EP0562893B2 - Process for the production of high pressure nitrogen and oxygen - Google Patents

Process for the production of high pressure nitrogen and oxygen Download PDF

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Publication number
EP0562893B2
EP0562893B2 EP93400522A EP93400522A EP0562893B2 EP 0562893 B2 EP0562893 B2 EP 0562893B2 EP 93400522 A EP93400522 A EP 93400522A EP 93400522 A EP93400522 A EP 93400522A EP 0562893 B2 EP0562893 B2 EP 0562893B2
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EP
European Patent Office
Prior art keywords
pressure
nitrogen
oxygen
column
compressor
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EP93400522A
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German (de)
French (fr)
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EP0562893B1 (en
EP0562893A1 (en
Inventor
Yves Koeberle
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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    • 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
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • F25J3/04145—Mechanically coupling of different compressors of the air fractionation process to the same driver(s)
    • 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
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/04018—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of main feed air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/0403—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • F25J3/04115—Arrangements of compressors and /or their drivers characterised by the type of prime driver, e.g. hot gas expander
    • F25J3/04121—Steam turbine as the prime mechanical driver
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04315—Lowest pressure or impure nitrogen, so-called waste nitrogen expansion
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—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
    • F25J3/04412—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
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
    • 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
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
    • F25J3/04545—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels for the gasification of solid or heavy liquid fuels, e.g. integrated gasification combined cycle [IGCC]
    • 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
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating
    • F25J3/04587—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating for the NH3 synthesis, e.g. for adjusting the H2/N2 ratio
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/50—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/12—Particular process parameters like pressure, temperature, ratios

