EP0605262B1 - Process and apparatus for the production of gaseous oxygen under pressure - Google Patents

Process and apparatus for the production of gaseous oxygen under pressure Download PDF

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Publication number
EP0605262B1
EP0605262B1 EP93402665A EP93402665A EP0605262B1 EP 0605262 B1 EP0605262 B1 EP 0605262B1 EP 93402665 A EP93402665 A EP 93402665A EP 93402665 A EP93402665 A EP 93402665A EP 0605262 B1 EP0605262 B1 EP 0605262B1
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EP
European Patent Office
Prior art keywords
pressure
column
low
oxygen
production
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Revoked
Application number
EP93402665A
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German (de)
French (fr)
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EP0605262A1 (en
Inventor
Alain Guillard
Norbert Rieth
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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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
Publication of EP0605262A1 publication Critical patent/EP0605262A1/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
    • F25J3/042—Division of the main heat exchange line in consecutive sections having different functions having an intermediate feed connection
    • 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
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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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04157—Afterstage cooling and so-called "pre-cooling" of the feed air upstream the air purification unit and main heat exchange line
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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
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    • 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
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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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
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    • 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
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F25J3/0426—The cryogenic component does not participate in the fractionation
    • 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
    • F25J3/04406—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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • F25J3/0486—Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/0489—Modularity and arrangement of parts of the air fractionation unit, in particular of the cold box, e.g. pre-fabrication, assembling and erection, dimensions, horizontal layout "plot"
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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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04945—Details of internal structure; insulation and housing of the cold box
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/50—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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being nitrogen
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • 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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
    • F25J2240/44—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval the fluid being nitrogen
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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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
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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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62—Details of storing a fluid in a tank
    • 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
    • Y10S62/912—External refrigeration system
    • Y10S62/913—Liquified gas

