression sert à chauffer le rebouilleur de cuve de la colonne basse pression mais d'autres moyens de chauffage peuvent être envisagés, tel que des systèmes à doubles rebouilleurs, dont un chauffé par de l'air.The installation of Figure 4 includes a high pressure column 101 operating at 14.3 bara, an intermediate pressure column 102 operating at 8.5 bara and a low pressure column 103 operating at 4.8 bara. All the nitrogen gas overhead high pressure column is used to heat the bottom column tank reboiler pressure but other means of heating can be envisaged, such as double reboiler systems, one of which is heated by air.

    Un débit de 1000 Nm3/h d'air 1 à environ 14,3 bara est divisé en deux pour former un premier débit 17 et un deuxième débit 3 qui est surpressé dans un surpresseur 5 à une pression plus élevée de l'ordre de 75 bara. A flow of 1000 Nm 3 / h of air 1 at around 14.3 bara is divided into two to form a first flow 17 and a second flow 3 which is boosted in a booster 5 at a higher pressure of the order of 75 bara.

    Les deux débits 3,17 se refroidissent en traversant un échangeur 100. Le débit 17 est envoyé en cuve de la colonne haute pression 101 et le débit liquide 3 est détendu dans une turbine produisant un débit au moins partiellement liquide à sa sortie, le fluide ou mélange de fluides sortant de la turbine étant envoyé au moins en partie à la colonne haute pression 101.The two flows 3.17 cool by passing through an exchanger 100. The flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine producing an at least partially liquid flow at its outlet, the fluid or mixture of fluids leaving the turbine being sent at least in part to the high pressure column 101.

    Un débit de liquide riche 10 de la colonne haute pression 101 se refroidit dans le sousrefroidisseur 83 avant d'être détendu et envoyé à un niveau intermédiaire de la colonne à pression intermédiaire 102 entre deux sections, par exemple de garnissages structurés de type ondulé-croisé. Le liquide peut être envoyé à un autre niveau de la colonne et la colonne peut également recevoir un débit d'air gazeux ou liquide.A flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being expanded and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured fillings of wavy-cross type. Liquid can be sent to another column level and the column can also receive a flow of gaseous air or liquid.

    Ce liquide est séparé en un deuxième liquide enrichi en oxygène 20 et un liquide enrichi en azote 25. Le liquide 25 se refroidit dans le sousrefroidisseur 83, avant d'être détendu et envoyé en tête de la colonne basse pression 103, après être mélangé avec un débit de liquide pauvre 15 de la tête de la colonne haute pression 101 qui a également été refroidi dans le sousrefroidisseur 83 et détendu dans une vanne.This liquid is separated into a second oxygen-enriched liquid 20 and a liquid enriched in nitrogen 25. The liquid 25 cools in the subcooler 83, before to be relaxed and sent to the head of the low pressure column 103, after being mixed with a lean liquid flow 15 from the head of the high pressure column 101 which has also been cooled in the subcooler 83 and expanded in a valve.

    Le liquide de cuve 20 de la colonne à pression intermédiaire est divisé en deux. Une partie est détendue et envoyée à la colonne basse pression directement tandis que le reste est détendu dans une vanne, envoyé au condenseur de tête 22 de la colonne à pression intermédiaire où il se vaporise au moins partiellement avant d'être envoyé à la colonne basse pression 103.The tank liquid 20 of the intermediate pressure column is divided into of them. A part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 22 of the intermediate pressure column where it vaporizes at least partially before to be sent to the low pressure column 103.

    Un débit d'air liquide 12 est soutiré de la colonne haute pression, refroidi dans le sousrefroidisseur 83, détendu et envoyé à la colonne basse pression.A liquid air flow 12 is withdrawn from the high pressure column, cooled in the subcooler 83, expanded and sent to the low pressure column.

    Le rebouilleur de cuve 24 de la colonne à pression intermédiaire 102 est chauffé au moyen d'un débit gazeux enrichi en argon 233 contenant environ 5 à 15 % mol., préférablement 8 à 10 % mol. d'argon provenant de la colonne basse pression 103. Ce débit se condense au moins partiellement dans le rebouilleur 24 avant d'être renvoyé à la colonne basse pression 103.The tank reboiler 24 of the intermediate pressure column 102 is heated by means of a gas flow enriched in argon 233 containing approximately 5 to 15% mol., preferably 8 to 10% mol. argon from the low pressure column 103. This flow condenses at least partially in the reboiler 24 before being returned to low pressure column 103.

