EP0677713A1 - Process and installation for the production of oxygen by distillation of air - Google Patents

Process and installation for the production of oxygen by distillation of air Download PDF

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Publication number
EP0677713A1
EP0677713A1 EP95400752A EP95400752A EP0677713A1 EP 0677713 A1 EP0677713 A1 EP 0677713A1 EP 95400752 A EP95400752 A EP 95400752A EP 95400752 A EP95400752 A EP 95400752A EP 0677713 A1 EP0677713 A1 EP 0677713A1
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EP
European Patent Office
Prior art keywords
pressure column
low pressure
column
air
level
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EP95400752A
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German (de)
French (fr)
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EP0677713B1 (en
Inventor
Yves Koeberle
Philippe Fraysse
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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    • 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
    • F25J3/04006—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
    • F25J3/04103—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 using solely hydrostatic liquid head
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04642—Recovering noble gases from air
    • F25J3/04648—Recovering noble gases from air argon
    • F25J3/04654—Producing crude argon in a crude argon column
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/92—Details relating to the feed point
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/58—Argon
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/40—One fluid being air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen

Definitions

  • the present invention relates to a method and an installation for the production of oxygen by air distillation and more particularly to a method and an installation for the production of oxygen under pressure.
  • EP-A-422,974 describes a process for the production of oxygen under pressure by cryogenic distillation of air in a double column. Liquid oxygen is withdrawn from the tank of the low pressure column 7, as illustrated in FIG. 1, and is vaporized in the auxiliary exchanger 9 by heat exchange with a fraction of the supply air. The remaining part of the supply air is divided into two flows, one of which goes directly to the medium pressure column 6, via line 14, and the other of which is expanded in a turbine 4 before being sent at the low pressure column 7.
  • a first object of this invention is to reduce the costs of the energy used by a process for producing pressurized oxygen compared to those of known processes.
  • a second object of this invention is to improve the argon yields in the case where the installation also includes an argon column supplied by the low pressure column.
  • the subject of the invention is a process for the production of gaseous oxygen under pressure by cryogenic distillation of air in a double column comprising a medium pressure column and a low pressure column, in which the rich liquid from the medium pressure column in first and second liquid fractions which are sent to different levels in the low pressure column, characterized in that the different levels are below a level of drawing off impure nitrogen from the column low pressure.
  • the rich liquid of the medium pressure column is divided into first and second fractions and the first and second fractions are sent to different levels in the low pressure column after sub-cooling. prior. This notably makes it possible to substantially improve the extraction of argon in the case where the installation also comprises an argon column.
  • the two fractions can be sent to the low pressure column at different temperatures, in order to further improve the reflux in the low pressure column and the extraction of argon in the case where the installation also includes an argon column.
  • part of the supply air is expanded before being sent to the double column, the remaining part of the supply air being partially condensed in the auxiliary exchanger.
  • the temperature difference in the auxiliary exchanger can be reduced to an average value of 0.6 ° C.
  • the invention also relates to an installation for producing gaseous oxygen under pressure by cryogenic distillation of air comprising a double column, consisting of at least one medium pressure column surmounted by a column of a low pressure column, means for withdrawing impure nitrogen from the low pressure column, and means for withdrawing rich liquid from the tank of the medium pressure column and sending it to two different levels of the low pressure column, located below the withdrawal level impure nitrogen.
  • the installation shown in FIG. 1 essentially comprises a main air compressor 1 with variable flow rate, for example of the centrifugal type with moving blades, an air blower with moving blades 2, a heat exchange line 3, a turbine 4 for keeping cold, an air distillation apparatus 5 constituted by a double column itself comprising a medium pressure column 6 surmounted by a low pressure column 7 and a minaret 7A, a vaporizer-condenser 8, a heat exchanger auxiliary heat 9 and a pump 10.
  • This installation is intended to produce a variable flow of gaseous oxygen via a line 12, under a pressure greater than atmospheric pressure.
  • the nominal flow of air to be treated, compressed to 6 bar by compressor 1, cooled to room temperature and purified, is divided into two fractions.
  • the first fraction is boosted by the booster 2 and the second fraction goes directly to the exchange line 3 where it is divided into two flows, each having a constant flow: -