Definitions

  • the present invention relates to a production process gaseous oxygen under pressure by means of a double column of distillation.
  • gaseous oxygen under pressure takes place generally either by compression of gaseous oxygen withdrawn from the column low pressure at a pressure close to atmospheric pressure, i.e. by vaporization of liquid oxygen brought by pump to the pressure of production.
  • the corresponding installations are complex because they require special rotating machines such as a compressor of oxygen or one or more expansion turbines.
  • EP-A-0102190 describes a process of the "toggle" type which allows the production of variable oxygen flows.
  • FR-A-2578532 describes a double column process, the column medium pressure and the low pressure column each having a condenser with means for sending liquid nitrogen from the column low pressure at the medium pressure column.
  • US-A-3316725 describes an air separation apparatus in which the air is purified after a relaxation step in a relaxation machine. Air liquid sent to and from the purification device is expanded by expansion Joule-Thomson.
  • EP-A-461804 describes a method according to the preamble of claim 1.
  • the process of Figures 1 and 2 can be modified to allow production pure oxygen.
  • the object of the invention is to provide a method for producing particularly economical way of gaseous oxygen under pressure moderate.
  • the invention also relates to an installation according to the claim 3.
  • the double column can in particular be vacuum-insulated, in particular by a vacuum envelope which contains only the double column and pipe sections, the rest of the cold parts of the installation, with the possible exception of sources of liquid nitrogen and / or of liquid oxygen and the pipes which leave from it, being insulated by a box cold at atmospheric pressure containing a solid insulator, in particular particulate.
  • FIG. 1 essentially comprises a air compressor 1, adsorption purification device 2, one line heat exchange 3, a sub-cooler 4 and a double column of distillation 5.
  • the latter consists essentially of a column medium pressure 6 surmounted by a low pressure column 7, and a vaporizer-condenser 8 which brings the indirect heat exchange relationship into overhead vapor (practically pure nitrogen) from column 6 and tank liquid (oxygen at desired purity) from column 7.
  • the air to be distilled is compressed in 1 at a pressure, so-called medium pressure, of the order of 8 to 16 bars, purified in water and anhydride carbonic in 2, cooled near its dew point in 3 and introduced in the bottom of column 6.
  • the "rich liquid” (oxygen enriched air) collected in tank of this column is sub-cooled in 4, expanded in an expansion valve 9 at a pressure, called low pressure, which is substantially the production pressure, of the order of 2 to 5 bars, and introduced at a level column 7 via line 10.
  • From “poor liquid” (practically pure nitrogen) collected in head of column 6 is sub-cooled in 4, expanded in an expansion valve 11 at low pressure, and introduced at the head of column 7 via a line 12.
  • Oxygen production is withdrawn in gaseous form from the tank from column 7, heated in exchange line 3 and recovered directly as a product via a pipe 13.
  • the residual gas W (impure nitrogen), withdrawn at top of column 7 via line 14, is relaxed in free expansion at a pressure slightly higher than atmospheric pressure in an expansion valve 15, heated in sub-cooler 4 then in the line exchange 3, and evacuated via a pipe 16. This gas can serve to regenerate the adsorbers of the device 2.
  • the installation shown is isolated thermally as follows.
  • the double column 5 is arranged in a vacuum envelope 22, which ensures one high performance insulation.
  • This envelope does contains, in addition to the double column, that the sections of conducts that lead to it or leave it, these conducts passing through the enclosure by means of appropriate fittings 23. In practice, it is advantageous to bring together all fittings 23 in the same region of the envelope.
  • the vacuum envelope can have a diameter closely matched to the outside diameter of the double column, which can be of constant diameter on its full height, which allows for a set double column 5-envelope 22 conveniently transportable.
  • this solution is also very beneficial, although it is much less expensive than vacuum insulation containing the entire installation. Indeed, in an air distillation installation, 75 to 85% of heat losses are borne by the double column and, in the heat exchange line, the losses are concentrated in the coldest part. In total, insulation performance of the 22-24 assembly is around 90% of those that would be obtained with a vacuum insulation of the entire installation.
  • the double column may include a "minaret", that is to say an upper section of the low pressure column 7 enabling sound to be produced top of nitrogen gas under low pressure.
  • this nitrogen gas can also be expanded in an expansion valve to the vicinity of the pressure atmospheric to produce cold, before being reheated in 4 then in 3 then to be recovered as second product of the installation.
  • the cold behavior of installation is carried out by free expansion of the gas W waste in 15, supplemented by an oxygen supply liquid from a source 19 constituted as previously from storage 19A at atmospheric pressure and a 19B pump.
  • the oxygen make-up liquid pumped in 19B at some pressure little higher than the low pressure, is injected, in one intermediate point 25 of the heat exchange line 3, in gaseous oxygen during heating.
  • an oxygen purge line 26 liquid fitted with a valve 27, starts from the tank of the column 7 and opens into storage 19A to supply it partly, the supplement of liquid oxygen being brought in by tankers 28.
  • the purge intended to evacuate the hydrocarbons from column 7, corresponds to about 0.2% of the flow treated air and preferably takes place discontinuously, usually automatically; it is independent of "bottle feeding" of the installation by liquid oxygen.
  • the injection point 25 is chosen so that liquid oxygen vaporizes at a temperature high enough for the oil to show more danger of explosion or flammability when vaporization of oxygen. This temperature can thus be of the order of -100 ° C.

Description

La présente invention est relative à un procédé de production d'oxygène gazeux sous pression au moyen d'une double colonne de distillation.The present invention relates to a production process gaseous oxygen under pressure by means of a double column of distillation.

Les pressions dont il est question dans le présent mémoire sont des pressions absolues.The pressures discussed in this brief are absolute pressures.

