EP0547946B1 - Process and apparatus for the production of impure oxygen - Google Patents

Process and apparatus for the production of impure oxygen Download PDF

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Publication number
EP0547946B1
EP0547946B1 EP92403330A EP92403330A EP0547946B1 EP 0547946 B1 EP0547946 B1 EP 0547946B1 EP 92403330 A EP92403330 A EP 92403330A EP 92403330 A EP92403330 A EP 92403330A EP 0547946 B1 EP0547946 B1 EP 0547946B1
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EP
European Patent Office
Prior art keywords
column
pressure column
nitrogen
medium pressure
condenser
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Expired - Lifetime
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EP92403330A
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German (de)
French (fr)
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EP0547946A1 (en
EP0547946B2 (en
Inventor
Jean-Louis Girault
Philippe Mazières
Jean-Pierre Tranier
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Priority to EP96200235A priority Critical patent/EP0713069B1/en
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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
    • F25J3/04151—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
    • F25J3/04006—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
    • F25J3/0429—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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, 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
    • F25J3/04406—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
    • F25J3/04418—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 with thermally overlapping high and low pressure columns
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • 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
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • 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
    • F25J2250/10—Boiler-condenser with superposed stages
    • 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
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/939—Partial feed stream expansion, air

Definitions

  • the present invention relates to a process for producing impure oxygen by air distillation in a double column air distillation installation, as well as to an air distillation installation, in accordance with the preambles of claims 1, 3 and 7, 9 respectively.
  • Such a method and such an installation are known, for example, from document US-A-5,069,699.
  • the applications concerned by the invention are those which consume large quantities of impure oxygen. These include the gasification processes for coal or petroleum residues, as well as the direct reduction-smelting processes of iron ore.
  • the object of the invention is to further reduce the energy expenditure necessary for the production of impure oxygen and to overcome the faults of the prior systems.
  • a second vaporization gas more volatile than said first vaporization gas but less volatile than the top nitrogen of the medium pressure column, can be condensed to an intermediate level between those of said condensations.
  • the invention also relates to a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column, comprising means for supplying the medium pressure column with air to be distilled under at minus around 9 bar absolute, and in that the low pressure column comprises at least two superposed vaporizers-condensers, including a tank vaporizer-condenser, means for supplying this tank vaporizer-condenser with a first vaporization gas less volatile than the nitrogen at the head of the medium pressure column, means for supplying the second vaporizer-condenser with nitrogen at the head of the medium pressure column, and means for sending the nitrogen thus condensed to reflux at the head of the column medium pressure, characterized in that the means for supplying the tank vaporizer-condenser comprise means for sending a gas withdrawn therein at an intermediate level of the medium pressure column or means for sending thereto approximately pure or impure nitrogen, compressed to a pressure higher than that of the medium pressure column.
  • the invention also relates to a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column, comprising means for supplying the medium pressure column with air to be distilled at at least about 9 bar absolute, and in that the low pressure column comprises at least three superposed vaporizers-condensers, including a tank vaporizer-condenser, means for supplying this tank vaporizer-condenser with a first vaporization gas less volatile than the top nitrogen of the medium pressure column, means for supplying the second vaporizer-condenser with nitrogen from the top of the medium pressure column, means for send the nitrogen thus condensed in reflux at the head of the medium pressure column, means for supplying the tank vaporizer-condenser comprising means for sending medium pressure air therein, means for supplying the intermediate vaporizer-condenser with a second gas less volatile than this top nitrogen and more volatile than said first vaporizing gas, characterized in that the second gas is a gas withdrawn from the double column e.
  • the installation shown in Figure 1 is intended to produce oxygen at a purity of the order of 85% under a pressure of the order of 7.4 bar absolute. It essentially comprises a double column 1 for air distillation, consisting of a medium pressure column (or “MP column”) 2 operating at 15.7 bar absolute and a low pressure column (or “LP column”) 3 operating at 6.3 bar absolute, a main heat exchange line 4, a sub-cooler 5, an auxiliary evaporator-condenser 6 and a turbine 7 for blowing air into the low pressure column.
  • Column 3 is superimposed on column 2 and contains in the tank a vaporizer-condenser 8 and, above this, a second vaporizer-condenser 9.
  • the air to be distilled arrives at medium pressure via a line 10 and enters the exchange line 4. Most of this air is cooled to the vicinity of its dew point and leaves the cold end of the line d 'exchange, the rest having left the exchange line at an intermediate temperature, expanded at low pressure in the turbine 7 to keep the installation cold, and blown at an intermediate level in the LP column 3.
  • a fraction of the fully cooled air is introduced, via a pipe 11, at the base of the column MP 2, and the rest is condensed in the vaporizer-condenser 6; part of the liquid obtained is introduced via a line 12 at an intermediate point in column 2, and the rest is, after sub-cooling in 5 and expansion in an expansion valve 13, introduced at an intermediate point in column BP 3 .
  • the "rich liquid” (oxygen-enriched air) collected in the bottom of the MP column is, after sub-cooling in 5 and expansion in an expansion valve 14, introduced at an intermediate point of the LP column.
  • “lean liquid” (impure nitrogen) withdrawn at an intermediate point of the column MP is, after sub-cooling in 5 and expansion in an expansion valve 15, introduced at the top of the column BP.
  • the approximately pure nitrogen produced at the head of the MP column is partly removed from the installation as a product, after heating in the exchange line, via a line 16, and, for the rest, sent in the form gas via a line 17, at medium pressure, in the upper evaporator-condenser 9. After condensation, this nitrogen is returned to reflux at the head of the column MP via a line 18.
  • impure nitrogen gas drawn off at an intermediate point in column 2 and, in this example, at the same level as the lean liquid, is sent via a line 19, under medium pressure, to the vaporizer-condenser lower 8.
  • the liquid thus obtained is returned under reflux to the column MP, at approximately the same level, via a line 20.
  • the pump 23 could be omitted, the impure oxygen then being vaporized at 6 under the low pressure.
  • the temperature of the bottom liquid of the LP column is determined by that of the gas condensed in this vaporizer-condenser.
  • the temperature of the tank liquid, which is impure oxygen is relatively high.
  • the pressure of the LP column that is to say the low pressure, can be increased.
  • impure oxygen and impure nitrogen are obtained under increased pressure, which makes it possible to make savings on their recovery, for example on the energy required to compress the impure nitrogen to the desired pressure in a gas turbine (not shown) coupled to the installation, for example as described in the aforementioned US-A-4,224,045.
  • the upper vaporizer-condenser 9 serves to provide the necessary reflux at the top of the column MP.
  • the impure oxygen is withdrawn in gaseous form from the LP column 3, and is simply reheated in the exchange line 4 before its evacuation via the pipe 24. This is particularly advantageous when the impure oxygen is desired under the low pressure. Consequently, the vaporizer-condenser 6 is eliminated.
  • a fraction of the medium pressure air cooled near its dew point is sent, via a line 26, to the lower vaporizer-condenser 8 in place of the intermediate gas of Figure 1.
  • This intermediate gas feeds an intermediate vaporizer-condenser 27 located between the lower vaporizers-condensers 8 and upper 9.
  • the liquefied air from the vaporizer-condenser 8 is sent partly, via a line 28, to the column MP and partly, after sub-cooling in 5 and expansion in the expansion valve 13, in the column BP.
  • the impure oxygen is withdrawn in liquid form from the tank of the LP column, then is brought by a pump 23 to the desired production pressure, then vaporized and heated under this pressure in the exchange line 4 before being evacuated from the installation via line 24.
  • a nitrogen cycle is provided, known as the rectification support cycle, which is used at the same time to ensure the vaporization of impure oxygen: part of the nitrogen produced at the head of column 3 (which, in this case, has at the head a "minaret" 30 which is supplied at its top with pure liquid nitrogen coming from the upper evaporator-condenser 9 and which, consequently, produces pure nitrogen under low pressure) is, after heating in the exchange line, compressed by a compressor 31 at medium pressure.
  • the rectification support cycle which is used at the same time to ensure the vaporization of impure oxygen: part of the nitrogen produced at the head of column 3 (which, in this case, has at the head a "minaret" 30 which is supplied at its top with pure liquid nitrogen coming from the upper evaporator-condenser 9 and which, consequently, produces pure nitrogen under low pressure) is, after heating in the exchange line, compressed by a compressor 31 at medium pressure.
  • This medium pressure nitrogen combined with a current of medium pressure nitrogen taken from the line 16, is compressed again by a compressor 33 to a vaporization pressure of the impure oxygen compressed by the pump 23, liquefied in the line of exchange, then, after expansion in an expansion valve 34, introduced under reflux at the head of the column MP.
  • the installation of Figure 4 also includes a BP 3 column with minaret 30. However, unlike the previous case, it is high air pressure, boosted to a vaporization pressure of the impure oxygen by a booster 35, which ensures the vaporization of the impure oxygen in the exchange line 4. In this example, this air is, after liquefaction and expansion in a valve expansion valve 36 and in the expansion valve 13, distributed between the two columns 2 and 3. consequently, the compressor 33 and the expansion valve 34 of FIG. 3 are eliminated.
  • This nitrogen pressure can be chosen between medium pressure and the pressure for which the nitrogen condenses at the cold end of the exchange line .

