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EP1189003B1 - 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
EP1189003B1
EP1189003B1 EP01402310A EP01402310A EP1189003B1 EP 1189003 B1 EP1189003 B1 EP 1189003B1 EP 01402310 A EP01402310 A EP 01402310A EP 01402310 A EP01402310 A EP 01402310A EP 1189003 B1 EP1189003 B1 EP 1189003B1
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EP
European Patent Office
Prior art keywords
pressure column
low
column
pressure
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.)
Expired - Lifetime
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EP01402310A
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German (de)
French (fr)
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EP1189003A1 (en
Inventor
Benoit Davidian
Francois De Bussy
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 a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude
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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 of air separation by cryogenic distillation according to the preamble of claims 1 and 9, respectively.
  • Such a process and such installation are known from US-A-5,657,644.
  • An object of the invention is to reduce the energy consumption of the process separation from the prior art methods.
  • Another object of the invention is to produce oxygen with a purity of minus 95 mol%, or even at least 98 mol%. with improved performance.
  • Figure 1 shows a conventional method with a low pressure column 103 operating at 1.3 bara to make oxygen at 99.5 mol%. with a 92% yield.
  • a flow rate of 1000 Nm 3 / h of air 1 at approximately 5 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged in a booster 5 at a higher pressure of the order of 75 bara. .
  • Both flow rates 3.17 cool through crossing a heat exchanger 100.
  • flow 17 is sent to the tank of the high pressure column 101 and the liquefied flow 3 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 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 flow of residual nitrogen 72 is withdrawn at the top of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow rate 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 to 40 bara and vaporizes 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 top 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 to be mixed with the waste gas 72.
  • a flow rate of 1000 Nm 3 / h of air 1 to about 14.3 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged in a booster 5 at a higher pressure of the order of 75 bara.
  • Both flow rates 3.17 cool through crossing a heat exchanger 100.
  • 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 a flow at least rectally liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least part of the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the subrefroder 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 flow of residual nitrogen 72 is withdrawn at the top 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 to 40 bara and vaporizes in the exchanger 100 to form a gas flow under pressure.
  • a separation installation of air by cryogenic distillation comprising a high pressure column, a column at intermediate pressure having a bottom reboiler and a low pressure column, the high pressure column and the low pressure column being thermally connected between them, means for sending a mixture of at least oxygen, nitrogen and argon at least to the high pressure column, means for sending a flow enriched with 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 bottom reboiler of the column to intermediate pressure, means for withdrawing a nitrogen-enriched fluid and a fluid enriched with oxygen in 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 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 the introduction of a fluid enriched in oxygen from the intermediate pressure column.
  • the intermediate pressure column has a head condenser.
  • the fluids known as 'enriched in oxygen' or 'enriched in nitrogen' are enriched in these components compared to air.
  • the apparatus operates with a low column pressure at 1.3 bara and in the case of Figure 4, the apparatus operates with a low pressure column at 4.8 bara.
  • 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 nitrogen gas head of the high pressure column is used to heat the bottom reboiler of the column pressure but other means of heating can be envisaged, such as double reboiler systems, one heated by air.
  • a flow rate of 1000 Nm 3 / h of air 1 at approximately 5 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged in a booster 5 at a higher pressure of the order of 75 bara. .
  • Both flow rates 3.17 cool through crossing a heat exchanger 100.
  • flow 17 is sent to the tank of the high pressure column 101 without being relaxed or compressed and the liquid flow 3 is expanded in a turbine 6 producing a flow rate 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 relaxed and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured packings of corrugated-cross type.
  • the liquid can be sent to another level of the column and the column can also receive a gaseous air flow or liquid.
  • This liquid is separated into a second oxygen-enriched liquid 20 and a nitrogen-enriched liquid 25.
  • the liquid 25 cools in the subcooler 83, before to be relaxed and sent to the top of the low pressure column 103, after being mixed with a poor liquid flow 15 from the top of the high pressure column 101 which was also cooled in the subcooler 83 and relaxed in a valve.
  • the bottom liquid of the intermediate pressure column is divided into two. Part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 29 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 reboiler 24 of the intermediate pressure column 102 is heated by means of an argon-enriched gas flow 233 containing about 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 flow of residual nitrogen 72 is withdrawn at the top of the low pressure column 103, sent to the subcooler 83 and then to the exchanger 100 where it heats up.
  • a flow rate 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 to 40 bara and vaporizes in the exchanger 100 to form a gas flow under pressure.
  • a flow rate of 200 Nm 3 / h of nitrogen gas is withdrawn at the top 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 mixed with the waste gas 72. The rest of the nitrogen continues its heating and is a product of the apparatus.
  • 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 in the head 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 heated by air.
  • a flow rate of 1000 Nm 3 / h of air 1 to about 14.3 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged in a booster 5 at a higher pressure of the order of 75 bara.
  • Both flow rates 3.17 cool through crossing a heat exchanger 100.
  • flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine producing a flow at least partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine being sent at least part of the high pressure column 101.
  • a flow of rich liquid 10 from the high pressure column 101 cools in the subcooler 83 before being relaxed and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured packings of corrugated-cross type.
  • the liquid can be sent to another level of the column and the column can also receive a gaseous air flow or liquid.
  • This liquid is separated into a second oxygen-enriched liquid 20 and a nitrogen-enriched liquid 25.
  • the liquid 25 cools in the subcooler 83, before to be relaxed and sent to the top of the low pressure column 103, after being mixed with a poor liquid flow 15 from the top of the high pressure column 101 which was also cooled in the subcooler 83 and relaxed in a valve.
  • the bottom liquid of the intermediate pressure column is divided into two. Part is relaxed and sent to the low pressure column directly while the rest is relaxed 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 reboiler 24 of the intermediate pressure column 102 is heated by means of an argon-enriched gas flow 233 containing about 5 to 15% mol., preferably 8 to 10 mol%. argon from the low pressure column 103. This flow is condensed at least partially in the reboiler 24 before being returned to the low pressure column 103.
  • a flow of residual nitrogen 72 is withdrawn at the top 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 to 40 bara and vaporizes in the exchanger 100 to form a gas flow under pressure.
  • the apparatus may receive all or a portion of its supply air from a compressor of a gas turbine, the residual nitrogen of the apparatus being returned to the gas turbine.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)