Definitions

  • the present invention relates to a process for the simultaneous production of a portion of pure nitrogen under a high nitrogen pressure and secondly oxygen, by air distillation in a double distillation column comprising a medium pressure column and a low pressure column of the "minaret" type producing pure nitrogen at the head.
  • a particular application of the invention is the production simultaneous one part of high purity nitrogen, containing less than 10 ppm oxygen, in large quantities (i.e. representing at least 20% and typically more than 30% of the treated air flow), under 50 to 60 bar, for a ammonia, and secondly purity oxygen manufacturing unit medium to high, i.e. 95 to 99.5 mol%, at a pressure of the order of 65 bar with high extraction yield, for production of hydrogen by reaction of oxygen with heavy hydrocarbons, hydrogen being intended to supply the same manufacturing unit ammonia.
  • Low pressure column of the minaret type means a low pressure column forming part of a double distillation column air, the upper end part of which is supplied at the head by "upper poor liquid” (practically pure nitrogen) withdrawn at the top of the medium pressure and relaxed column, and produces pure nitrogen at the top low pressure.
  • US-A-2,982,108 describes a process for simultaneous production pressurized nitrogen and oxygen in which a compressor is used pressurize the nitrogen produced to a pressure which cannot exceed 40 bar, if it is assumed that the compressor has at most six wheels.
  • the nitrogen compressor and the air compressor can particular be connected to a common motor source.
  • the installation shown in the drawings is intended to produce on the one hand, under 55 bar, high purity nitrogen gas (containing typically less than 10 ppm oxygen), at a flow rate at least equal to 20% of the treated air flow, and on the other hand, under 65 bar, oxygen having a purity from 95 to 99.5%, with a high extraction yield.
  • high purity nitrogen gas containing typically less than 10 ppm oxygen
  • 65 bar oxygen having a purity from 95 to 99.5%
  • the installation essentially comprises an air compressor 1, an apparatus 2 for air purification by adsorption, an exchange line thermal 3 of the counter-current type, a double distillation column 4, an expansion turbine 5, a liquid oxygen pump 6, a compressor of nitrogen 7, an oxygen compressor 8 and an energy source 9 consisting for example by a steam turbine.
  • the double column 4 comprises a medium pressure column 10 surmounted by a low pressure column 11, the end portion of which upper forms an 11A minaret of pure nitrogen production under the lower pressure.
  • a condenser-vaporizer 12 puts in exchange relationship thermal the overhead vapor (practically pure nitrogen) from column 10 and the tank liquid (oxygen from determined purity) of column 11.
  • an equipped pipe an expansion valve 13 makes it possible to raise "liquid rich "(oxygen-enriched air) from the column tank 10 at an intermediate point in column 11; a pipe fitted with an expansion valve 14 allows rise from the "lower lean liquid” (impure nitrogen) of a intermediate point of column 10 at the base of the minaret 11A; and a pipe fitted with an expansion valve 15 makes it possible to raise "upper lean liquid” (nitrogen practically pure) from the head of column 10 to the top minaret.
  • the nitrogen compressor 7 consists of a single three-stage compressor.
  • the first two floors each include two compression wheels and have average compression ratios per wheel of 2 and 1.73 respectively, while the third floor comprises a single compression wheel with a compression ratio of 1.83.
  • the overall compression ratio of the compressor is therefore 22.
  • Each wheel has at its output a refrigerant.
  • the oxygen compressor 8 is also consisting of a single compressor. This compressor has six wheels with an average compression ratio per wheel of 1.37. The overall compression ratio is therefore 6.5.
  • the shaft 16 of the compressor 7 is coupled to the shaft 17 of the compressor 1 by a coupling 18, and the whole is driven by the common energy source 9.
  • the shaft 16 can cause the different compressor 7 stages via speed multipliers suitable for each stage.
  • the compressor 8 is driven by an energy source separate 19.
  • the incoming air is compressed to 11 bars in compressor 1, purified in 2, cooled from the hot end at the cold end of the exchange line 3, and introduced to the near its dew point in tank of column 10.
  • the pure low pressure nitrogen leaving gas from the top of the 11A minaret and warmed to room temperature cold end at the hot end of the exchange line is introduced to the suction of the first stage of the compressor 7, with the possible exception of a nitrogen flow produced at low pressure via line 20.
  • Nitrogen high pressure is produced at the discharge of the third compressor stage and evacuated via line 21.
  • Compressor 7 is also used as nitrogen cycle compressor. Nitrogen medium pressure is drawn off at the top of column 10, via line 22, warmed to room temperature in the exchange line and introduced via a pipe 23 at the suction of the second stage of compressor 7. From nitrogen at high cycle pressure is released at discharge of this second stage via a pipe 24, cooled, liquefied and sub-cooled in the line exchange, expanded at medium pressure in a valve trigger 25 and introduced at the top of column 10.
  • the nitrogen flow flowing in the pipe 24 is greater than the flow rate by a predetermined amount of nitrogen flowing in line 23.
  • the difference constitutes an additional flow of liquid nitrogen, known as rectification support, introduced at reflux at the top of column 10. This flow is taken from the current low pressure nitrogen drawn in from the first stage of the compressor 7.
  • Impure nitrogen constituting the waste gas of the installation, is withdrawn at the base of the minaret 11A via a pipe 25, heated to a temperature intermediary in the exchange line, out of the latter, relaxed at atmospheric pressure in a turbine 5 which keeps the installation cold, then reintroduced into the exchange line, warmed up to room temperature, and finally used to regenerate the adsorption bottles of device 2 and evacuated from the installation via a pipe 26.
  • Oxygen at 65 bar is produced from the next way.
  • the desired liquid oxygen flow is withdrawn in the tank of column 11, brought by pump 6 to a intermediate oxygen pressure, vaporized and heated at room temperature in exchange line 3, then compressed to production pressure by compressor 8.

Description

La présente invention est relative à un procédé de production simultanée d'une part d'azote pur sous une haute pression d'azote et d'autre part d'oxygène, par distillation d'air dans une double colonne de distillation comprenant une colonne moyenne pression et une colonne basse pression du type "à minaret" produisant l'azote pur en tête.The present invention relates to a process for the simultaneous production of a portion of pure nitrogen under a high nitrogen pressure and secondly oxygen, by air distillation in a double distillation column comprising a medium pressure column and a low pressure column of the "minaret" type producing pure nitrogen at the head.