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  • 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)

Description

La présente invention est relative à un procédé de production d'oxygène impur par distillation d'air dans une installation de distillation d'air à double colonne, ainsi qu'à une installation de distillation d'air, conformément aux préambules des revendications 1, 3 et 7, 9 respectivement. Un tel procédé et une telle installation sont connus, par exemple, du document US-A-5 069 699.The present invention relates to a process for producing impure oxygen by air distillation in a double column air distillation installation, as well as to an air distillation installation, in accordance with the preambles of claims 1, 3 and 7, 9 respectively. Such a method and such an installation are known, for example, from document US-A-5,069,699.

Les applications concernées par l'invention sont celles qui consomment de grandes quantités d'oxygène impur. On citera les procédés de gazéification de charbon ou de résidus pétroliers, ainsi que les procédés de réduction-fusion directe du minerai de fer.The applications concerned by the invention are those which consume large quantities of impure oxygen. These include the gasification processes for coal or petroleum residues, as well as the direct reduction-smelting processes of iron ore.

Il est connu que pour produire par distillation d'air de l'oxygène impur, c'est-à-dire ayant une pureté inférieure à 99,5 % et généralement inférieure à 98 %, il est possible de diminuer la dépense d'énergie en augmentant la pression de marche de la double colonne, à condition que l'on puisse valoriser l'énergie disponible dans la colonne basse pression sous forme de pression.It is known that to produce by distillation of air impure oxygen, that is to say having a purity of less than 99.5% and generally less than 98%, it is possible to reduce the energy expenditure by increasing the operating pressure of the double column, provided that the energy available in the low pressure column can be used in the form of pressure.

Un moyen connu de valoriser cette pression, décrit par exemple dans US-A-4.224.045, consiste à combiner l'appareil de distillation d'air à une turbine à gaz : l'air à séparer est prélevé totalement ou partiellement au refoulement du compresseur de cette turbine, et le gaz résiduaire basse pression de l'appareil de distillation est renvoyé après compression à la turbine à gaz, l'oxygène impur et l'azote étant envoyés vers l'utilisation sous la pression de la colonne qui les produit.One known means of developing this pressure, described for example in US-A-4,224,045, consists in combining the air distillation apparatus with a gas turbine: the air to be separated is taken wholly or partially at the discharge of the compressor of this turbine, and the low pressure waste gas from the distillation apparatus is returned after compression to the gas turbine, the impure oxygen and the nitrogen being sent to use under the pressure of the column which produces them .

De cette manière, la basse pression est entièrement valorisée et l'on obtient une énergie de séparation réduite.In this way, the low pressure is fully developed and a reduced separation energy is obtained.

Dans US-A-5.069.699, on décrit un procédé de distillation d'air dans une installation comprenant une double colonne et une colonne opérant à pression très élevée. Un des deux condenseurs de la colonne basse pression est alimenté par un débit d'air ou un débit d'azote provenant de la colonne opérant à pression très élevée.In US-A-5,069,699, an air distillation process is described in an installation comprising a double column and a column operating at very high pressure. One of the two condensers of the low pressure column is supplied by an air flow or a nitrogen flow coming from the column operating at very high pressure.