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 selon le préambule des revendications 1 et 9, respectivement. Un tel procédé et une telle installation sont connus du US-A-5 657 644.The present invention relates to a method and an installation of air separation by cryogenic distillation according to the preamble of claims 1 and 9, respectively. Such a process and such installation are known from US-A-5,657,644.

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 method of this kind to separate of air, the intermediate pressure column having a bottom reboiler heated by nitrogen from the high pressure column, thereby reducing the heating of the reboiler vessel of the low pressure column.

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 from the prior art methods.

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 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 conventional method with a low pressure column 103 operating at 1.3 bara to make 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 rate of 1000 Nm 3 / h of air 1 at approximately 5 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged 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.Both flow rates 3.17 cool through crossing a heat exchanger 100. flow 17 is sent to the tank of the high pressure column 101 and the liquefied flow 3 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 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 flow of residual nitrogen 72 is withdrawn at the top 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 rate 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 to 40 bara and vaporizes 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 top 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 to be mixed with the 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 scheme shown in Figure 2, the low column pressure operates at 4.8 bara and the high pressure column 101 operates at 14.3 bara. This process produces 99.5 mol% oxygen. 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 rate of 1000 Nm 3 / h of air 1 to about 14.3 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged 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 parliellement 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.Both flow rates 3.17 cool through crossing a heat exchanger 100. 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 a flow at least parlamentally liquid at its outlet, the fluid or mixture of fluids leaving the turbine 6 being sent at least part of 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 subrefroder 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 flow of residual nitrogen 72 is withdrawn at the top 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 to 40 bara and vaporizes 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 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 at intermediate pressure of a triple-column system with an argon-enriched gas is also used to feed 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 this application have discovered that even without using an argon separation column, the purification of the oxygen in the bottom of the column Low pressure remains satisfactory for the production of oxygen at high purity.

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 of separating air in a separation apparatus comprising a high pressure column, an intermediate pressure column having a bottom reboiler and a low pressure column in which
  • a) at least one mixture of at least oxygen, nitrogen and argon is sent at least to the high pressure column where it separates into a first oxygen-enriched flow and a first nitrogen-enriched flow;
  • b) at least a portion of the first oxygen-enriched flow 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 a portion of the second oxygen enriched flow and / or the second nitrogen enriched flow is sent to the low pressure column
  • d) a gas is fed from the lower part of the low pressure column to the bottom reboiler of the intermediate pressure column where it condenses at least partially before being returned to the low pressure column
  • e) at least one oxygen-enriched fluid and at least one nitrogen-enriched fluid are 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 at least partially condensed fluid 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 apparatus other than high pressure columns, low pressure and intermediate pressure.