  • a first flow is cooled in passages of the exchange line; a portion has left this exchange line after partial cooling, expanded to 1 bar in the turbine 4 and blown into the low pressure column 7 near its dew point; a second flow continues to cool down to the vicinity of its dew point under 6 bar, then is injected at the bottom of the medium pressure column 6 via a pipe 14.
  • the first overpressed fraction is cooled to the vicinity of its dew point in passages of the exchange line and then condensed in the auxiliary exchanger 9 and is divided into a first constant flow expanded under 6 bar sent to the medium pressure column. via a line 16, and a second constant flow expanded to around 1 bar in an expansion valve 13 then injected into the low pressure column 7.
  • the vaporizer-condenser 8 vaporizes a constant flow of liquid oxygen in the bottom of the low pressure column by condensing a roughly equal flow of nitrogen from the top of the medium pressure column.
  • "Rich liquid” oxygen-enriched air
  • "lean liquid” nitrogen approximately pure taken at the head of the medium pressure column and expanded to around 1 bar in an expansion valve 19 is injected at the top of the low pressure column.
  • Liquid nitrogen is injected at the top of the minaret 7A through the expansion valve 21. Pure nitrogen is withdrawn from the top of the minaret 7A and sent to the exchange line 3 to be reheated before coming out through the line 20. The impure nitrogen leaves via line 25 from the top of the low pressure column 7 and is sent to the outside via line 18.
  • Liquid oxygen withdrawn from the tank of the low pressure column 7 is pumped to production pressure before being vaporized in the auxiliary exchanger 9 (constituted by a "film” type vaporizer) by heat exchange with the air that partially condenses there.
  • the vaporized oxygen leaves, after heating in the exchange line 3, via line 12.
  • an argon-rich fraction is drawn from the lower part of the low pressure column 7 and is sent to the argon column 16 for distillation.
  • This fraction mainly comprises argon and oxygen.
  • the tank liquid resulting from the distillation in column 16 is returned to the lower part of the low pressure column 7.
  • the overhead condenser 29 of the argon column 16 is cooled by rich liquid coming from the tank of the medium pressure column 6 , expanded by valve 23, vaporized and sent to the low pressure column.
  • the remaining part of the rich liquid from the tank of the medium pressure column 6 is expanded by the valve 18 to a pressure slightly above atmospheric pressure and sent into the low pressure column 7 by the valve 18, substantially at the same level as the injection level of the air expanded by the turbine 4 (the blowing air).
  • the installation shown in FIG. 2 differs from the prior art in that all the air which is not overpressed by the booster 2 is sent to the turbine 4 to be expanded and sent to the low pressure column 7.
  • the pressurized and partially condensed air in the auxiliary exchanger 9 is entirely injected into the tank of the medium pressure column 6.
  • the remaining part of rich liquid not vaporized at 29 is divided into two fractions: a first fraction is injected, as shown in FIG. 1, after expansion by the valve 18 in the low pressure column 7 at the level of the air supply and the second fraction of rich liquid is sent to the low pressure column 7, after expansion to the pressure of the latter by the valve 17, at an intermediate level between the level of injection of the first fraction of rich liquid through the valve 18 and the level of withdrawal of nitrogen through the line 25.
  • FIG. 3 has only one air compressor 1, all the compressed air being sent either to the turbine 4 or to the exchanger 9.
  • the partially condensed air in the exchanger 9 passes entirely to the tank of the medium pressure column 6.
  • the difference in level between the level of liquid oxygen in the tank of the LP column and its entry into the vaporizer 9 fixes, in this case, the vaporization pressure of the oxygen; the pump 10 in Figure 2 is therefore deleted.
  • the fractions of rich liquid can be sub-cooled so that the temperature of the fraction injected at the level of air blowing is lower than that of the fraction injected at the intermediate level.
  • This arrangement of the exchanger 9 allows a gain of about 6% on the compression of the air and therefore on the specific energy of the oxygen produced.

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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)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

Producing gaseous oxygen under pressure from the cryogenic distn. of air in a double column (5) comprising a medium pressure column (6) and a low pressure column (7), comprises dividing the enriched liq. from the medium pressure column into first and second liq. fractions which are sent to different levels in the low pressure column. These different levels are below the extn. level of impure nitrogen from the low pressure column. The appts. to carry out the above process comprises a double distn. column (medium and low pressure columns), a means for extracting impure nitrogen from the low pressure column, and a means for extracting enriched liq. from the base of the medium pressure column and sending it to two levels in the low pressure column below the nitrogen extn. level. <IMAGE>

Description

La présente invention est relative à un procédé et une installation pour la production de l'oxygène par distillation d'air et plus particulièrement à un procédé et une installation pour la production de l'oxygène sous pression.The present invention relates to a method and an installation for the production of oxygen by air distillation and more particularly to a method and an installation for the production of oxygen under pressure.