La production d'oxygène gazeux sous pression s'effectue généralement soit par compression d'oxygène gazeux soutiré de la colonne basse pression sous une pression voisine de la pression atmosphérique, soit par vaporisation d'oxygène liquide amené par pompe à la pression de production. Les installations correspondantes sont complexes, car elles nécessitent des machines tournantes spéciales tel qu'un compresseur d'oxygène ou une ou plusieurs turbines de détente.The production of gaseous oxygen under pressure takes place generally either by compression of gaseous oxygen withdrawn from the column low pressure at a pressure close to atmospheric pressure, i.e. by vaporization of liquid oxygen brought by pump to the pressure of production. The corresponding installations are complex because they require special rotating machines such as a compressor of oxygen or one or more expansion turbines.

EP-A-0102190 décrit un procédé du type "à bascule" qui permet la production de débits variables d'oxygène.EP-A-0102190 describes a process of the "toggle" type which allows the production of variable oxygen flows.

FR-A-2578532 décrit un procédé à double colonne, la colonne moyenne pression et la colonne basse pression étant chacune surmontée d'un condenseur avec des moyens pour envoyer de l'azote liquide de la colonne basse pression à la colonne moyenne pression.FR-A-2578532 describes a double column process, the column medium pressure and the low pressure column each having a condenser with means for sending liquid nitrogen from the column low pressure at the medium pressure column.

US-A-3316725 décrit un appareil de séparation d'air dans lequel l'air est épuré après une étape de détente dans une machine de détente. De l'air liquide envoyé à et provenant de l'appareil d'épuration est détendu par détente Joule-Thomson.US-A-3316725 describes an air separation apparatus in which the air is purified after a relaxation step in a relaxation machine. Air liquid sent to and from the purification device is expanded by expansion Joule-Thomson.

EP-A-461804 décrit un procédé selon le préambule de la revendication 1. Le procédé des figures 1 et 2 peut être modifié pour permettre la production d'oxygène pur.EP-A-461804 describes a method according to the preamble of claim 1. The process of Figures 1 and 2 can be modified to allow production pure oxygen.

L'invention a pour but de fournir un procédé permettant de produire de façon particulièrement économique de l'oxygène gazeux sous une pression modérée.The object of the invention is to provide a method for producing particularly economical way of gaseous oxygen under pressure moderate.

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

Suivant d'autres caractéristiques :

  • on détend par détente libre un gaz résiduaire soutiré de la tête de la colonne basse pression.
According to other characteristics:
  • a residual gas withdrawn from the head of the low pressure column is released by free expansion.

L'invention a également pour objet une installation selon la revendication 3.The invention also relates to an installation according to the claim 3.

Dans une telle installation, la double colonne peut en particulier être isolée sous vide, notamment par une enveloppe sous vide qui ne contient que la double colonne et des tronçons de conduite, le reste des parties froides de l'installation, à l'exception éventuellement des sources d'azote liquide et/ou d'oxygène liquide et des conduites qui en partent, étant isolées par une boíte froide à la pression atmosphérique contenant un isolant solide, notamment particulaire.In such an installation, the double column can in particular be vacuum-insulated, in particular by a vacuum envelope which contains only the double column and pipe sections, the rest of the cold parts of the installation, with the possible exception of sources of liquid nitrogen and / or of liquid oxygen and the pipes which leave from it, being insulated by a box cold at atmospheric pressure containing a solid insulator, in particular particulate.

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

  • la Figure 1 représente schématiquement une installation de production d'oxygène conforme à l'invention; et
  • la Figure 2 représente schématiquement une variante.
Examples of implementation of the invention will now be described with reference to the accompanying drawings, in which:
  • Figure 1 schematically shows an oxygen production installation according to the invention; and
  • Figure 2 schematically shows a variant.