Une application particulière de l'invention est la production simultanée d'une part d'azote à haute pureté, contenant moins de 10 ppm d'oxygène, en grande quantité (c'est-à-dire représentant au moins 20 % et typiquement plus de 30 % du débit d'air traité), sous 50 à 60 bar, pour une unité de fabrication d'ammoniac, et d'autre part d'oxygène de pureté moyenne à haute, soit 95 à 99,5 % en moles, à une pression de l'ordre de 65 bar avec un rendement d'extraction élevé, pour la production d'hydrogène par réaction de l'oxygène sur des hydrocarbures lourds, l'hydrogène étant destiné à alimenter la même unité de fabrication d'ammoniac.A particular application of the invention is the production simultaneous one part of high purity nitrogen, containing less than 10 ppm oxygen, in large quantities (i.e. representing at least 20% and typically more than 30% of the treated air flow), under 50 to 60 bar, for a ammonia, and secondly purity oxygen manufacturing unit medium to high, i.e. 95 to 99.5 mol%, at a pressure of the order of 65 bar with high extraction yield, for production of hydrogen by reaction of oxygen with heavy hydrocarbons, hydrogen being intended to supply the same manufacturing unit ammonia.

On entend par "colonne basse pression du type à minaret", une colonne basse pression faisant partie d'une double colonne de distillation d'air, dont la partie d'extrémité supérieure est alimentée en tête par du "liquide pauvre supérieur" (azote pratiquement pur) soutiré en tête de la colonne moyenne pression et détendu, et produit en tête de l'azote pur sous la basse pression."Low pressure column of the minaret type" means a low pressure column forming part of a double distillation column air, the upper end part of which is supplied at the head by "upper poor liquid" (practically pure nitrogen) withdrawn at the top of the medium pressure and relaxed column, and produces pure nitrogen at the top low pressure.

Les pressions dont il est question ici sont des pressions absolues. De plus, on entend par "basse pression" et "moyenne pression" les pressions de fonctionnement de la colonne basse pression et de la colonne moyenne pression de la double colonne respectivement.The pressures we are talking about here are absolute pressures. In addition, "low pressure" and "medium pressure" mean the operating pressures of the low pressure column and the column medium pressure of the double column respectively.

US-A-2.982.108, décrit un procédé de production simultanée d'azote sous pression et d'oxygène dans lequel un compresseur sert à pressuriser l'azote produit jusqu'à une pression qui ne peut pas excéder 40 bar, si on suppose que le compresseur a au plus six roues.US-A-2,982,108, describes a process for simultaneous production pressurized nitrogen and oxygen in which a compressor is used pressurize the nitrogen produced to a pressure which cannot exceed 40 bar, if it is assumed that the compressor has at most six wheels.

A cet effet, selon l'invention, il est prévu un procédé selon la revendication 1. To this end, according to the invention, a method is provided according to claim 1.

Suivant un mode particulier de réalisation de l'invention:

  • l'azote de cycle est comprimé à une pression subcritique pour laquelle la température de condensation de l'azote est légèrement supérieure à la température de vaporisation de l'oxygène sous ladite pression intermédiaire d'oxygène.
According to a particular embodiment of the invention:
  • the cycle nitrogen is compressed to a subcritical pressure for which the condensation temperature of the nitrogen is slightly higher than the vaporization temperature of the oxygen under said intermediate oxygen pressure.

Suivant encore un autre mode particulier de réalisation de l'invention:

  • on assure le maintien en froid de l'installation de distillation d'air en détendant dans une turbine de l'azote impur soutiré de la colonne basse pression, cet azote impur, après détente et réchauffement, étant de préférence utilisé pour régénérer des bouteilles d'adsorbant servant à l'épuration de l'air traité.
According to yet another particular embodiment of the invention:
  • the air distillation installation is kept cold by expelling impure nitrogen withdrawn from the low pressure column in a turbine, this impure nitrogen, after expansion and reheating, is preferably used to regenerate bottles of adsorbent used to purify the treated air.

Le compresseur d'azote et le compresseur d'air peuvent en particulier être reliés à une source motrice commune.The nitrogen compressor and the air compressor can particular be connected to a common motor source.

Un exemple de mise en oeuvre de l'invention va maintenant être décrit en regard du dessin annexé, dont la figure unique représente schématiquement une installation de production simultanée d'azote et d'oxygène sous haute pression pour réaliser un procédé conforme à l'invention.An example of implementation of the invention will now be described with reference to the appended drawing, the single figure of which represents schematically a plant for the simultaneous production of nitrogen and oxygen under high pressure to carry out a process in accordance with the invention.