    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 provided that:
    • the oxygen-enriched fluid withdrawn from the low pressure column contains at least 95 mol%. of oxygen, optionally at least 98 mol%. oxygen.
    • no gas flow enriched in nitrogen 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 least 1.3 bara, optionally 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 coming from the lower part of the low pressure column sent to the bottom reboiler contains between 1 and 20 mol%. argon, preferably between 5 and 15 mol%. argon, still more preferably between 8 and 10 mol%. argon.
    • at least a portion of the second nitrogen-enriched stream condenses, optionally in a top condenser of the intermediate pressure column.

    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 of air by cryogenic distillation comprising a high pressure column, a column at intermediate pressure having a bottom reboiler and a low pressure column, the high pressure column and the low pressure column being thermally connected between them, means for sending a mixture of at least oxygen, nitrogen and argon at least to the high pressure column, means for sending a flow enriched with 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 bottom reboiler of the column to intermediate pressure, means for withdrawing a nitrogen-enriched fluid and a fluid enriched with oxygen in 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 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 of the low pressure column to this turbine without compressing it.
    • means for supplying an air flow to the intermediate pressure and / or low pressure and / or high pressure column.

    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 the 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 a head condenser.

    Les fluides dits 'enrichi en oxygène' ou 'enrichi en azote' sont enrichi en ces composants par rapport à de l'air.The fluids known as '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 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 apparatus operates with a low column pressure at 1.3 bara and in the case of Figure 4, the apparatus 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 nitrogen gas head of the high pressure column is used to heat the bottom reboiler of the column pressure but other means of heating can be envisaged, such as double reboiler systems, one 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 rate of 1000 Nm 3 / h of air 1 at approximately 5 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged 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.Both flow rates 3.17 cool through crossing a heat exchanger 100. flow 17 is sent to the tank of the high pressure column 101 without being relaxed or compressed and the liquid flow 3 is expanded in a turbine 6 producing a flow rate 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 relaxed and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured packings of corrugated-cross type. The liquid can be sent to another level of the column and the column can also receive a gaseous air flow 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 nitrogen-enriched liquid 25. The liquid 25 cools in the subcooler 83, before to be relaxed and sent to the top of the low pressure column 103, after being mixed with a poor liquid flow 15 from the top of the high pressure column 101 which was also cooled in the subcooler 83 and relaxed 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 29 de la colonne à pression intermédiaire où il se vaporise au moins partiellement avant d'être envoyé à la colonne basse pression 103.The bottom liquid of the intermediate pressure column is divided into two. Part is relaxed and sent to the low pressure column directly while the rest is expanded in a valve, sent to the head condenser 29 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 reboiler 24 of the intermediate pressure column 102 is heated by means of an argon-enriched gas flow 233 containing about 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 flow of residual nitrogen 72 is withdrawn at the top 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 rate 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 to 40 bara and vaporizes 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 rate of 200 Nm 3 / h of nitrogen gas is withdrawn at the top 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 mixed with the waste gas 72. The rest of the nitrogen continues its heating and is 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.It is possible to withdraw liquids from the appliance but the appliance produces no fluid rich in argon.

    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 in the head 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 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 rate of 1000 Nm 3 / h of air 1 to about 14.3 bara is divided in two to form a first flow 17 and a second flow 3 which is supercharged 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.Both flow rates 3.17 cool through crossing a heat exchanger 100. flow 17 is sent to the tank of the high pressure column 101 and the liquid flow 3 is expanded in a turbine producing a flow at least partially liquid at its outlet, the fluid or mixture of fluids leaving the turbine being sent at least part of 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 relaxed and sent to an intermediate level of the intermediate pressure column 102 between two sections, for example of structured packings of corrugated-cross type. The liquid can be sent to another level of the column and the column can also receive a gaseous air flow 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 nitrogen-enriched liquid 25. The liquid 25 cools in the subcooler 83, before to be relaxed and sent to the top of the low pressure column 103, after being mixed with a poor liquid flow 15 from the top of the high pressure column 101 which was also cooled in the subcooler 83 and relaxed 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 bottom liquid of the intermediate pressure column is divided into two. Part is relaxed and sent to the low pressure column directly while the rest is relaxed 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 reboiler 24 of the intermediate pressure column 102 is heated by means of an argon-enriched gas flow 233 containing about 5 to 15% mol., preferably 8 to 10 mol%. argon from the low pressure column 103. This flow is condensed 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 flow of residual nitrogen 72 is withdrawn at the top 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 to 40 bara and vaporizes 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 withdraw liquid products from the apparatus but the apparatus produces no argon-enriched fluid.