    Un débit d'azote résiduaire 72 est soutiré en tête de la colonne basse pression 103, envoyé au sousrefroidisseur 83 et ensuite à l'échangeur 100 où il se réchauffe.A residual nitrogen flow 72 is drawn off at the head of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.

    Un débit 31 de 177 Nm3/h d'oxygène à 99,5% mol. est soutiré sous forme liquide de la colonne basse pression, pompé dans la pompe 19 à 40 bara et se vaporise dans l'échangeur 100 pour former un débit gazeux sous pression. A flow 31 of 177 Nm 3 / h of oxygen at 99.5% mol. is withdrawn in liquid form from the low pressure column, pumped into the pump 19 at 40 bara and vaporized in the exchanger 100 to form a gas flow under pressure.

    II est possible de soutirer des produits liquides de l'appareil mais l'appareil ne produit aucun fluide enrichi en argon.It is possible to draw off liquid products from the appliance but the appliance does not produces no fluid enriched with argon.

    Les avantages de l'invention apparaítront clairement à l'étude des tableaux ci-dessus.The advantages of the invention will become apparent from the study of the above tables.

    D'autres moyens de production de froid alternatifs ou supplémentaires peuvent être envisagés, tel qu'une turbine d'insufflation, une turbine Claude ou une autre turbine qui n'est pas alimentée par un débit liquide ou une turbine de gaz provenant de la colonne basse pression.Other alternative or additional means of cooling can be considered, such as an insufflation turbine, a Claude turbine or a other turbine which is not supplied by a liquid flow or a gas turbine from the low pressure column.

    L'appareil peut recevoir tout ou une partie de son air d'alimentation d'un compresseur d'une turbine à gaz, l'azote résiduaire de l'appareil étant renvoyé à la turbine à gaz. Procédé de la Figure 1 Procédé de la Figure 3 (invention)    Pression de la colonne haute pression 5 bara 5 bara    Pression de la colonne basse pression 1.3 bara 1.3 bara    Pression de la colonne à pression intermédiaire 2.7 bara    Débit total d'air traité 1000 Nm3/h 1000 Nm3/h    Teneur en oxygène du produit gazeux 99.5% O2 99.5% O2    Production d'oxygène, compté pur 193 Nm3/h 203 Nm3/h    Production d'azote gazeux haute pression 200 Nm3/h 200 Nm3/h    Rendement d'extraction d'oxygène 92% 97%    Energie de séparation Base : 100 95 Procédé de la Figure 2 Procédé de la Figure 4 (invention)    Pression de la colonne haute pression 14.3 bara 14.3 bara    Pression de la colonne basse pression 4.8 bara 4.8 bara    Pression de la colonne à pression intermédiaire 8.5 bara    Débit d'air total 1000 Nm3/h 1000 Nm3/h    Teneur en oxygène du produit gazeux 99.5% O2 99.5% O2    Production d'oxygène, compté pur 164 Nm3/h 177 Nm3/h    Production d'azote gazeux haute pression 0 Nm3/h 0 Nm3/h    Rendement d'extraction d'oxygène 78% 85%    Energie de séparation Base : 100 90 The appliance can receive all or part of its supply air from a compressor of a gas turbine, the residual nitrogen from the appliance being returned to the gas turbine. Figure 1 process Figure 3 process (invention) High pressure column pressure 5 bara 5 bara Low pressure column pressure 1.3 bara 1.3 bara Intermediate pressure column pressure 2.7 bara Total treated air flow 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.5% O2 99.5% O2 Oxygen production, counted pure 193 Nm 3 / h 203 Nm 3 / h High pressure nitrogen gas production 200 Nm 3 / h 200 Nm 3 / h Oxygen extraction efficiency 92% 97% Separation energy Base: 100 95 Figure 2 process Figure 4 process (invention) High pressure column pressure 14.3 bara 14.3 bara Low pressure column pressure 4.8 bara 4.8 bara Intermediate pressure column pressure 8.5 bara Total air flow 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.5% O2 99.5% O2 Oxygen production, counted pure 164 Nm 3 / h 177 Nm 3 / h High pressure nitrogen gas production 0 Nm 3 / h 0 Nm 3 / h Oxygen extraction efficiency 78% 85% Separation energy Base: 100 90

    Claims (13)