L'invention a pour but de réduire encore la dépense d'énergie nécessaire à la production de l'oxygène impur et de pallier les défauts des systèmes antérieurs.The object of the invention is to further reduce the energy expenditure necessary for the production of impure oxygen and to overcome the faults of the prior systems.

A cet effet, l'invention a pour objet un procédé de production d'oxygène impur dans une installation de distillation d'air à double colonne, la double colonne comprenant une colonne moyenne pression et une colonne basse pression comprenant les étapes de :

  • faire fonctionner la colonne moyenne pression sous une pression supérieure à 6 bar et de préférence au moins égale à 9 bar absolus environ ;
  • condenser dans un condenseur de cuve de la colonne basse pression un premier gaz de vaporisation moins volatil que l'azote de tête de la colonne moyenne pression ; et
  • condenser de l'azote de tête de la colonne moyenne pression que l'on envoie ensuite en reflux en tête de la colonne moyenne pression dans un deuxième condenseur, à un niveau de la colonne basse pression situé au-dessus dudit condenseur de cuve,
   caractérisé en ce que le premier gaz de vaporisation est un gaz soutiré à un niveau intermédiaire de la colonne moyenne pression ou de l'azote à peu près pur ou impur comprimé à une pression supérieure à celle de la colonne moyenne pression.To this end, the subject of the invention is a process for producing impure oxygen in a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column comprising the steps of:
  • operate the medium pressure column under a pressure greater than 6 bar and preferably at least equal to approximately 9 bar absolute;
  • condensing in a tank condenser of the low pressure column a first vaporization gas which is less volatile than the top nitrogen of the medium pressure column; and
  • condensing nitrogen from the top of the medium pressure column which is then sent to reflux at the top of the medium pressure column in a second condenser, at a level of the low pressure column located above said tank condenser,
characterized in that the first vaporizing gas is a gas withdrawn at an intermediate level from the medium pressure column or approximately pure or impure nitrogen compressed to a pressure higher than that of the medium pressure column.

On peut condenser un deuxième gaz de vaporisation, plus volatil que ledit premier gaz de vaporisation mais moins volatil que l'azote de tête de la colonne moyenne pression, à un niveau intermédiaire entre ceux desdites condensations.A second vaporization gas, more volatile than said first vaporization gas but less volatile than the top nitrogen of the medium pressure column, can be condensed to an intermediate level between those of said condensations.

L'invention a également pour objet un procédé de production d'oxygène impur par distillation d'air dans une installation de distillation d'air à double colonne, la double colonne comprenant une colonne moyenne pression et une colonne basse pression comprenant les étapes de :

  • faire fonctionner la colonne moyenne pression sous une pression supérieure à 6 bar et de préférence au moins égale à 9 bar absolus environ ;
  • condenser dans un condenseur de cuve de la colonne basse pression un premier gaz de vaporisation moins volatil que l'azote de tête de la colonne moyenne pression ; et
  • condenser de l'azote de tête de la colonne moyenne pression, que l'on envoie ensuite en reflux en tête de la colonne moyenne pression dans un deuxième condenseur, à un niveau de la colonne basse pression situé au-dessus dudit condenseur de cuve,
   le premier gaz de vaporisation étant de l'air à la pression de la colonne moyenne pression et condenser un deuxième gaz de vaporisation, plus volatil que ledit premier gaz de vaporisation mais moins volatil que l'azote de tête de la colonne moyenne pression, à un niveau intermédiaire entre ceux desdites condensations,
   caractérisé en ce que le deuxième gaz de vaporisation est un gaz soutiré de la double colonne.The invention also relates to a process for producing impure oxygen by air distillation in a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column comprising the steps of:
  • operate the medium pressure column under a pressure greater than 6 bar and preferably at least equal to approximately 9 bar absolute;
  • condensing in a tank condenser of the low pressure column a first vaporization gas which is less volatile than the top nitrogen of the medium pressure column; and
  • condensing nitrogen from the top of the medium pressure column, which is then sent to reflux at the top of the medium pressure column in a second condenser, at a level of the low pressure column located above said tank condenser,
the first vaporizing gas being air at the pressure of the medium pressure column and condensing a second vaporizing gas, more volatile than said first vaporizing gas but less volatile than the nitrogen at the head of the medium pressure column, at an intermediate level between those of said condensations,
characterized in that the second vaporizing gas is a gas withdrawn from the double column.

Suivant des modes de réalisation préférés de l'invention :

  • on soutire l'oxygène impur sous forme liquide de la cuve de la colonne basse pression, on l'amène sous forme liquide à la pression de production désirée, et on le vaporise sous cette pression par condensation d'un troisième gaz de vaporisation ;
  • le troisième gaz de vaporisation est de l'azote à peu près pur ou impur produit par la double colonne et comprimé à une pression de vaporisation de l'oxygène impur sous la pression de production ;
  • le troisième gaz de vaporisation est de l'air alimentant la double colonne, comprimé à une pression de vaporisation de l'oxygène impur sous la pression de production.
According to preferred embodiments of the invention:
  • the impure oxygen is withdrawn in liquid form from the tank of the low pressure column, it is brought in liquid form to the desired production pressure, and it is vaporized under this pressure by condensation of a third vaporization gas;
  • the third vaporization gas is almost pure or impure nitrogen produced by the double column and compressed to a vaporization pressure of the impure oxygen under the production pressure;
  • the third vaporization gas is air supplying the double column, compressed to a vaporization pressure of the impure oxygen under the production pressure.