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

    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 means of alternative or supplementary cold production may be considered, such as an insufflation turbine, a Claude turbine or a other turbine that is not powered 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% 02 99.5% 02 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% 02 99.5% 02 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 apparatus may receive all or a portion of its supply air from a compressor of a gas turbine, the residual nitrogen of the apparatus being returned to the gas turbine. Process of Figure 1 Process of Figure 3 (Invention) Pressure of the high pressure column 5 bara 5 bara Pressure of the low pressure column 1.3 bara 1.3 bara Pressure of the intermediate pressure column 2.7 bara Total flow of treated air 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.5% 02 99.5% 02 Oxygen production, counted pure 193 Nm 3 / h 203 Nm 3 / h Production of high pressure nitrogen gas 200 Nm 3 / h 200 Nm 3 / h Oxygen extraction efficiency 92% 97% Separation energy Base: 100 95 Process of Figure 2 Process of Figure 4 (Invention) Pressure of the high pressure column 14.3 bara 14.3 bara Pressure of the low pressure column 4.8 bara 4.8 bara Pressure of the intermediate pressure column 8.5 bara Total air flow 1000 Nm 3 / h 1000 Nm 3 / h Oxygen content of the gaseous product 99.5% 02 99.5% 02 Oxygen production, counted pure 164 Nm 3 / h 177 Nm 3 / h Production of high pressure nitrogen gas 0 Nm 3 / h 0 Nm 3 / h Oxygen extraction efficiency 78% 85% Separation energy Base: 100 90

    Claims (13)

    1. Process for separating air in a separation apparatus comprising a high-pressure column (101), an intermediate-pressure column (102) having a bottom 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 at least to the high-pressure column where it is separated into a first oxygen-enriched stream and a first nitrogen-enriched stream,
      b) at least part of the first oxygen-enriched stream (10) is sent to the column operating at intermediate pressure where it is separated into a second oxygen-enriched stream (20) and a second nitrogen-enriched stream (25),
      c) at least part of the second oxygen-enriched stream and/or the second nitrogen-enriched stream is sent to the low-pressure column,
      d) a gas (233) is sent from the lower part of the low-pressure column to the bottom reboiler of the intermediate-pressure column where it is condensed at least partially before being sent back to the low-pressure column,
      e) at least one oxygen-enriched fluid (31) and at least one nitrogen-enriched fluid (72) are withdrawn from the low-pressure column and
      f) at least part of the first nitrogen-enriched fluid is condensed at least partially in a reboiler-condenser associated with the low-pressure column and at least part of the at least partially condensed fluid is sent back to the high-pressure column
      characterized in that no fluid containing between 3 and 20 mol% argon is enriched with argon in a column of the apparatus other than the high-pressure, low-pressure and intermediate-pressure columns.
    2. Process according to Claim 1 in which the oxygen-enriched fluid (31) withdrawn from the low-pressure column contains at least 95 mol% oxygen, possibly at least 98 mol% oxygen.
    3. Process according to Claim 1 or 2 in which no nitrogen-enriched gas stream is withdrawn from the top of the high-pressure column (101).
    4. Process according to Claim 1 or 2 in which a nitrogen-enriched gas stream (33) is withdrawn from the top of the high-pressure column (101).
    5. Process according to Claim 1, 2, 3 or 4 in which the low-pressure column (103) operates at at least 1.3 bara, optionally at least 2 bara, preferably at least 4 bara.
    6. Process according to one of the preceding claims in which one or more of the gaseous and/or liquid air stream(s) is (are) sent to the intermediate-pressure column and/or to the low-pressure column and/or to the high-pressure column.
    7. Process according to one of the preceding claims in which the gas (233) coming from the lower part of the low-pressure column sent to the bottom reboiler contains between 1 and 20 mol% argon.
    8. Process according to one of the preceding claims in which at least part of the second nitrogen-enriched stream is condensed, optionally in a top condenser (29) of the intermediate-pressure column.
    9. Plant for separating air by cryogenic distillation comprising a high-pressure column (101), an intermediate-pressure column (102) having a bottom reboiler (24) and a low-pressure column (103), the high-pressure column and the low-pressure column 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 to send an oxygen-enriched stream (10) from the high-pressure column to the intermediate-pressure column, means to send an oxygen-enriched fluid (20) and/or a nitrogen-enriched fluid (25) from the intermediate-pressure column to the low-pressure column, means to send a fluid (233) from the low-pressure column to the bottom reboiler of the intermediate-pressure column, means to withdraw a nitrogen-enriched fluid (72) and an oxygen-enriched fluid (31) from the low-pressure column
      characterized in that it does not comprise means for the argon enrichment of a fluid containing between 3 and 20 mol% argon other than the high-pressure, low-pressure and intermediate-pressure columns.
    10. Plant according to Claim 9 comprising an expansion turbine and means to direct a stream from the low-pressure column to this turbine without compressing the stream.
    11. Plant according to Claim 9 or 10 comprising means to direct an air stream to the intermediate-pressure and/or low-pressure and/or high-pressure column (101, 102, 103).
    12. Plant 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 lower than the level at which an oxygen-enriched fluid coming from the intermediate-pressure column is introduced.
    13. Plant according to one of Claims 9 to 12 in which the intermediate-pressure column (102) has a top condenser (29).
    EP01402310A 2000-09-19 2001-09-06 Process and apparatus for air separation by cryogenic distillation Expired - Lifetime EP1189003B1 (en)