EP-A-422.974 décrit un procédé de production d'oxygène sous pression par distillation cryogénique d'air dans une double colonne. L'oxygène liquide est soutiré de la cuve de la colonne basse pression 7, comme illustré à la figure 1, et se vaporise dans l'échangeur auxiliaire 9 par échange de chaleur avec une fraction de l'air d'alimentation. La partie restante de l'air d'alimentation est divisée en deux débits, dont l'un va directement à la colonne moyenne pression 6, via la conduite 14, et dont l'autre est détendu dans une turbine 4 avant d'être envoyé à la colonne basse pression 7.EP-A-422,974 describes a process for the production of oxygen under pressure by cryogenic distillation of air in a double column. Liquid oxygen is withdrawn from the tank of the low pressure column 7, as illustrated in FIG. 1, and is vaporized in the auxiliary exchanger 9 by heat exchange with a fraction of the supply air. The remaining part of the supply air is divided into two flows, one of which goes directly to the medium pressure column 6, via line 14, and the other of which is expanded in a turbine 4 before being sent at the low pressure column 7.

Un premier objet de cette invention est de réduire les coûts de l'énergie utilisée par un procédé de production d'oxygène sous pression par rapport à ceux des procédés connus.A first object of this invention is to reduce the costs of the energy used by a process for producing pressurized oxygen compared to those of known processes.

Un deuxième objet de cette invention est d'améliorer les rendements d'argon dans le cas où l'installation comprend également une colonne argon alimentée par la colonne basse pression.A second object of this invention is to improve the argon yields in the case where the installation also includes an argon column supplied by the low pressure column.

A cet effet, l'invention a pour objet un procédé de production d'oxygène gazeux sous pression par distillation cryogénique d'air dans une double colonne comprenant une colonne moyenne pression et une colonne basse pression, dans lequel on divise du liquide riche provenant de la colonne moyenne pression en une première et une deuxième fractions liquides que l'on envoie à des niveaux différents dans la colonne basse pression, caractérisé en ce que les niveaux différents sont au dessous d'un niveau de soutirage d'azote impur de la colonne basse pression.To this end, the subject of the invention is a process for the production of gaseous oxygen under pressure by cryogenic distillation of air in a double column comprising a medium pressure column and a low pressure column, in which the rich liquid from the medium pressure column in first and second liquid fractions which are sent to different levels in the low pressure column, characterized in that the different levels are below a level of drawing off impure nitrogen from the column low pressure.

Afin d'améliorer le reflux de la colonne basse pression, on divise le liquide riche de la colonne moyenne pression en une première et une deuxième fractions et on envoie les première et deuxième fractions à des niveaux différents dans la colonne basse pression après sous-refroidissement préalable. Ceci permet notamment d'améliorer sensiblement l'extraction d'argon dans le cas où l'installation comprend également une colonne argon.In order to improve the reflux of the low pressure column, the rich liquid of the medium pressure column is divided into first and second fractions and the first and second fractions are sent to different levels in the low pressure column after sub-cooling. prior. This notably makes it possible to substantially improve the extraction of argon in the case where the installation also comprises an argon column.

Les deux fractions peuvent être envoyées dans la colonne basse pression à des températures différentes, ce afin d'améliorer encore les reflux dans la colonne basse pression et l'extraction d'argon dans le cas où l'installation comprend également une colonne argon.The two fractions can be sent to the low pressure column at different temperatures, in order to further improve the reflux in the low pressure column and the extraction of argon in the case where the installation also includes an argon column.

De préférence, une partie de l'air d'alimentation est détendue avant d'être envoyée à la double colonne, la partie restante de l'air d'alimentation étant partiellement condensée dans l'échangeur auxiliaire.Preferably, part of the supply air is expanded before being sent to the double column, the remaining part of the supply air being partially condensed in the auxiliary exchanger.

Quand l'air ne se condense que partiellement dans l'échangeur auxiliaire, I'échange de chaleur avec l'oxygène sous pression s'effectue à une température moyenne plus chaude que s'il se condensait totalement.When the air only partially condenses in the auxiliary exchanger, the heat exchange with the pressurized oxygen takes place at an average temperature hotter than if it condensed completely.

Pour un même écart de température dans l'échangeur auxiliaire, on peut donc réduire la pression de l'air. En utilisant un vaporiseur à film comme échangeur auxiliaire, tel que décrit en EP-A-130.122, I'écart de température peut être réduit à une valeur moyenne de 0,6°C.For the same temperature difference in the auxiliary exchanger, it is therefore possible to reduce the air pressure. By using a film vaporizer as an auxiliary exchanger, as described in EP-A-130.122, the temperature difference can be reduced to an average value of 0.6 ° C.