L'installation représentée à la Figure 1 comprend essentiellement un compresseur d'air 1, un appareil 2 d'épuration par adsorption, une ligne d'échange thermique 3, un sous-refroidisseur 4 et une double colonne de distillation 5. Cette dernière est essentiellement constituée d'une colonne moyenne pression 6 surmontée d'une colonne basse pression 7, et d'un vaporiseur-condenseur 8 qui met en relation d'échange thermique indirect la vapeur de tête (azote pratiquement pur) de la colonne 6 et le liquide de cuve (oxygène à la pureté désirée) de la colonne 7.The installation shown in Figure 1 essentially comprises a air compressor 1, adsorption purification device 2, one line heat exchange 3, a sub-cooler 4 and a double column of distillation 5. The latter consists essentially of a column medium pressure 6 surmounted by a low pressure column 7, and a vaporizer-condenser 8 which brings the indirect heat exchange relationship into overhead vapor (practically pure nitrogen) from column 6 and tank liquid (oxygen at desired purity) from column 7.

En fonctionnement, l'air à distiller est comprimé en 1 à une pression, dite moyenne pression, de l'ordre de 8 à 16 bars, épuré en eau et en anhydride carbonique en 2, refroidi au voisinage de son point de rosée en 3 et introduit en cuve de la colonne 6. Le "liquide riche" (air enrichi en oxygène) recueilli en cuve de cette colonne est sous-refroidi en 4, détendu dans une vanne de détente 9 à une pression, dite basse pression, qui est sensiblement la pression de production, de l'ordre de 2 à 5 bars, et introduit à un niveau intermédiaire de la colonne 7 via une conduite 10. Du "liquide pauvre" (azote pratiquement pur) recueilli en tête de la colonne 6 est sous-refroidi en 4, détendu dans une vanne de détente 11 à la basse pression, et introduit en tête de la colonne 7 via une conduite 12. L'oxygène de production est soutiré sous forme gazeuse de la cuve de la colonne 7, réchauffé dans la ligne d'échange 3 et récupéré directement en tant que produit via une conduite de production 13.In operation, the air to be distilled is compressed in 1 at a pressure, so-called medium pressure, of the order of 8 to 16 bars, purified in water and anhydride carbonic in 2, cooled near its dew point in 3 and introduced in the bottom of column 6. The "rich liquid" (oxygen enriched air) collected in tank of this column is sub-cooled in 4, expanded in an expansion valve 9 at a pressure, called low pressure, which is substantially the production pressure, of the order of 2 to 5 bars, and introduced at a level column 7 via line 10. From "poor liquid" (practically pure nitrogen) collected in head of column 6 is sub-cooled in 4, expanded in an expansion valve 11 at low pressure, and introduced at the head of column 7 via a line 12. Oxygen production is withdrawn in gaseous form from the tank from column 7, heated in exchange line 3 and recovered directly as a product via a pipe 13.

Pour assurer le maintien en froid de l'installation, le gaz résiduaire W (azote impur), soutiré au sommet de la colonne 7 via une conduite 14, est détendu en détente libre à une pression légèrement supérieure à la pression atmosphérique dans une vanne de détente 15, réchauffé dans le sous-refroidisseur 4 puis dans la ligne d'échange 3, et évacué via une conduite 16. Ce gaz peut servir à régénérer les adsorbeurs de l'appareil 2.To keep the installation cold, the residual gas W (impure nitrogen), withdrawn at top of column 7 via line 14, is relaxed in free expansion at a pressure slightly higher than atmospheric pressure in an expansion valve 15, heated in sub-cooler 4 then in the line exchange 3, and evacuated via a pipe 16. This gas can serve to regenerate the adsorbers of the device 2.

Si le froid produit par cette détente libre est insuffisant, on peut le compléter par l'un au moins des moyens suivants, représentés en trait mixte sur le dessin.