L'invention a également pour objet une installation de distillation d'air à double colonne, la double colonne comprenant une colonne moyenne pression et une colonne basse pression, comprenant des moyens pour fournir à la colonne moyenne pression de l'air à distiller sous au moins 9 bar absolus environ, et en ce que la colonne basse pression comprend au moins deux vaporiseurs-condenseurs superposés, dont un vaporiseur-condenseur de cuve, des moyens pour alimenter ce vaporiseur-condenseur de cuve avec un premier gaz de vaporisation moins volatil que l'azote de tête de la colonne moyenne pression, des moyens pour alimenter le deuxième vaporiseur-condenseur avec de l'azote de tête de la colonne moyenne pression, et des moyens pour envoyer l'azote ainsi condensé en reflux en tête de la colonne moyenne pression, caractérisée en ce que les moyens pour alimenter le vaporiseur-condenseur de cuve comprennent des moyens pour y envoyer un gaz soutiré à un niveau intermédiaire de la colonne moyenne pression ou des moyens pour y envoyer de l'azote à peu près pur ou impur, comprimé à une pression supérieure à celle de la colonne moyenne pression.The invention also relates to a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column, comprising means for supplying the medium pressure column with air to be distilled under at minus around 9 bar absolute, and in that the low pressure column comprises at least two superposed vaporizers-condensers, including a tank vaporizer-condenser, means for supplying this tank vaporizer-condenser with a first vaporization gas less volatile than the nitrogen at the head of the medium pressure column, means for supplying the second vaporizer-condenser with nitrogen at the head of the medium pressure column, and means for sending the nitrogen thus condensed to reflux at the head of the column medium pressure, characterized in that the means for supplying the tank vaporizer-condenser comprise means for sending a gas withdrawn therein at an intermediate level of the medium pressure column or means for sending thereto approximately pure or impure nitrogen, compressed to a pressure higher than that of the medium pressure column.

L'invention a également pour objet une installation de distillation d'air à double colonne, la double colonne comprenant une colonne moyenne pression et une colonne basse pression, comprenant des moyens pour fournir à la colonne moyenne pression de l'air à distiller sous au moins 9 bar absolus environ, et en ce que la colonne basse pression comprend au moins trois vaporiseurs-condenseurs superposés, dont un vaporiseur-condenseur de cuve, des moyens pour alimenter ce vaporiseur-condenseur de cuve avec un premier gaz de vaporisation moins volatil que l'azote de tête de la colonne moyenne pression, des moyens pour alimenter le deuxième vaporiseur-condenseur avec de l'azote de tête de la colonne moyenne pression, des moyens pour envoyer l'azote ainsi condensé en reflux en tête de la colonne moyenne pression, des moyens pour alimenter le vaporiseur-condenseur de cuve comprenant des moyens pour y envoyer de l'air moyenne pression, des moyens pour alimenter le vaporiseur-condenseur intermédiaire avec un deuxième gaz moins volatil que cet azote de tête et plus volatil que ledit premier gaz de vaporisation, caractérisée en ce que le deuxième gaz est un gaz soutiré de la double colonne.The invention also relates to a double column air distillation installation, the double column comprising a medium pressure column and a low pressure column, comprising means for supplying the medium pressure column with air to be distilled at at least about 9 bar absolute, and in that the low pressure column comprises at least three superposed vaporizers-condensers, including a tank vaporizer-condenser, means for supplying this tank vaporizer-condenser with a first vaporization gas less volatile than the top nitrogen of the medium pressure column, means for supplying the second vaporizer-condenser with nitrogen from the top of the medium pressure column, means for send the nitrogen thus condensed in reflux at the head of the medium pressure column, means for supplying the tank vaporizer-condenser comprising means for sending medium pressure air therein, means for supplying the intermediate vaporizer-condenser with a second gas less volatile than this top nitrogen and more volatile than said first vaporizing gas, characterized in that the second gas is a gas withdrawn from the double column e.

Suivant des modes de réalisation préférés de l'invention :

  • au moins deux vaporiseurs-condenseurs de la colonne basse pression sont immédiatement superposés l'un à l'autre, sans moyen de distillation intermédiaire;
  • l'installation comprend des moyens de soutirage d'oxygène impur sous forme liquide de la cuve de la colonne basse pression, des moyens de compression de cet oxygène impur liquide à une pression de production, ainsi qu'un cycle à azote de soutien de rectification comprenant des moyens pour comprimer, liquéfier, détendre et introduire dans la colonne moyenne pression une fraction de l'azote à peu près pur ou impur produit par la double colonne ;
  • lesdits moyens de compression sont adaptés pour comprimer ladite fraction d'azote à une pression de vaporisation de l'oxygène impur sous ladite pression de production.
According to preferred embodiments of the invention:
  • at least two vaporizers-condensers of the low pressure column are immediately superimposed on each other, without any intermediate distillation means;
  • the installation comprises means for withdrawing impure oxygen in liquid form from the tank of the low pressure column, means for compressing this impure oxygen liquid at a production pressure, as well as a nitrogen cycle for rectification support comprising means for compressing, liquefying, expanding and introducing into the medium pressure column a fraction of the approximately pure or impure nitrogen produced by the double column;
  • said compression means are adapted to compress said fraction of nitrogen to a vaporization pressure of the impure oxygen under said production pressure.

Des exemples de mise en oeuvre de l'invention vont maintenant être décrits en regard des dessins annexés, sur lesquels les Figures 1 à 4 représentent schématiquement quatre modes de réalisation de l'installation de distillation d'air conforme à l'invention.Examples of implementation of the invention will now be described with reference to the accompanying drawings, in which Figures 1 to 4 schematically represent four embodiments of the air distillation installation according to the invention.

L'installation représentée à la Figure 1 est destinée à produire de l'oxygène à une pureté de l'ordre de 85% sous une pression de l'ordre de 7,4 bars absolus. Elle comprend essentiellement une double colonne 1 de distillation d'air, constituée d'une colonne moyenne pression (ou "colonne MP") 2 fonctionnant sous 15,7 bars absolus et d'une colonne basse pression (ou "colonne BP") 3 fonctionnant sous 6,3 bars absolus, une ligne d'échange thermique principale 4, un sous-refroidisseur 5, un vaporiseur-condenseur auxiliaire 6 et une turbine 7 d'insufflation d'air dans la colonne basse pression. La colonne 3 est superposée à la colonne 2 et contient en cuve un vaporiseur-condenseur 8 et, au-dessus de celui-ci, un second vaporiseur-condenseur 9.The installation shown in Figure 1 is intended to produce oxygen at a purity of the order of 85% under a pressure of the order of 7.4 bar absolute. It essentially comprises a double column 1 for air distillation, consisting of a medium pressure column (or "MP column") 2 operating at 15.7 bar absolute and a low pressure column (or "LP column") 3 operating at 6.3 bar absolute, a main heat exchange line 4, a sub-cooler 5, an auxiliary evaporator-condenser 6 and a turbine 7 for blowing air into the low pressure column. Column 3 is superimposed on column 2 and contains in the tank a vaporizer-condenser 8 and, above this, a second vaporizer-condenser 9.