L'invention a également pour objet une installation de production d'oxygène gazeux sous pression par distillation cryogénique d'air comprenant une double colonne, constituée par au moins une colonne moyenne pression surmontée d'une colonne d'une colonne basse pression, des moyens pour soutirer de l'azote impur de la colonne basse pression, et des moyens pour soutirer du liquide riche de la cuve de la colonne moyenne pression et l'envoyer à deux niveaux différents de la colonne basse pression, situés en dessous du niveau de soutirage de l'azote impur.The invention also relates to an installation for producing gaseous oxygen under pressure by cryogenic distillation of air comprising a double column, consisting of at least one medium pressure column surmounted by a column of a low pressure column, means for withdrawing impure nitrogen from the low pressure column, and means for withdrawing rich liquid from the tank of the medium pressure column and sending it to two different levels of the low pressure column, located below the withdrawal level impure nitrogen.

L'inconvénient principal des oxytonnes à pompe résulte de la surpression de l'air à sa pression de condensation. Si l'oxygène doit être pompé à des pressions conséquentes telles qu'il soit nécessaire de supresser l'air à une pression supérieure à celle de la colonne moyenne pression, cette invention ne présente pas d'intérêt puisque l'on dépense globalement plus d'énergie de compression avec cette situation, étant donné que le débit d'air surpressé est approximativement trois fois supérieur à celui du système selon EP-A-422.974, si tout l'air non turbiné passe à l'échangeur auxiliaire.The main drawback of pump oxytonnes results from the overpressure of air at its condensing pressure. If the oxygen has to be pumped at consequent pressures such that it is necessary to supress the air at a pressure higher than that of the medium pressure column, this invention is of no interest since more than one spends compression energy with this situation, since the pressure air flow is approximately three times that of the system according to EP-A-422,974, if all the non-turbinated air passes to the auxiliary exchanger.

Si le reflux de tête de la colonne basse pression est faible, lorsqu'on veut séparer l'argon selon une méthode classique de distillation dans une colonne en parallèle avec la colonne basse pression, ceci conduit à un mauvais rendement en argon.If the head reflux of the low pressure column is low, when it is desired to separate the argon according to a conventional distillation method in a column in parallel with the low pressure column, this leads to a poor yield of argon.

Cette réduction du reflux de tête peut être due à plusieurs facteurs :This reduction in head reflux can be due to several factors:

Si de l'air est condensé dans un vaporiseur d'oxygène ne participe pas à la distillation dans la colonne moyenne pression et donc ne participe pas au chauffage dans le vaporiseur principal en cuve de la colonne basse pression. Ainsi, la quantité d'azote liquide pour le reflux de tête de la colonne basse pression est réduite.If air is condensed in an oxygen vaporizer, it does not participate in the distillation in the medium pressure column and therefore does not participate in the heating in the main vaporizer in the bottom of the low pressure column. Thus, the amount of liquid nitrogen for the head reflux of the low pressure column is reduced.

Il en est de même si l'air turbiné est envoyé uniquement dans la colonne basse pression, réduisant encore plus le reflux de tête de la colonne basse pression.The same is true if the turbined air is sent only to the low pressure column, further reducing the head reflux of the low pressure column.

Pour pallier ces défauts, on proposait dans EP-A-422.974 d'envoyer une partie de l'air condensé dans la colonne moyenne pression, quelques plateaux au-dessus de la cuve pour qu'elle puisse participer, au moins faiblement, à la distillation dans cette colonne.To overcome these defects, it was proposed in EP-A-422.974 to send part of the condensed air in the medium pressure column, a few trays above the tank so that it can participate, at least weakly, in the distillation in this column.

Or, dans la présente invention, pour compenser les pertes de reflux, due par exemple, au fait que la phase liquide de l'air condensé dans le vaporiseur extérieur se retrouve dans le liquide riche en cuve de la colonne moyenne pression, ce liquide riche est divisé en deux fractions :

  • une première fraction est envoyée dans la colonne basse pression à un premier niveau, habituellement au niveau de l'insufflation d'air dans le cas où il y a une turbine d'insufflation ;
  • une deuxième fraction est envoyée dans la colonne basse pression à un niveau intermédiaire entre le premier niveau et le niveau de soutirage d'azote impur.
However, in the present invention, to compensate for the reflux losses, due for example, to the fact that the liquid phase of the air condensed in the external vaporizer is found in the liquid rich in the bottom of the medium pressure column, this rich liquid is divided into two fractions:
  • a first fraction is sent to the low pressure column at a first level, usually at the level of air insufflation in the case where there is an insufflation turbine;
  • a second fraction is sent to the low pressure column at an intermediate level between the first level and the level of withdrawal of impure nitrogen.