  • Une source 17 d'azote liquide sous la basse pression, reliée à la tête de la colonne 7 via une conduite 18 et munie de moyens de régulation de débit. Comme représenté, il peut s'agir notamment d'un stockage 17A d'azote liquide sous la pression atmosphérique muni à sa sortie d'une pompe 17B.
  • Une source 19 d'oxygène liquide sous la basse pression, reliée à la cuve de la colonne 7 via une conduite 20 et munie de moyens de régulation de débit. Comme représenté, il peut s'agir de nouveau d'un stockage 19A d'oxygène liquide sous la pression atmosphérique muni à sa sortie d'une pompe 19B.
  • Un groupe frigorifique 21, par exemple à l'ammoniac, monté entre le compresseur 1 et l'appareil d'épuration 2 et prérefroidissant l'air comprimé jusqu'à une température de l'ordre de 0 à +° 5°C par exemple.
If the cold produced by this free expansion is insufficient, it can be supplemented by at least one of the following means, shown in phantom in the drawing.
  • A source 17 of liquid nitrogen under low pressure, connected to the head of the column 7 via a pipe 18 and provided with flow control means. As shown, it may especially be a storage 17A of liquid nitrogen at atmospheric pressure provided at its outlet with a pump 17B.
  • A source 19 of liquid oxygen under low pressure, connected to the tank of the column 7 via a pipe 20 and provided with flow regulation means. As shown, it may again be a storage 19A of liquid oxygen under atmospheric pressure provided at its outlet with a pump 19B.
  • A refrigeration unit 21, for example with ammonia, mounted between the compressor 1 and the purification device 2 and pre-cooling the compressed air to a temperature of the order of 0 to + 5 ° C for example .

L'installation représentée est isolée thermiquement de la manière suivante.The installation shown is isolated thermally as follows.

D'une part, la double colonne 5 est disposée dans une enveloppe sous vide 22, qui en assure une isolation à haute performance. Cette enveloppe ne contient, outre la double colonne, que les tronçons de conduite qui y aboutissent ou en partent, ces conduites traversant l'enveloppe au moyen de raccords appropriés 23. En pratique, il est avantageux de rassembler tous les raccords 23 dans une même région de l'enveloppe.On the one hand, the double column 5 is arranged in a vacuum envelope 22, which ensures one high performance insulation. This envelope does contains, in addition to the double column, that the sections of conducts that lead to it or leave it, these conducts passing through the enclosure by means of appropriate fittings 23. In practice, it is advantageous to bring together all fittings 23 in the same region of the envelope.

D'autre part, à l'exception des sources de liquides cryogéniques 17 et 19 et des conduites qui en partent, qui possèdent leur propre isolation, généralement sous vide, toutes les autres parties froides de l'installation sont isolées au moyen d'une boíte froide 24 sous la pression atmosphérique contenant un matériau isolant solide particulaire, qui est de préférence de la perlite.On the other hand, with the exception of sources of cryogenic liquids 17 and 19 and pipes which leave, which have their own insulation, usually under vacuum, all other cold parts of the installation are isolated by means of a cold box 24 at atmospheric pressure containing material particulate solid insulation, which is preferably of the perlite.

Ce mode d'isolation est très avantageux d'une part, l'enveloppe sous vide peut avoir un diamètre étroitement adapté au diamètre extérieur de la double colonne, laquelle peut être de diamètre constant sur toute sa hauteur, ce qui permet de réaliser un ensemble double colonne 5-enveloppe 22 commodément transportable.This method of isolation is very advantageous on the one hand, the vacuum envelope can have a diameter closely matched to the outside diameter of the double column, which can be of constant diameter on its full height, which allows for a set double column 5-envelope 22 conveniently transportable.

De plus, tous les accessoires froids tels que 9, 11, 15 sont facilement accessibles puisqu'ils sont constamment à la pression atmosphérique.In addition, all cold accessories such as 9, 11, 15 are easily accessible since they are constantly at atmospheric pressure.