L'installation représentée aux dessins est destinée à produire d'une part, sous 55 bar, de l'azote gazeux à haute pureté (contenant typiquement moins de 10 ppm d'oxygène), en un débit au moins égal à 20 % du débit d'air traité, et d'autre part, sous 65 bar, de l'oxygène ayant une pureté de 95 à 99,5 %, avec un rendement d'extraction élevé. Ces deux gaz sous haute pression seront utilisés sur un même site : on produira de l'hydrogène par réaction de l'oxygène sur des hydrocarbures lourds, et l'on fera réagir cet hydrogène et l'azote pour produire de l'ammoniac.The installation shown in the drawings is intended to produce on the one hand, under 55 bar, high purity nitrogen gas (containing typically less than 10 ppm oxygen), at a flow rate at least equal to 20% of the treated air flow, and on the other hand, under 65 bar, oxygen having a purity from 95 to 99.5%, with a high extraction yield. These two gases under high pressure will be used on the same site: we will produce hydrogen by reaction of oxygen with heavy hydrocarbons, and we will react this hydrogen and nitrogen to produce ammonia.

L'installation comprend essentiellement un compresseur d'air 1, un appareil 2 d'épuration de l'air par adsorption, une ligne d'échange thermique 3 du type à contre-courant, une double colonne de distillation 4, une turbine de détente 5, une pompe d'oxygène liquide 6, un compresseur d'azote 7, un compresseur d'oxygène 8 et une source d'énergie 9 constituée par exemple par une turbine à vapeur.The installation essentially comprises an air compressor 1, an apparatus 2 for air purification by adsorption, an exchange line thermal 3 of the counter-current type, a double distillation column 4, an expansion turbine 5, a liquid oxygen pump 6, a compressor of nitrogen 7, an oxygen compressor 8 and an energy source 9 consisting for example by a steam turbine.

La double colonne 4 comprend une colonne moyenne pression 10 surmontée d'une colonne basse pression 11 dont la partie d'extrémité supérieure forme un minaret 11A de production d'azote pur sous la basse pression. Un condenseur-vaporiseur 12 met en relation d'échange thermique la vapeur de tête (azote pratiquement pur) de la colonne 10 et le liquide de cuve (oxygène de pureté déterminée) de la colonne 11.The double column 4 comprises a medium pressure column 10 surmounted by a low pressure column 11, the end portion of which upper forms an 11A minaret of pure nitrogen production under the lower pressure. A condenser-vaporizer 12 puts in exchange relationship thermal the overhead vapor (practically pure nitrogen) from column 10 and the tank liquid (oxygen from determined purity) of column 11.

Comme il est classique, une conduite équipée d'une vanne de détente 13 permet de remonter du "liquide riche" (air enrichi en oxygène) de la cuve de la colonne 10 à un point intermédiaire de la colonne 11; une conduite équipée d'une vanne de détente 14 permet de remonter du "liquide pauvre inférieur"(azote impur) d'un point intermédiaire de la colonne 10 à la base du minaret 11A; et une conduite équipée d'une vanne de détente 15 permet de remonter du "liquide pauvre supérieur" (azote pratiquement pur) de la tête de la colonne 10 au sommet du minaret.As is conventional, an equipped pipe an expansion valve 13 makes it possible to raise "liquid rich "(oxygen-enriched air) from the column tank 10 at an intermediate point in column 11; a pipe fitted with an expansion valve 14 allows rise from the "lower lean liquid" (impure nitrogen) of a intermediate point of column 10 at the base of the minaret 11A; and a pipe fitted with an expansion valve 15 makes it possible to raise "upper lean liquid" (nitrogen practically pure) from the head of column 10 to the top minaret.

Le compresseur d'azote 7 est constitué d'un compresseur unique à trois étages. Les deux premiers étages comprennent chacun deux roues de compression et ont des taux de compression moyens par roue de 2 et 1,73 respectivement, tandis que le troisième étage comprend une roue de compression unique ayant un taux de compression de 1,83. Le taux de compression global du compresseur est donc 22. Chaque roue comporte à sa sortie un réfrigérant.The nitrogen compressor 7 consists of a single three-stage compressor. The first two floors each include two compression wheels and have average compression ratios per wheel of 2 and 1.73 respectively, while the third floor comprises a single compression wheel with a compression ratio of 1.83. The overall compression ratio of the compressor is therefore 22. Each wheel has at its output a refrigerant.