Il est clair que cette disposition des niveaux d'injection peut présenter un intérêt pour des procédés de distribution cryogénique autres que celui décrit dans la présente demande.It is clear that this arrangement of the injection levels may be of interest for cryogenic distribution methods other than that described in the present application.

Des exemples de mise en oeuvre de l'invention et de l'art antérieur vont maintenant être décrits en regard des dessins annexés, sur lesquels :

  • la figure 1 représente schématiquement un mode de réalisation de l'installation selon l'art antérieur ; et
  • les figures 2 et 3 représentent schématiquement deux modes de réalisation de l'installation conforme à l'invention.
Examples of implementation of the invention and of the prior art will now be described with reference to the accompanying drawings, in which:
  • FIG. 1 schematically represents an embodiment of the installation according to the prior art; and
  • Figures 2 and 3 schematically represent two embodiments of the installation according to the invention.

L'installation représentée à la figure 1 comprend essentiellement un compresseur d'air principal 1 à débit variable, par exemple du type centrifuge à aubages mobiles, un surpresseur d'air à aubages mobiles 2, une ligne d'échange thermique 3, une turbine 4 de maintien en froid, un appareil 5 de distillation d'air constitué par une double colonne comprenant elle-même une colonne moyenne pression 6 surmontée d'une colonne basse pression 7 et un minaret 7A, un vaporiseur-condenseur 8, un échangeur de chaleur auxiliaire 9 et une pompe 10. Cette installation est destinée à produire un débit variable d'oxygène gazeux via une conduite 12, sous une pression supérieure à la pression atmosphérique.The installation shown in FIG. 1 essentially comprises a main air compressor 1 with variable flow rate, for example of the centrifugal type with moving blades, an air blower with moving blades 2, a heat exchange line 3, a turbine 4 for keeping cold, an air distillation apparatus 5 constituted by a double column itself comprising a medium pressure column 6 surmounted by a low pressure column 7 and a minaret 7A, a vaporizer-condenser 8, a heat exchanger auxiliary heat 9 and a pump 10. This installation is intended to produce a variable flow of gaseous oxygen via a line 12, under a pressure greater than atmospheric pressure.

Le débit nominal d'air à traiter, comprimé à 6 bar par le compresseur 1, refroidi à la température ambiante et épuré, est divisé en deux fractions. La première fraction est surpressée par le surpresseur 2 et la deuxième fraction passe directement à la ligne d'échange 3 où elle est divisée en deux flux ayant chacun un débit constant :
   - un premier flux est refroidi dans des passages de la ligne d'échange; une partie est sortie de cette ligne d'échange après un refroidissement partiel, détendue vers 1 bar dans la turbine 4 et insufflée dans la colonne basse pression 7 au voisinage de son point de rosée ; un second flux poursuit son refroidissement jusqu'au voisinage de son point de rosée sous 6 bar, puis est injecté au bas de la colonne moyenne pression 6 via une conduite 14.The nominal flow of air to be treated, compressed to 6 bar by compressor 1, cooled to room temperature and purified, is divided into two fractions. The first fraction is boosted by the booster 2 and the second fraction goes directly to the exchange line 3 where it is divided into two flows, each having a constant flow:
- A first flow is cooled in passages of the exchange line; a portion has left this exchange line after partial cooling, expanded to 1 bar in the turbine 4 and blown into the low pressure column 7 near its dew point; a second flow continues to cool down to the vicinity of its dew point under 6 bar, then is injected at the bottom of the medium pressure column 6 via a pipe 14.

La première fraction surpressée est refroidie jusqu'au voisinage de son point de rosée dans des passages de la ligne d'échange puis condensée dans l'échangeur auxiliaire 9 et est divisée en un premier débit constant détendu sous 6 bar envoyé dans la colonne moyenne pression via une conduite 16, et un second débit constant détendu vers 1 bar dans une vanne de détente 13 puis injecté dans la colonne basse pression 7.The first overpressed fraction is cooled to the vicinity of its dew point in passages of the exchange line and then condensed in the auxiliary exchanger 9 and is divided into a first constant flow expanded under 6 bar sent to the medium pressure column. via a line 16, and a second constant flow expanded to around 1 bar in an expansion valve 13 then injected into the low pressure column 7.