L'air à distiller arrive sous la moyenne pression via une conduite 10 et pénètre dans la ligne d'échange 4. La majeure partie de cet air est refroidie jusqu'au voisinage de son point de rosée et sort au bout froid de la ligne d'échange, le reste étant sorti de la ligne d'échange à une température intermédiaire, détendu à la basse pression dans la turbine 7 pour assurer le maintien en froid de l'installation, et insufflé à un niveau intermédiaire dans la colonne BP 3.The air to be distilled arrives at medium pressure via a line 10 and enters the exchange line 4. Most of this air is cooled to the vicinity of its dew point and leaves the cold end of the line d 'exchange, the rest having left the exchange line at an intermediate temperature, expanded at low pressure in the turbine 7 to keep the installation cold, and blown at an intermediate level in the LP column 3.

Une fraction de l'air entièrement refroidi est introduit, via une conduite 11, à la base de la colonne MP 2, et le reste est condensé dans le vaporiseur-condenseur 6; une partie du liquide obtenu est introduit via une conduite 12 en un point intermédiaire de la colonne 2, et le reste est, après sous-refroidissement en 5 et détente dans une vanne de détente 13, introduit en un point intermédiaire de la colonne BP 3.A fraction of the fully cooled air is introduced, via a pipe 11, at the base of the column MP 2, and the rest is condensed in the vaporizer-condenser 6; part of the liquid obtained is introduced via a line 12 at an intermediate point in column 2, and the rest is, after sub-cooling in 5 and expansion in an expansion valve 13, introduced at an intermediate point in column BP 3 .

Le "liquide riche" (air enrichi en oxygène) recueilli en cuve de la colonne MP est, après sous-refroidissement en 5 et détente dans une vanne de détente 14, introduit en un point intermédiaire de la colonne BP. De même, du "liquide pauvre" (azote impur) soutiré en un point intermédiaire de la colonne MP est, après sous-refroidissement en 5 et détente dans une vanne de détente 15, introduit au sommet de la colonne BP.The "rich liquid" (oxygen-enriched air) collected in the bottom of the MP column is, after sub-cooling in 5 and expansion in an expansion valve 14, introduced at an intermediate point of the LP column. Likewise, "lean liquid" (impure nitrogen) withdrawn at an intermediate point of the column MP is, after sub-cooling in 5 and expansion in an expansion valve 15, introduced at the top of the column BP.

L'azote à peu près pur produit en tête de la colonne MP est pour partie évacué de l'installation en tant que produit, après réchauffement dans la ligne d'échange, via une conduite 16, et, pour le reste, envoyé sous forme gazeuse via une conduite 17, sous la moyenne pression, dans le vaporiseur-condenseur supérieur 9. Après condensation, cet azote est renvoyé en reflux en tête de la colonne MP via une conduite 18.The approximately pure nitrogen produced at the head of the MP column is partly removed from the installation as a product, after heating in the exchange line, via a line 16, and, for the rest, sent in the form gas via a line 17, at medium pressure, in the upper evaporator-condenser 9. After condensation, this nitrogen is returned to reflux at the head of the column MP via a line 18.

De plus, de l'azote impur gazeux, soutiré en un point intermédiaire de la colonne 2 et, dans cet exemple, au même niveau que le liquide pauvre, est envoyé via une conduite 19, sous la moyenne pression, dans le vaporiseur-condenseur inférieur 8. Le liquide ainsi obtenu est renvoyé en reflux dans la colonne MP, à peu près au même niveau, via une conduite 20.In addition, impure nitrogen gas, drawn off at an intermediate point in column 2 and, in this example, at the same level as the lean liquid, is sent via a line 19, under medium pressure, to the vaporizer-condenser lower 8. The liquid thus obtained is returned under reflux to the column MP, at approximately the same level, via a line 20.

Les courants de fluides sortant de la double colonne sont :

  • au sommet de la colonne MP, de l'azote moyenne pression, dont il a été question plus haut;
  • au sommet de la colonne BP, de l'azote impur, constituant le gaz résiduaire de l'installation. Cet azote impur, après réchauffement dans le sous-refroidisseur 5 et dans la ligne d'échange 4, est évacué via une conduite 21; et
  • en cuve de la colonne BP, de l'oxygène impur liquide. Ce liquide est soutiré via une conduite 22, comprimé par une pompe 23 à la pression de production (7,4 bars absolus dans cet exemple), puis vaporisé dans le vaporiseur-condenseur 6 en condensant la fraction d'air moyenne pression qui traverse ce dernier, puis réchauffé sous forme gazeuse dans la ligne d'échange et évacué de l'installation via une conduite de production 24.
The streams of fluids leaving the double column are:
  • at the top of the MP column, medium pressure nitrogen, which was discussed above;
  • at the top of the LP column, impure nitrogen, constituting the waste gas from the installation. This impure nitrogen, after heating in the sub-cooler 5 and in the exchange line 4, is discharged via a line 21; and
  • in the bottom of the BP column, liquid impure oxygen. This liquid is drawn off via a line 22, compressed by a pump 23 to the production pressure (7.4 bar absolute in this example), then vaporized in the evaporator-condenser 6 by condensing the fraction of medium pressure air which passes through this last, then heated in gaseous form in the exchange line and discharged from the installation via a production line 24.

En variante, la pompe 23 pourrait être supprimée, l'oxygène impur étant alors vaporisé en 6 sous la basse pression.As a variant, the pump 23 could be omitted, the impure oxygen then being vaporized at 6 under the low pressure.