Du point de vue énergétique, cette solution est également très avantageuse, bien qu'elle soit beaucoup moins coûteuse qu'une isolation sous vide renfermant l'ensemble de l'installation. En effet, dans une installation de distillation d'air, 75 à 85% des pertes thermiques sont supportées par la double colonne et, dans la ligne d'échange thermique, les pertes sont concentrées dans la partie la plus froide. Au total, les performances d'isolation de l'ensemble 22-24 sont de l'ordre de 90% de celles qui seraient obtenues avec une isolation sous vide de l'ensemble de l'installation.From an energy point of view, this solution is also very beneficial, although it is much less expensive than vacuum insulation containing the entire installation. Indeed, in an air distillation installation, 75 to 85% of heat losses are borne by the double column and, in the heat exchange line, the losses are concentrated in the coldest part. In total, insulation performance of the 22-24 assembly is around 90% of those that would be obtained with a vacuum insulation of the entire installation.

En variante, la double colonne peut comporter un "minaret", c'est-à-dire un tronçon supérieur de la colonne basse pression 7 permettant de produire à son sommet de l'azote gazeux sous la basse pression. Dans ce cas, cet azote gazeux peut également être détendu dans une vanne de détente jusqu'au voisinage de la pression atmosphérique pour produire du froid, avant d'être réchauffé en 4 puis en 3 puis d'être récupéré en tant que second produit de l'installation.Alternatively, the double column may include a "minaret", that is to say an upper section of the low pressure column 7 enabling sound to be produced top of nitrogen gas under low pressure. In this case, this nitrogen gas can also be expanded in an expansion valve to the vicinity of the pressure atmospheric to produce cold, before being reheated in 4 then in 3 then to be recovered as second product of the installation.

La simplicité de l'installation suivant l'invention rend celle-ci particulièrement intéressante pour la production de quantités modérées, par exemple de l'ordre de quelques dizaines de tonnes par jour, d'oxygène gazeux sous une pression de quelques bars.The simplicity of the following installation the invention makes it particularly interesting for the production of moderate quantities, for example of the order of a few tens of tonnes per day of oxygen gaseous under a pressure of a few bars.

Dans la variante représentée à la Figure 2 sans son isolation thermique, la tenue en froid de l'installation s'effectue par détente libre du gaz résiduaire W en 15, complétée par un apport d'oxygène liquide provenant d'une source 19 constituée comme précédemment d'un stockage 19A à la pression atmosphérique et d'une pompe 19B.In the variant shown in Figure 2 without its thermal insulation, the cold behavior of installation is carried out by free expansion of the gas W waste in 15, supplemented by an oxygen supply liquid from a source 19 constituted as previously from storage 19A at atmospheric pressure and a 19B pump.

Toutefois, dans cette variante, l'oxygène liquide d'appoint, pompé en 19B à une pression quelque peu supérieure à la basse pression, est injecté, en un point intermédiaire 25 de la ligne d'échange thermique 3, dans l'oxygène gazeux en cours de réchauffement.However, in this variant, the oxygen make-up liquid, pumped in 19B at some pressure little higher than the low pressure, is injected, in one intermediate point 25 of the heat exchange line 3, in gaseous oxygen during heating.

De plus, une conduite 26 de purge d'oxygène liquide, munie d'une vanne 27, part de la cuve de la colonne 7 et débouche dans le stockage 19A pour l'alimenter en partie, le complément d'oxygène liquide étant apporté par des camions-citernes 28.In addition, an oxygen purge line 26 liquid, fitted with a valve 27, starts from the tank of the column 7 and opens into storage 19A to supply it partly, the supplement of liquid oxygen being brought in by tankers 28.

La purge, destinée à évacuer les hydrocarbures de la colonne 7, correspond à environ 0,2% du débit d'air traité et s'effectue de préférence en discontinu, généralement automatiquement; elle est indépendante du "biberonnage" de l'installation par l'oxygène liquide.The purge, intended to evacuate the hydrocarbons from column 7, corresponds to about 0.2% of the flow treated air and preferably takes place discontinuously, usually automatically; it is independent of "bottle feeding" of the installation by liquid oxygen.