Le compresseur d'oxygène 8 est également constitué d'un compresseur unique. Ce compresseur possède six roues ayant un taux de compression moyen par roue de 1,37. Le taux de compression global est donc 6,5.The oxygen compressor 8 is also consisting of a single compressor. This compressor has six wheels with an average compression ratio per wheel of 1.37. The overall compression ratio is therefore 6.5.

L'arbre 16 du compresseur 7 est couplé à l'arbre 17 du compresseur 1 par un accouplement 18, et l'ensemble est entraíné par la source d'énergie commune 9. Eventuellement, l'arbre 16 peut entraíner les différents étages du compresseur 7 par l'intermédiaire de multiplicateurs de vitesse appropriés à chaque étage. Le compresseur 8 est entraíné par une source d'énergie séparée 19.The shaft 16 of the compressor 7 is coupled to the shaft 17 of the compressor 1 by a coupling 18, and the whole is driven by the common energy source 9. Optionally, the shaft 16 can cause the different compressor 7 stages via speed multipliers suitable for each stage. The compressor 8 is driven by an energy source separate 19.

La basse pression est choisie de manière que, multipliée par le taux de compression du compresseur 7, elle fournisse la haute pression de production désirée pour l'azote. Ainsi, en négligeant les pertes de charge, pour une haute pression d'azote de 55 bars, on choisit comme basse pression 55/22 = 2,5 bars. Pour un écart de température de 2°C dans le vaporiseur-condenseur 12, ceci correspond à une moyenne pression de l'ordre de 11 bars.The low pressure is chosen so that, multiplied by the compression ratio of compressor 7, it provides the desired high production pressure for nitrogen. So, by neglecting the pressure drops, for a high nitrogen pressure of 55 bars, we choose as low pressure 55/22 = 2.5 bars. For a difference of temperature of 2 ° C in the vaporizer-condenser 12, this corresponds to an average pressure of the order of 11 bars.

Ainsi, l'air entrant est comprimé à 11 bars dans le compresseur 1, épuré en 2, refroidi du bout chaud au bout froid de la ligne d'échange 3, et introduit au voisinage de son point de rosée en cuve de la colonne 10. L'azote basse pression pur sortant gazeux du sommet du minaret 11A et réchauffé à la température ambiante du bout froid au bout chaud de la ligne d'échange est introduit à l'aspiration du premier étage du compresseur 7, à l'exception éventuellement d'un débit d'azote produit en basse pression via une conduite 20. L'azote haute pression est produit au refoulement du troisième étage du compresseur et évacué via une conduite 21.Thus, the incoming air is compressed to 11 bars in compressor 1, purified in 2, cooled from the hot end at the cold end of the exchange line 3, and introduced to the near its dew point in tank of column 10. The pure low pressure nitrogen leaving gas from the top of the 11A minaret and warmed to room temperature cold end at the hot end of the exchange line is introduced to the suction of the first stage of the compressor 7, with the possible exception of a nitrogen flow produced at low pressure via line 20. Nitrogen high pressure is produced at the discharge of the third compressor stage and evacuated via line 21.

Le compresseur 7 est également utilisé comme compresseur de cycle à azote. En effet, de l'azote moyenne pression est soutiré en tête de la colonne 10, via une conduite 22, réchauffé à la température ambiante dans la ligne d'échange et introduit via une conduite 23 à l'aspiration du deuxième étage du compresseur 7. De l'azote à la haute pression de cycle est sorti au refoulement de ce deuxième étage via une conduite 24, refroidi, liquéfié et sous-refroidi dans la ligne d'échange, détendu à la moyenne pression dans une vanne de détente 25 et introduit en tête de la colonne 10.Compressor 7 is also used as nitrogen cycle compressor. Nitrogen medium pressure is drawn off at the top of column 10, via line 22, warmed to room temperature in the exchange line and introduced via a pipe 23 at the suction of the second stage of compressor 7. From nitrogen at high cycle pressure is released at discharge of this second stage via a pipe 24, cooled, liquefied and sub-cooled in the line exchange, expanded at medium pressure in a valve trigger 25 and introduced at the top of column 10.