La description ci-dessus montre que, pour un écart de température donné dans le vaporiseur-condenseur 8, la température du liquide de cuve de la colonne BP est déterminée par celle du gaz condensé dans ce vaporiseur-condenseur. Comme il s'agit d'un gaz intermédiaire de la colonne MP, plus chaud que l'azote de tête de cette colonne, la température du liquide de cuve, qui est l'oxygène impur, est relativement élevée. Par suite, pour une pureté désirée de cet oxygène impur, la pression de la colonne BP, c'est-à-dire la basse pression, peut être augmentée. Finalement, on obtient de l'oxygène impur et de l'azote impur sous une pression accrue, ce qui permet de réaliser des économies sur leur valorisation, par exemple sur l'énergie nécessaire pour comprimer l'azote impur à la pression voulue dans une turbine à gaz (non représentée) couplée à l'installation, par exemple de la manière décrite dans le US-A-4 224 045 précité.The above description shows that, for a given temperature difference in the vaporizer-condenser 8, the temperature of the bottom liquid of the LP column is determined by that of the gas condensed in this vaporizer-condenser. As it is an intermediate gas in column MP, hotter than the nitrogen at the top of this column, the temperature of the tank liquid, which is impure oxygen, is relatively high. As a result, for a desired purity of this impure oxygen, the pressure of the LP column, that is to say the low pressure, can be increased. Finally, impure oxygen and impure nitrogen are obtained under increased pressure, which makes it possible to make savings on their recovery, for example on the energy required to compress the impure nitrogen to the desired pressure in a gas turbine (not shown) coupled to the installation, for example as described in the aforementioned US-A-4,224,045.

Dans ce contexte, le vaporiseur-condenseur supérieur 9 sert à fournir le reflux nécessaire en tête de la colonne MP.In this context, the upper vaporizer-condenser 9 serves to provide the necessary reflux at the top of the column MP.

Si les températures des deux gaz alimentant les deux vaporiseurs-condenseurs sont nettement différentes l'une de l'autre, il est nécessaire de prévoir un certain nombre de plateaux de distillation 25 entre ces vaporiseurs-condenseurs. Dans le cas contraire, ces plateaux peuvent être supprimés, ce qui simplifie la constructions de la colonne BP, les deux vaporiseurs-condenseurs pouvant même être intégrés en un seul échangeur de chaleur. C'est pourquoi les plateaux 25 ont été représentés en trait interrompu.If the temperatures of the two gases supplying the two vaporizers-condensers are clearly different from each other, it is necessary to provide a number of distillation plates 25 between these vaporizers-condensers. Otherwise, these plates can be removed, which simplifies the construction of the LP column, the two vaporizers-condensers can even be integrated into a single heat exchanger. This is why the plates 25 have been shown in broken lines.

L'installation représentée à la Figure 2 ne diffère de la Figure 1 que par les points suivants.The installation shown in Figure 2 differs from Figure 1 only in the following points.

L'oxygène impur est soutiré sous forme gazeuse de la colonne BP 3, et est simplement réchauffé dans la ligne d'échange 4 avant son évacuation via la conduite 24. Ceci est particulièrement intéressant lorsque l'oxygène impur est désiré sous la basse pression. En conséquence, le vaporiseur-condenseur 6 est supprimé.The impure oxygen is withdrawn in gaseous form from the LP column 3, and is simply reheated in the exchange line 4 before its evacuation via the pipe 24. This is particularly advantageous when the impure oxygen is desired under the low pressure. Consequently, the vaporizer-condenser 6 is eliminated.

De plus, une fraction de l'air moyenne pression refroidi au voisinage de son point de rosée est envoyée, via une conduite 26, dans le vaporiseur-condenseur inférieur 8 à la place du gaz intermédiaire de la Figure 1. Ce gaz intermédiaire, quant à lui, alimente un vaporiseur-condenseur intermédiaire 27 situé entre les vaporiseurs-condenseurs inférieur 8 et supérieur 9. Comme précédemment, il peut y avoir ou non des plateaux entre les paires de vaporiseurs-condenseurs. L'air liquéfié issu du vaporiseur-condenseur 8 est envoyé pour partie, via une conduite 28, dans la colonne MP et pour partie, après sous-refroidissement en 5 et détente dans la vanne de détente 13, dans la colonne BP.In addition, a fraction of the medium pressure air cooled near its dew point is sent, via a line 26, to the lower vaporizer-condenser 8 in place of the intermediate gas of Figure 1. This intermediate gas, as to it, feeds an intermediate vaporizer-condenser 27 located between the lower vaporizers-condensers 8 and upper 9. As before, there may or may not be plates between the pairs of vaporizers-condensers. The liquefied air from the vaporizer-condenser 8 is sent partly, via a line 28, to the column MP and partly, after sub-cooling in 5 and expansion in the expansion valve 13, in the column BP.

Par rapport à la solution de la Figure 1, on obtient une température plus élevée en cuve de la colonne BP, ce qui est favorable à l'augmentation de la basse pression. En revanche, on doit vaporiser un liquide plus riche en oxygène que l'oxygène impur à produire, ce qui tend à réduire la basse pression.Compared to the solution of Figure 1, a higher temperature is obtained in the bottom of the LP column, which is favorable for the increase in the low pressure. On the other hand, one must vaporize a liquid more rich in oxygen than impure oxygen to produce, which tends to reduce low pressure.

Ce dernier inconvénient est supprimé dans l'installation de la Figure 3, qui permet de produire l'oxygène impur sous une pression élevée, et qui diffère de la précédente par les points suivants.This last drawback is eliminated in the installation of FIG. 3, which makes it possible to produce impure oxygen under high pressure, and which differs from the previous one in the following points.

D'une part, l'oxygène impur est soutiré sous forme liquide de la cuve de la colonne BP, puis est amené par une pompe 23 à la pression de production désirée, puis vaporisé et réchauffé sous cette pression dans la ligne d'échange 4 avant d'être évacué de l'installation via la conduite 24.On the one hand, the impure oxygen is withdrawn in liquid form from the tank of the LP column, then is brought by a pump 23 to the desired production pressure, then vaporized and heated under this pressure in the exchange line 4 before being evacuated from the installation via line 24.