Le vaporiseur-condenseur 8 vaporise un débit constant d'oxygène liquide en cuve de la colonne basse pression par condensation d'un débit à peu près égal d'azote de tête de la colonne moyenne pression. Du "liquide riche" (air enrichi en oxygène) prélevé en cuve de la colonne moyenne pression et détendu vers 1 bar dans une vanne de détente 18 est injecté à un niveau intermédiaire de la colonne basse pression, et du "liquide pauvre" (azote à peu près pur) prélevé en tête de la colonne moyenne pression et détendu vers 1 bar dans une vanne de détente 19 est injecté au sommet de la colonne basse pression.The vaporizer-condenser 8 vaporizes a constant flow of liquid oxygen in the bottom of the low pressure column by condensing a roughly equal flow of nitrogen from the top of the medium pressure column. "Rich liquid" (oxygen-enriched air) taken from the tank of the medium pressure column and expanded to 1 bar in an expansion valve 18 is injected at an intermediate level of the low pressure column, and "lean liquid" (nitrogen approximately pure) taken at the head of the medium pressure column and expanded to around 1 bar in an expansion valve 19 is injected at the top of the low pressure column.

De l'azote liquide est injecté au sommet du minaret 7A à travers la vanne de détente 21. De l'azote pur est soutiré du sommet du minaret 7A et envoyé à la ligne d'échange 3 pour y être réchauffé avant de ressortir par la conduite 20. L'azote impur sort par la conduite 25 du sommet de la colonne basse pression 7 et est envoyé à l'extérieur par la conduite 18.Liquid nitrogen is injected at the top of the minaret 7A through the expansion valve 21. Pure nitrogen is withdrawn from the top of the minaret 7A and sent to the exchange line 3 to be reheated before coming out through the line 20. The impure nitrogen leaves via line 25 from the top of the low pressure column 7 and is sent to the outside via line 18.

L'oxygène liquide soutiré de la cuve de la colonne basse pression 7 est pompé à la pression de production avant d'être vaporisé dans l'échangeur auxiliaire 9 (constitué par un vaporiseur du type "à film") par échange de chaleur avec l'air qui s'y condense partiellement. L'oxygène vaporisé sort, après réchauffement dans la ligne d'échange 3, par la conduite 12.Liquid oxygen withdrawn from the tank of the low pressure column 7 is pumped to production pressure before being vaporized in the auxiliary exchanger 9 (constituted by a "film" type vaporizer) by heat exchange with the air that partially condenses there. The vaporized oxygen leaves, after heating in the exchange line 3, via line 12.

Pour produire de l'argon, une fraction riche en argon est soutirée de la partie inférieure de la colonne basse pression 7 et est envoyée à la colonne d'argon 16 pour y être distillée. Cette fraction comprend essentiellement de l'argon et de l'oxygène. Le liquide de cuve résultant de la distillation dans la colonne 16 est renvoyée en partie inférieure de la colonne basse pression 7. Le condenseur de tête 29 de la colonne argon 16 est refroidi par du liquide riche provenant de la cuve de la colonne moyenne pression 6, détendu par la vanne 23, vaporisé et envoyé à la colonne basse pression.To produce argon, an argon-rich fraction is drawn from the lower part of the low pressure column 7 and is sent to the argon column 16 for distillation. This fraction mainly comprises argon and oxygen. The tank liquid resulting from the distillation in column 16 is returned to the lower part of the low pressure column 7. The overhead condenser 29 of the argon column 16 is cooled by rich liquid coming from the tank of the medium pressure column 6 , expanded by valve 23, vaporized and sent to the low pressure column.

La partie restante du liquide riche de la cuve de la colonne moyenne pression 6 est détendu par la vanne 18 à une pression légèrement au-dessus de la pression atmosphérique et envoyée dans la colonne basse pression 7 par la vanne 18, sensiblement au même niveau que le niveau d'injection de l'air détendu par la turbine 4 (l'air d'insufflation).The remaining part of the rich liquid from the tank of the medium pressure column 6 is expanded by the valve 18 to a pressure slightly above atmospheric pressure and sent into the low pressure column 7 by the valve 18, substantially at the same level as the injection level of the air expanded by the turbine 4 (the blowing air).