Grâce à des moyens de réglage de débit non représentés, le débit d'azote circulant dans la conduite 24 est supérieur d'une quantité prédéterminée au débit d'azote circulant dans la conduite 23. La différence constitue un débit d'azote liquide additionnel, dit de soutien de rectification, introduit en reflux en tête de la colonne 10. Ce débit est prélevé sur le courant d'azote basse pression aspiré par le premier étage du compresseur 7.Thanks to non-adjustable flow adjustment means shown, the nitrogen flow flowing in the pipe 24 is greater than the flow rate by a predetermined amount of nitrogen flowing in line 23. The difference constitutes an additional flow of liquid nitrogen, known as rectification support, introduced at reflux at the top of column 10. This flow is taken from the current low pressure nitrogen drawn in from the first stage of the compressor 7.

De l'azote impur, constituant le gaz résiduaire de l'installation, est soutiré à la base du minaret 11A via une conduite 25, réchauffé à une température intermédiaire dans la ligne d'échange, sorti de cette dernière, détendu à la pression atmosphérique dans une turbine 5 qui assure le maintien en froid de l'installation, puis réintroduit dans la ligne d'échange, réchauffé jusqu'à la température ambiante, et enfin utilisé pour régénérer les bouteilles d'adsorption de l'appareil 2 et évacué de l'installation via une conduite 26.Impure nitrogen, constituting the waste gas of the installation, is withdrawn at the base of the minaret 11A via a pipe 25, heated to a temperature intermediary in the exchange line, out of the latter, relaxed at atmospheric pressure in a turbine 5 which keeps the installation cold, then reintroduced into the exchange line, warmed up to room temperature, and finally used to regenerate the adsorption bottles of device 2 and evacuated from the installation via a pipe 26.

L'oxygène sous 65 bars est produit de la manière suivante.Oxygen at 65 bar is produced from the next way.

Le débit d'oxygène liquide désiré est soutiré en cuve de la colonne 11, amené par la pompe 6 à une pression intermédiaire d'oxygène, vaporisé et réchauffé à la température ambiante dans la ligne d'échange 3, puis comprimé à la pression de production par le compresseur 8.The desired liquid oxygen flow is withdrawn in the tank of column 11, brought by pump 6 to a intermediate oxygen pressure, vaporized and heated at room temperature in exchange line 3, then compressed to production pressure by compressor 8.

Pour limiter au maximum les irréversibilités thermodynamiques dans la ligne d'échange, on fait en sorte que la vaporisation de l'oxygène liquide sous la pression intermédiaire d'oxygène s'effectue par condensation de l'azote sous la haute pression de cycle, avec une valeur subcritique pour cette haute pression, soit par exemple 30 bars. Cette valeur correspond à une vaporisation d'oxygène liquide sous environ 11 bars, qui est donc la pression fournie par la pompe 6.To minimize irreversibility thermodynamics in the exchange line, we do so that the vaporization of liquid oxygen under the intermediate oxygen pressure is achieved by condensation nitrogen under the high cycle pressure, with a subcritical value for this high pressure, either by example 30 bars. This value corresponds to a spray liquid oxygen at about 11 bar, which is therefore the pressure supplied by the pump 6.

Les considérations ci-dessus donnent les pressions pour les différents étages du compresseur 7 : 2,5 bars à l'entrée du premier étage, 11 bars à l'entrée du deuxième étage, 30 bars à l'entrée du troisième étage et 55 bars à la sortie de ce troisième étage.The above considerations give the pressures for the different stages of compressor 7: 2.5 bars at the entrance to the first floor, 11 bars at the entrance from the second floor, 30 bars at the entrance to the third floor and 55 bars at the exit of this third floor.