    Procédé de séparation d'air dans un appareil de séparation comprenant une colonne haute pression (101), une colonne à pression intermédiaire (102) ayant un rebouilleur de cuve (24) et une colonne basse pression (103) dans lequel a) on envoie au moins un mélange (1) au moins d'oxygène, d'azote et d'argon au moins à la colonne haute pression où il se sépare en un premier débit enrichi en oxygène et un premier débit enrichi en azote b) on envoie au moins une partie du premier débit (10) enrichi en oxygène à la colonne opérant à pression intermédiaire où il se sépare en un deuxième débit enrichi en oxygène (20) et un deuxième débit enrichi en azote (25) c) on envoie au moins une partie du deuxième débit enrichi en oxygène et/ou du deuxième débit enrichi en azote à la colonne basse pression d) on envoie un gaz (233) de la partie inférieure de la colonne basse pression au rebouilleur de cuve de la colonne à pression intermédiaire où il se condense au moins partiellement avant d'être renvoyé à la colonne basse pression e) on soutire au moins un fluide enrichi en oxygène (31) et au moins un fluide (72) enrichi en azote de la colonne basse pression et f) on condense au moins partiellement au moins une partie du premier fluide enrichi en azote dans un vaporiseur-condenseur associé à la colonne basse pression et on renvoie au moins une partie du fluide au moins partiellement condensé à la colonne haute pression    caractérisé en ce qu'aucun fluide contenant entre 3 et 20 % mol. d'argon ne s'enrichit en argon dans une colonne de l'appareil autre que les colonnes haute pression, basse pression et pression intermédiaire.A method of separating air in a separation apparatus comprising a high pressure column (101), an intermediate pressure column (102) having a tank reboiler (24) and a low pressure column (103) in which a) at least one mixture (1) of at least oxygen, nitrogen and argon is sent to the high pressure column where it separates in a first flow enriched in oxygen and a first flow enriched in nitrogen b) at least part of the first flow (10) enriched in oxygen is sent to the column operating at intermediate pressure where it separates into a second flow enriched in oxygen (20) and a second flow enriched in nitrogen (25) c) at least part of the second flow enriched in oxygen and / or the second flow enriched in nitrogen is sent to the low pressure column d) a gas (233) is sent from the lower part of the low pressure column to the tank reboiler of the intermediate pressure column where it at least partially condenses before being returned to the low pressure column e) at least one fluid enriched in oxygen (31) and at least one fluid (72) enriched in nitrogen is withdrawn from the low pressure column, and f) at least partially condensing at least a portion of the first nitrogen-enriched fluid in a vaporizer-condenser associated with the low pressure column and returning at least a portion of the fluid at least partially condensed to the high pressure column characterized in that no fluid containing between 3 and 20% mol. argon is enriched in argon in a column of the device other than the high pressure, low pressure and intermediate pressure columns. Procédé selon la revendication 1 dans lequel le fluide (31) enrichi en oxygène soutiré de la colonne basse pression contient au moins 95 % mol. d'oxygène, éventuellement au moins 98 % mol. d'oxygène.The method of claim 1 wherein the fluid (31) enriched in oxygen withdrawn from the low pressure column contains at least 95 mol%. oxygen, possibly at least 98% mol. oxygen. Procédé selon la revendication 1 ou 2 dans lequel aucun débit gazeux enrichi en azote n'est soutiré en tête de la colonne haute pression (101).Method according to claim 1 or 2 in which no gas flow enriched in nitrogen is not withdrawn at the top of the high pressure column (101). Procédé selon la revendication 1 ou 2 dans lequel un débit gazeux (33) enrichi en azote est soutiré en tête de la colonne haute pression (101). The method of claim 1 or 2 wherein a gas flow (33) enriched in nitrogen is withdrawn at the top of the high pressure column (101). Procédé selon la revendication 1,2,3 ou 4 dans lequel la colonne basse pression (103) opère à au moins 1,3 bara, éventuellement au moins 2 bara, de préférence au moins 4 bara.The method of claim 1,2,3 or 4 wherein the lower column pressure (103) operates at at least 1.3 bara, possibly at least 2 bara, preferably at least 4 bara. Procédé selon une des revendications précédentes dans lequel on envoie un (des) débit(s) d'air gazeux et/ou liquide à la colonne à pression intermédiaire et/ou à la colonne basse pression et/ou à la colonne haute pression.Method according to one of the preceding claims, in which sends a flow (s) of gaseous and / or liquid air to the pressure column intermediate and / or low pressure column and / or high pressure column. Procédé selon une des revendications précédentes dans lequel le gaz (233) provenant de la partie inférieure de la colonne basse pression envoyé au rebouilleur de cuve contient entre 1 et 20 % mol. d'argon.Method according to one of the preceding claims, in which the gas (233) from the lower part of the low pressure column sent to tank reboiler contains between 1 and 