D'autre part, pour compenser la perte de reflux dans la colonne MP résultant du soutirage d'oxygène liquide en cuve de la colonne BP, il est prévu un cycle azote, dit cycle de soutien de rectification, qui est utilisé en même temps pour assurer la vaporisation de l'oxygène impur : une partie de l'azote produit en tête de la colonne 3 (laquelle, dans ce cas, possède en tête un "minaret" 30 qui est alimenté à son sommet par de l'azote liquide pur provenant du vaporiseur-condenseur supérieur 9 et qui, par suite, produit de l'azote pur sous la basse pression) est, après réchauffement dans la ligne d'échange, comprimée par un compresseur 31 à la moyenne pression. Cet azote moyenne pression, réuni à un courant d'azote moyenne pression prélevé sur la conduite 16, est comprimé de nouveau par un compresseur 33 à une pression de vaporisation de l'oxygène impur comprimé par la pompe 23, liquéfié dans la ligne d'échange, puis, après détente dans une vanne de détente 34, introduit en reflux en tête de la colonne MP.On the other hand, to compensate for the loss of reflux in the MP column resulting from the withdrawal of liquid oxygen from the bottom of the LP column, a nitrogen cycle is provided, known as the rectification support cycle, which is used at the same time to ensure the vaporization of impure oxygen: part of the nitrogen produced at the head of column 3 (which, in this case, has at the head a "minaret" 30 which is supplied at its top with pure liquid nitrogen coming from the upper evaporator-condenser 9 and which, consequently, produces pure nitrogen under low pressure) is, after heating in the exchange line, compressed by a compressor 31 at medium pressure. This medium pressure nitrogen, combined with a current of medium pressure nitrogen taken from the line 16, is compressed again by a compressor 33 to a vaporization pressure of the impure oxygen compressed by the pump 23, liquefied in the line of exchange, then, after expansion in an expansion valve 34, introduced under reflux at the head of the column MP.

L'installation de la Figure 4 comporte également une colonne BP 3 à minaret 30. Toutefois, contrairement au cas précédent, c'est de l'air haute pression, surpressé à une pression de vaporisation de l'oxygène impur par un surpresseur 35, qui assure la vaporisation de l'oxygène impur dans la ligne d'échange 4. Dans cet exemple, cet air est, après liquéfaction et détente dans une vanne de détente 36 et dans la vanne de détente 13, réparti entre les deux colonnes 2 et 3. par conséquent, le compresseur 33 et la vanne de détente 34 de la Figure 3 sont supprimés.The installation of Figure 4 also includes a BP 3 column with minaret 30. However, unlike the previous case, it is high air pressure, boosted to a vaporization pressure of the impure oxygen by a booster 35, which ensures the vaporization of the impure oxygen in the exchange line 4. In this example, this air is, after liquefaction and expansion in a valve expansion valve 36 and in the expansion valve 13, distributed between the two columns 2 and 3. consequently, the compressor 33 and the expansion valve 34 of FIG. 3 are eliminated.

De plus, l'azote issu du compresseur 31, comprimé à une pression supérieure à la moyenne pression, alimente sous forme gazeuse, après refroidissement dans la ligne d'échange, le vaporiseur-condenseur inférieur 8, et l'azote liquide résultant est, après détente dans une vanne de détente 37, réuni à l'azote liquide moyenne pression issu du vaporiseur-condenseur supérieur 9. Ceci présente l'avantage de permettre un réglage de la température de cuve de la colonne BP, et donc de la pression de cette colonne, par réglage de la pression de l'azote alimentant le vaporiseur-condenseur 8. Cette pression d'azote peut être choisie entre la moyenne pression et la pression pour laquelle l'azote se condense au bout froid de la ligne d'échange.In addition, the nitrogen from the compressor 31, compressed to a pressure higher than the medium pressure, feeds in gaseous form, after cooling in the exchange line, the lower vaporizer-condenser 8, and the resulting liquid nitrogen is, after expansion in an expansion valve 37, combined with medium-pressure liquid nitrogen from the upper vaporizer-condenser 9. This has the advantage of allowing adjustment of the tank temperature of the LP column, and therefore of the pressure of this column, by adjusting the pressure of the nitrogen supplying the vaporizer-condenser 8. This nitrogen pressure can be chosen between medium pressure and the pressure for which the nitrogen condenses at the cold end of the exchange line .

Claims (13)