    Applications Claiming Priority (2)

    Application Number Priority Date Filing Date Title
    FR0011932A FR2814229B1 (en) 2000-09-19 2000-09-19 METHOD AND PLANT FOR AIR SEPARATION BY CRYOGENIC DISTILLATION
    FR0011932 2000-09-19

    Publications (2)

    Publication Number Publication Date
    EP1189003A1 EP1189003A1 (en) 2002-03-20
    EP1189003B1 true EP1189003B1 (en) 2005-01-26

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    Application Number Title Priority Date Filing Date
    EP01402310A Expired - Lifetime EP1189003B1 (en) 2000-09-19 2001-09-06 Process and apparatus for air separation by cryogenic distillation

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    US (1) US6536232B2 (en)
    EP (1) EP1189003B1 (en)
    AT (1) ATE288064T1 (en)
    CA (1) CA2357302A1 (en)
    DE (1) DE60108579T2 (en)
    FR (1) FR2814229B1 (en)
    ZA (1) ZA200107210B (en)

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    ATE356326T1 (en) * 2001-12-04 2007-03-15 Air Prod & Chem METHOD AND DEVICE FOR CRYOGENIC AIR SEPARATION
    FR2875588B1 (en) * 2004-09-21 2007-04-27 Air Liquide AIR SEPARATION METHOD BY CRYOGENIC DISTILLATION
    DE102004047961A1 (en) * 2004-10-01 2006-05-18 Siemens Ag Device and method for driving a piezoelectric actuator
    EP2597409B1 (en) * 2011-11-24 2015-01-14 L'AIR LIQUIDE, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process and apparatus for the separation of air by cryogenic distillation
    EP2634517B1 (en) * 2012-02-29 2018-04-04 L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process and apparatus for the separation of air by cryogenic distillation
    FR3017698B1 (en) * 2014-02-14 2019-03-29 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude AIR SEPARATION COLUMN BY CRYOGENIC DISTILLATION, AIR SEPARATION APPARATUS COMPRISING SUCH A COLUMN, AND METHOD OF MANUFACTURING SUCH A COLUMN
    EP3620739A1 (en) * 2018-09-05 2020-03-11 Linde Aktiengesellschaft Method for the low-temperature decomposition of air and air separation plant
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    ATE288064T1 (en) 2005-02-15
    DE60108579T2 (en) 2005-12-22
    US6536232B2 (en) 2003-03-25
    DE60108579D1 (en) 2005-03-03
    US20020053219A1 (en) 2002-05-09
    CA2357302A1 (en) 2002-03-19
    EP1189003A1 (en) 2002-03-20
    FR2814229B1 (en) 2002-10-25
    ZA200107210B (en) 2002-03-04
    FR2814229A1 (en) 2002-03-22

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