20% mol. argon. Procédé selon une des revendications précédentes dans lequel au moins une partie du deuxième débit enrichi en azote se condense, éventuellement dans un condenseur de tête (22) de la colonne à pression intermédiaire.Method according to one of the preceding claims, in which at at least part of the second nitrogen-enriched flow condenses, possibly in a head condenser (22) of the intermediate pressure column. Installation de séparation d'air par distillation cryogénique comprenant une colonne haute pression (101), une colonne à pression intermédiaire (102) ayant un rebouilleur de cuve (24) et une colonne basse pression (103), la colonne haute pression et la colonne basse pression étant reliées thermiquement entre elles, des moyens pour envoyer un mélange (1) au moins d'oxygène, d'azote et d'argon au moins à la colonne haute pression, des moyens pour envoyer un débit enrichi en oxygène (10) de la colonne haute pression à la colonne à pression intermédiaire, des moyens pour envoyer un fluide enrichi en oxygène (20) et/ou un fluide enrichi en azote (25) de la colonne à pression intermédiaire à la colonne basse pression, des moyens pour envoyer un fluide (233) de la colonne basse pression au rebouilleur de cuve de la colonne à pression intermédiaire, des moyens pour soutirer un fluide enrichi en azote (72) et un fluide enrichi en oxygène (31) de la colonne basse pression
       caractérisée en ce qu'elle ne comprend pas de moyens d'enrichissement en argon d'un fluide contenant entre 3 et 20 % mol. d'argon autre que les colonnes haute pression, basse pression et pression intermédiaire.    Installation for air separation by cryogenic distillation comprising a high pressure column (101), an intermediate pressure column (102) having a tank reboiler (24) and a low pressure column (103), the high pressure column and the column low pressure being thermally connected together, means for sending a mixture (1) of at least oxygen, nitrogen and argon at least to the high pressure column, means for sending a flow enriched in oxygen (10) from the high pressure column to the intermediate pressure column, means for sending an oxygen-enriched fluid (20) and / or a nitrogen-enriched fluid (25) from the intermediate pressure column to the low pressure column, means for send a fluid (233) from the low pressure column to the reboiler of the intermediate pressure column, means for withdrawing a nitrogen-enriched fluid (72) and an oxygen-enriched fluid (31) from the low pressure column
    characterized in that it does not include means for enriching argon with a fluid containing between 3 and 20 mol%. argon other than the high pressure, low pressure and intermediate pressure columns.         Installation selon la revendication 9 comprenant une turbine de détente et des moyens pour amener un débit de la colonne basse pression à cette turbine sans le comprimer.Installation according to claim 9 comprising a turbine expansion and means for bringing a flow from the low pressure column to this turbine without compressing it. Installation selon la revendication 9 ou 10 comprenant des moyens pour amener un débit d'air à la colonne à pression intermédiaire et/ou basse pression et/ou haute pression (101,102,103). Installation according to claim 9 or 10 comprising means for supplying an air flow to the intermediate pressure column and / or low pressure and / or high pressure (101,102,103). Installation selon l'une des revendications 9 à 11 dans laquelle le fluide (233) envoyé au rebouilleur est soutiré de la colonne basse pression à un niveau inférieur au niveau de l'introduction d'un fluide enrichi en oxygène provenant de la colonne à pression intermédiaire.Installation according to one of claims 9 to 11 in which the fluid (233) sent to the reboiler is withdrawn from the low pressure column at a level below the level of introduction of an oxygen-enriched fluid from the intermediate pressure column. Installation selon l'une des revendications 9 à 12 dans laquelle la colonne à pression intermédiaire (102) a un condenseur de tête (22).Installation according to one of claims 9 to 12 in which the intermediate pressure column (102) has a head condenser (22).
    EP01402310A 2000-09-19 2001-09-06 Process and apparatus for air separation by cryogenic distillation Expired - Lifetime EP1189003B1 (en)

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    FR0011932A FR2814229B1 (en) 2000-09-19 2000-09-19 METHOD AND PLANT FOR AIR SEPARATION BY CRYOGENIC DISTILLATION

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    CN106211791A (en) * 2014-02-14 2016-12-07 乔治洛德方法研究和开发液化空气有限公司 For being separated the tower of air by low temperature distillation, including the air separation equipment of such tower and for the method producing such tower
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    FR2875588B1 (en) * 2004-09-21 2007-04-27 Air Liquide AIR SEPARATION METHOD BY CRYOGENIC DISTILLATION
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    DE60108579D1 (en) 2005-03-03
    EP1189003B1 (en) 2005-01-26
    ATE288064T1 (en) 2005-02-15
    FR2814229B1 (en) 2002-10-25
    FR2814229A1 (en) 2002-03-22
    US6536232B2 (en) 2003-03-25

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