L'installation représentée à la figure 2 diffère de l'art antérieur par le fait que tout l'air qui n'est pas surpressé par le surpresseur 2 est envoyé à la turbine 4 pour être détendu et envoyé à la colonne basse pression 7. L'air surpressé et partiellement condensé dans l'échangeur 9 auxiliaire est entièrement injecté en cuve de la colonne moyenne pression 6.The installation shown in FIG. 2 differs from the prior art in that all the air which is not overpressed by the booster 2 is sent to the turbine 4 to be expanded and sent to the low pressure column 7. The pressurized and partially condensed air in the auxiliary exchanger 9 is entirely injected into the tank of the medium pressure column 6.

Pour améliorer le rendement en argon, la partie restante de liquide riche non vaporisée en 29 est divisée en deux fractions : une première fraction est injectée, comme représenté sur la figure 1, après détente par la vanne 18 dans la colonne basse pression 7 au niveau de l'insufflation d'air et la deuxième fraction de liquide riche est envoyée à la colonne basse pression 7, après détente à la pression de celle-ci par la vanne 17, à un niveau intermédiaire entre le niveau d'injection de la première fraction de liquide riche à travers la vanne 18 et le niveau de soutirage d'azote à travers la conduite 25.To improve the argon yield, the remaining part of rich liquid not vaporized at 29 is divided into two fractions: a first fraction is injected, as shown in FIG. 1, after expansion by the valve 18 in the low pressure column 7 at the level of the air supply and the second fraction of rich liquid is sent to the low pressure column 7, after expansion to the pressure of the latter by the valve 17, at an intermediate level between the level of injection of the first fraction of rich liquid through the valve 18 and the level of withdrawal of nitrogen through the line 25.

Dans le cas où l'oxygène liquide est pressurisé à une pression dite concomitante à la pression de la colonne moyenne pression (c'est-à-dire à environ 2 bar), le système de la figure 2 peut être simplifié.In the case where the liquid oxygen is pressurized at a pressure called concomitant with the pressure of the medium pressure column (that is to say at about 2 bar), the system of FIG. 2 can be simplified.

La variante de la figure 3 ne comporte qu'un seul compresseur d'air 1, tout l'air comprimé étant envoyé soit à la turbine 4, soit à l'échangeur 9. L'air partiellement condensé dans l'échangeur 9 passe entièrement à la cuve de la colonne moyenne pression 6. La dénivellation entre le niveau d'oxygène liquide de la cuve de la colonne BP et son entrée dans le vaporiseur 9 fixe, dans ce cas, la pression de vaporisation de l'oxygène ; la pompe 10 de la figure 2 est donc supprimée.The variant of FIG. 3 has only one air compressor 1, all the compressed air being sent either to the turbine 4 or to the exchanger 9. The partially condensed air in the exchanger 9 passes entirely to the tank of the medium pressure column 6. The difference in level between the level of liquid oxygen in the tank of the LP column and its entry into the vaporizer 9 fixes, in this case, the vaporization pressure of the oxygen; the pump 10 in Figure 2 is therefore deleted.

Si besoin est, on peut sous-refroidir les fractions de liquide riche pour que la température de la fraction injectée au niveau de l'insufflation d'air soit moins élevée que celle de la fraction injectée au niveau intermédiaire.If necessary, the fractions of rich liquid can be sub-cooled so that the temperature of the fraction injected at the level of air blowing is lower than that of the fraction injected at the intermediate level.

Cette disposition de l'échangeur 9 permet un gain d'environ 6 % sur la compression de l'air et donc sur l'énergie spécifique de l'oxygène produit.This arrangement of the exchanger 9 allows a gain of about 6% on the compression of the air and therefore on the specific energy of the oxygen produced.

Cette disposition des niveaux d'injection du liquide riche permet d'obtenir un gain de production d'argon d'environ 5 %, en comparaison avec celle de EP-A422.974. Le rendement obtenu avec le procédé de la présente invention est d'environ 80 %.This arrangement of the injection levels of the rich liquid makes it possible to obtain a gain in the production of argon of approximately 5%, in comparison with that of EP-A422,974. The yield obtained with the process of the present invention is approximately 80%.