On peut montrer que le procédé décrit ci-dessus apporte un gain en investissement, par rapport au procédé classique où la basse pression est choisie légèrement supérieure à 1 bar, dès que le débit d'azote produit est au moins égal à 20% du débit d'air traité. Lorsque la production d'azote est supérieure à environ 30% du débit d'air, il apporte en outre un gain en énergie. Par ailleurs, le fait d'épurer l'air entrant sous 11 bars est très avantageux du point de vue économique.It can be shown that the process described above brings a gain in investment, compared to classic process where low pressure is chosen slightly higher than 1 bar, as soon as the nitrogen flow product is at least equal to 20% of the treated air flow. When nitrogen production is more than about 30% of the air flow, it also provides a gain in energy. Furthermore, purifying the incoming air under 11 bars is very advantageous from an economic point of view.

Claims (3)

  1. Process for the simultaneous production, on the one hand of pure nitrogen under a high nitrogen pressure between 50 and 60 bar and on the other hand oxygen, by distilling air in a double distillation column (4) comprising a medium pressure column (10) and a low pressure column (11) of the "minaret" type producing pure nitrogen at the top, wherein after heating the nitrogen coming from the low pressure column (11), it is compressed to the high pressure by means of a single nitrogen compressor (7) of the centrifuge type having at most six compression wheels, the low pressure column (11) is made to operate under a pressure of the order of PN/ρN, where PN denotes the high nitrogen pressure and ρN the compression ratio of the said nitrogen compressor; oxygen is produced under a high oxygen pressure greater than approximately 10 bar absolute, liquid oxygen withdrawn from the bottom of the low presure column (11) is brought by a pump (6) at an intermediate oxygen pressure and, after vaporizing and reheating the oxygen, it is compressed to the high oxygen pressure by means of a single oxygen compressor (8) of the centrifugal type having at most six compression wheels, the intermediate oxygen pressure being of the order of PO/ρO, where PO denotes the high oxygen pressure and ρO the compression ratio of the said oxygen compressor, the single nitrogen compressor (7) is used having three stages each with at most two wheels, and in addition the second stage is used to compress to an intermediate pressure between the medium pressure and the high pressure, a flow of cycle nitrogen withdrawn from the medium pressure column (10) and reheated, the compressed cycle nitrogen being cooled, liquefied, expanded to the medium pressure and introduced at the top of the medium pressure column (10) and in addition the first two stages are used for compressing from the low pressure to an intermediate pressure between the medium pressure and the high pressure a flow of nitrogen, a so called rectification maintenance flow, withdrawn from the top of the low pressure column (11) and reheated, this compressed nitrogen being cooled, liquefied, expanded to the medium pressure and introduced at the top of the medium pressure column (10).
  2. Process according to claim 1, characterized in that the cycle nitrogen is compressed to a sub-critical pressure for which the condensation temperature of nitrogen is slightly greater that the vaporization temperature of oxygen under the said intermediate oxygen pressure.
  3. Process according to either of claims 1 or 2, characterized in that the air distillation installation is kept cold by expanding in a turbine (5) impure nitrogen withdrawn from the low pressure column (11), this impure nitrogen, after expansion and reheating, being preferably used for regenerating bottles of absorbent (2) serving to purify the treated air.
EP93400522A 1992-03-24 1993-03-02 Process for the production of high pressure nitrogen and oxygen Expired - Lifetime EP0562893B2 (en)

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FR9203501A FR2689224B1 (en) 1992-03-24 1992-03-24 PROCESS AND PLANT FOR THE PRODUCTION OF NITROGEN AT HIGH PRESSURE AND OXYGEN.
FR9203501 1992-03-24

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CN106489059B (en) * 2014-07-05 2019-11-05 林德股份公司 Method and apparatus can be changed energy consumption low temperature air separating

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DE69310429T3 (en) 2001-08-23
EP0562893B1 (en) 1997-05-07
DE69310429T2 (en) 1997-12-11
CA2092140A1 (en) 1993-09-25
US5341647A (en) 1994-08-30
FR2689224A1 (en) 1993-10-01
CA2092140C (en) 1998-08-18
ES2101256T5 (en) 2001-03-16
EP0562893A1 (en) 1993-09-29
FR2689224B1 (en) 1994-05-06
ES2101256T3 (en) 1997-07-01
ZA932796B (en) 1993-09-30
DE69310429D1 (en) 1997-06-12

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