  1. Process for producing impure oxygen by distilling air in an air distillation installation with a double column (1), the double column comprising a medium pressure column (2) and a low pressure column (3) comprising the stages of :
    - operating the medium pressure column (2) at a pressure greater than 6 bar and preferably at least equal to about 9 bar absolute;
    - condensing in a vessel condenser (8) of the low pressure column (3) a first vaporization gas less volatile than nitrogen from the head of the medium pressure column (2); and
    - condensing nitrogen from the head of the medium pressure column in a second condenser (9), at a level of the low pressure column (3) situated above the said vessel condenser (8), this nitrogen being then conveyed in reflux to the head of the medium pressure column.
       characterised in that the first vaporization gas is a gas withdrawn at an intermediate level of the medium pressure column (2) or almost pure or impure nitrogen compressed to a pressure greater than that of the medium pressure column (2).
  2. Process according to claim 1, characterized in that a second vaporization gas is condensed, more volatile than the first vaporization gas but less volatile than nitrogen from the head of the medium pressure column (2), at a level intermediate between those of the said condensations.
  3. Process for producing impure oxygen by distilling air in an air distillation installation with a double column (1), the double column comprising a medium pressure column (2) and a low pressure column (3) comprising the stages of :
    - operating the medium pressure column (2) at a pressure greater than 6 bar and preferably at least equal to about 9 bar absolute;
    - condensing in a vessel condenser (8) of the low pressure column (3) a first vaporization gas less volatile than nitrogen from the head of the medium pressure column (2); and
    - condensing nitrogen from the head of the medium pressure column in a second condenser (9) at a level of the low pressure column (3) situated above the said vessel condenser (8), this nitrogen being then conveyed in reflux to the head of the medium pressure column,
       the first vaporization gas being air at the pressure of the medium pressure column (2) and condensing a second vaporization gas, more volatile than the said first vaporization gas but less volatile than nitrogen from the head of the medium pressure column (2), at a level intermediate between those of the said condensations,
       characterized in that the second vaporization gas is a gas withdrawn from the double column (1).
  4. Process according to one of claims 1, 2 and 3, characterized in that impure oxygen is withdrawn in liquid form from the vessel of the low pressure column (3), it is conveyed in liquid form at the desired production pressure, and is vaporized at this pressure by condensation of a third vaporization gas.
  5. Process according to claim 4, characterized in that the third vaporization gas is almost pure or impure nitrogen produced by the double column and compressed (in 33) to a vaporization pressure of impure oxygen at the production pressure.
  6. Process according to claim 4, characterized in that the third vaporization gas is air feeding the double column (1), compressed (in 35) to a vaporization pressure of impure oxygen at the production pressure.
  7. Installation for distilling air with a double column (1), the double column comprising a medium pressure column (2) and a low pressure column (3), comprising means (10) for feeding the medium pressure column (2) with air to be distilled under at least about 9 bar absolute, and in that the low pressure column (3) comprises at least two superimposed vaporizers - condensers (8,9; 8,9,27), one of which is a vessel vaporizer condenser (8), means for feeding this vessel vaporizer-condenser (8) with a first vaporization gas less volatile than nitrogen from the head of the medium pressure column (2), means for feeding the second vaporizer-condenser (9) with nitrogen from the head of the medium pressure column, and means (18) for conveying the nitrogen thus condensed in reflux into the head of the medium pressure column, characterised in that the means for feeding the vessel vaporizer-condenser (8) comprises means (19) for conveying there a gas withdrawn at an intermediate level of the medium pressure column (2) or means for conveying almost pure or impure nitrogen there, compressed to a pressure greater than that of the medium pressure column (2).
  8. Installation according to claim 7, characterised in that the low pressure column (3) comprises a third vaporizer - condenser (27) between the vessel vaporizer-condenser (2) and the second vaporizer-condenser (27).
  9. Installation for distilling air with a double column (1), the double column comprising a medium pressure column (2) and a low pressure column (3), comprising means (10) for feeding the medium pressure column (2) with air to be distilled under at least about 9 bar absolute, and in that the low pressure column (3) comprises at least three superimposed vaporizers-condensers (8, 9, 27) one of which is a vaporizer-condenser (2) of the vessel (8), means for feeding this vessel vaporizer-condenser (8) with a first vaporization gas less volatile than nitrogen from the head of the medium pressure column (2), means for feeding the second vaporizer-condenser (9) with nitrogen from the head of the medium pressure column, means (18) for conveying the nitrogen thus condensed in reflux to the head of the medium pressure column, means for feeding the vessel vaporizer-condenser (8) comprising means (26) for conveying medium pressure air there, means for feeding the intermediate vaporizer-condenser (27) with a second gas less volatile than this head nitrogen and more volatile than the said first vaporization gas, characterized in that the second gas is a gas withdrawn from the double column (1).
  10. Installation according to claim 7, 8 or 9, characterized in that at least two vaporizers-condensers (8, 9; 9, 27) of the low pressure column (3) are immediately superimposed on each other, without intermediate means of distillation (25).
  11. Installation according to any one of claims 7 to 10, characterized in that it comprises means (22) for withdrawing impure oxygen in liquid form from the vessel of the low pressure column (3), means (23) for compressing this impure liquid oxygen to a production pressure, as well as a nitrogen cycle for maintaining fractionation comprising means (33, 34) for compressing, liquefying, expanding and introducing into the medium pressure column (2) an almost pure or impure nitrogen fraction produced by the double column (1).
  12. Installation according to claim 11, characterized in that the said means of compression (33) are able to compress the said nitrogen fraction to a vaporization pressure of impure oxygen at the said production pressure.
  13. Installation according to any one of claims 7 to 12, characterized in that it comprises an air compressor (35) able to bring a fraction of the air to be distilled to a vaporization pressure of impure oxygen at the said production pressure.
EP92403330A 1991-12-18 1992-12-09 Process for the production of impure oxygen Expired - Lifetime EP0547946B2 (en)

Priority Applications (1)

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EP96200235A EP0713069B1 (en) 1991-12-18 1992-12-09 Process and plant for air separation

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FR9115705A FR2685459B1 (en) 1991-12-18 1991-12-18 PROCESS AND PLANT FOR PRODUCING IMPURATED OXYGEN.
FR9115705 1991-12-18

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EP96200235A Division EP0713069B1 (en) 1991-12-18 1992-12-09 Process and plant for air separation
EP96200235.8 Division-Into 1992-12-09

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EP0547946A1 EP0547946A1 (en) 1993-06-23
EP0547946B1 true EP0547946B1 (en) 1996-10-09
EP0547946B2 EP0547946B2 (en) 2000-03-22

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CN (1) CN1068428C (en)
AU (1) AU654601B2 (en)
BR (1) BR9205050A (en)
CA (1) CA2085561A1 (en)
DE (2) DE69214409T3 (en)
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EP0713069A1 (en) 1996-05-22
ES2092661T3 (en) 1996-12-01
DE69214409T3 (en) 2000-07-13
EP0713069B1 (en) 2000-04-26
FR2685459B1 (en) 1994-02-11
DE69214409D1 (en) 1996-11-14
CN1068428C (en) 2001-07-11
CA2085561A1 (en) 1993-06-19
DE69230975T2 (en) 2000-10-05
ES2145967T3 (en) 2000-07-16
EP0547946A1 (en) 1993-06-23
AU3022192A (en) 1993-06-24
FR2685459A1 (en) 1993-06-25
DE69230975D1 (en) 2000-05-31
AU654601B2 (en) 1994-11-10
BR9205050A (en) 1993-08-10
US5392609A (en) 1995-02-28
DE69214409T2 (en) 1997-05-22
EP0547946B2 (en) 2000-03-22
CN1088301A (en) 1994-06-22

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