Claims (10)

Procédé de production d'oxygène gazeux sous pression par distillation cryogénique d'air dans une double colonne (5) comprenant une colonne moyenne pression (6) et une colonne basse pression (7), dans lequel on divise du liquide riche provenant de la colonne moyenne pression en une première et une deuxième fractions liquides que l'on envoie à des niveaux différents dans la colonne basse pression (7), caractérisé en ce que les niveaux différents sont au dessous d'un niveau de soutirage d'azote impur de la colonne basse pression (7).Process for the production of gaseous oxygen under pressure by cryogenic distillation of air in a double column (5) comprising a medium pressure column (6) and a low pressure column (7), in which the rich liquid from the column is divided medium pressure in first and second liquid fractions which are sent to different levels in the low pressure column (7), characterized in that the different levels are below a level of withdrawal of impure nitrogen from the low pressure column (7). Procédé selon la revendication 1, dans lequel on soutire un fluide enrichi en argon de la colonne basse pression (7) et on le distille dans une colonne (16).The method of claim 1, wherein a fluid enriched in argon is drawn from the low pressure column (7) and distilled in a column (16). Procédé selon l'une des revendications 1 ou 2 dans lequel on soutire un liquide enrichi en oxygène d'une partie inférieure de la colonne basse pression (7).Method according to one of claims 1 or 2 wherein a liquid enriched in oxygen is withdrawn from a lower part of the low pressure column (7). Procédé selon l'une des revendications précédentes, dans lequel les deux fractions sont refroidies à des températures différentes avant d'être envoyées dans la colonne basse pression (7).Method according to one of the preceding claims, in which the two fractions are cooled to different temperatures before being sent to the low pressure column (7). Procédé selon l'une des revendications précédentes, dans lequel, une partie de l'air d'alimentation est insufflée à un niveau intermédiaire de la colonne basse pression (7) et les niveaux d'injection de liquide riche ne sont pas au-dessous de ce niveau intermédiaire.Method according to one of the preceding claims, in which part of the supply air is blown at an intermediate level of the low pressure column (7) and the levels of injection of rich liquid are not below. of this intermediate level. Installation de production d'oxygène gazeux sous pression par distillation cryogénique d'air comprenant une double colonne (5), constituée par au moins une colonne moyenne pression (6) surmontée d'une colonne basse pression (7), des moyens (12) pour soutirer de l'azote impur de la colonne basse pression (25), et des moyens pour soutirer du liquide riche de la cuve de la colonne moyenne pression (6) et l'envoyer à deux niveaux différents de la colonne basse pression (7), situés en dessous du niveau de soutirage de l'azote impur.Installation for producing gaseous oxygen under pressure by cryogenic distillation of air comprising a double column (5), constituted by at least one medium pressure column (6) surmounted by a low pressure column (7), means (12) for withdrawing impure nitrogen from the low pressure column (25), and means for withdrawing rich liquid from the tank of the medium pressure column (6) and sending it to two different levels of the low pressure column (7 ), located below the level of withdrawal of impure nitrogen. Installation selon la revendication 6, comprenant une colonne de distillation d'argon (16).Installation according to claim 6, comprising an argon distillation column (16). Installation selon l'une des revendications 6 et 7, comprenant des moyens (12) pour soutirer un liquide enrichi en oxygène de la partie inférieure de la colonne basse pression (7).Installation according to one of claims 6 and 7, comprising means (12) for withdrawing an oxygen-enriched liquid from the lower part of the low pressure column (7). Installation selon l'une des revendications 6 à 8, comprenant des moyens pour envoyer le liquide riche dans la colonne basse pression (7) à deux températures différentes.Installation according to one of claims 6 to 8, comprising means for sending the rich liquid into the low pressure column (7) at two different temperatures. Installation selon l'une des revendications 6 à 9, comprenant des moyens (4) pour envoyer de l'air à un niveau intermédiaire de la colonne basse pression (7) et des moyens pour envoyer les deux fractions de liquide riche à des niveaux dans le voisinage de ou au-dessus du niveau intermédiaire.Installation according to one of claims 6 to 9, comprising means (4) for sending air to an intermediate level of the low pressure column (7) and means for sending the two fractions of rich liquid to levels in the vicinity of or above the intermediate level.
EP95400752A 1994-04-12 1995-04-04 Process and installation for the production of oxygen by distillation of air Expired - Lifetime EP0677713B1 (en)

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FR9404298A FR2718518B1 (en) 1994-04-12 1994-04-12 Process and installation for the production of oxygen by air distillation.

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FR2854232A1 (en) * 2003-04-23 2004-10-29 Air Liquide Air separation procedure to produce argon uses cryogenic distillation with additional liquid flow containing 18-30 mol percent oxygen fed to low pressure column

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CN1121172A (en) 1996-04-24
JPH0854181A (en) 1996-02-27
DE69512821D1 (en) 1999-11-25
FR2718518B1 (en) 1996-05-03
US5586451A (en) 1996-12-24
CA2146831A1 (en) 1995-10-13
DE69512821T2 (en) 2000-05-25
FR2718518A1 (en) 1995-10-13
EP0677713B1 (en) 1999-10-20

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