Le point d'injection 25 est choisi de manière que l'oxygène liquide se vaporise à une température suffisamment élevée pour que les hydrocarbures ne présentent plus de danger d'explosion ou d'inflammabilité lors de la vaporisation de l'oxygène. Cette température peut ainsi être de l'ordre de -100°C.The injection point 25 is chosen so that liquid oxygen vaporizes at a temperature high enough for the oil to show more danger of explosion or flammability when vaporization of oxygen. This temperature can thus be of the order of -100 ° C.

Claims (5)

  1. Process for the production of gaseous oxygen under pressure by means of a double distillation column (5), in which process the gaseous production oxygen is collected directly in the bottom of a low-pressure column (7):
    the low-pressure column (7) is made to operate at a pressure well above atmospheric pressure and slightly above the oxygen production pressure, this low pressure being especially about 2 to 5 bar, and the medium-pressure column (6) is made to operate at a corresponding pressure, especially about 8 to 16 bar;
    characterized in that
    the plant is kept cold, at least partly, by the free expansion of at least one gaseous product leaving the low-pressure column and the plant is kept cold without having to use the expansion, with the production of external work, of a fluid intended for or coming from the double column and, if the plant is partially kept cold by free expansion, a stream of liquid nitrogen coming from a source (17) external to the double column (5) is injected at (18) into the low-pressure column (7) and/or a stream of liquid oxygen coming from a source (19) external to the double column (5) is injected (at 20) into the low-pressure column (7) and/or a stream of liquid oxygen coming from a source external to the double column is injected into the gaseous oxygen (at 25) at an intermediate point on the heat-exchange line (3) associated with the double column (5), and in that some purge liquid oxygen withdrawn (at 26) from the bottom of the low-pressure column (7) is sent into the said source (19) and/or the air to be treated, before it is purified by adsorption (at 2), is precooled by means of a refrigerating unit (21).
  2. Process according to Claim 1, characterized in that a waste gas (W) withdrawn from the top of the low-pressure column (7) is expanded by free expansion.
  3. Plant for the production of gaseous oxygen under pressure, of the type comprising: an air compressor (1); an apparatus (2) for purifying the compressed air; a double column (5) for distilling the purified air, the double column itself comprising a medium-pressure column (6) and a low-pressure column (7) which are coupled via a reboiler (8); a heat-exchange line (3) for cooling the purified air by indirect heat exchange with the product coming from the double column; and means (15, 17-18, 19-20, 21) for keeping the plant cold, an oxygen production pipe (13) being directly connected to the bottom of the low-pressure column in order to withdraw gaseous oxygen therefrom, the low-pressure column (7) operating at a pressure well above atmospheric pressure and slightly above the oxygen production pressure, this low pressure being especially about 2 to 5 bar, characterized in that the means for keeping the plant cold comprise a valve (15) for the free expansion of at least one gaseous product leaving the low-pressure column (7) and, optionally, at least one of the following means for keeping the plant cold:
    a) means for injecting a stream of liquid nitrogen and/or of liquid oxygen, coming from one or both sources (17, 19) at the low pressure(s) external to the double column, into the low-pressure column,
    b) means for injecting a stream of liquid oxygen at the low pressure, coming from a source (19) external to the double column, into the gaseous oxygen at an intermediate point on the heat-exchange line and means for sending some purged liquid oxygen withdrawn from the bottom of the low-pressure column into the said source,
    c) the refrigerating unit (21) mounted between the compressor (1) and the purification apparatus (2),
    which means for keeping the plant cold do not include a machine or turbine for the expansion, with production of external work, of a fluid intended for or coming from the double column.
  4. Plant according to Claim 3, characterized in that the expansion valve (15) is mounted in a pipe (14) for discharging waste gas (W) coming from the top of the low-pressure column (7).
  5. Plant according to Claim 3, in which the double column is vacuum-insulated.
EP93402665A 1992-12-30 1993-10-29 Process and apparatus for the production of gaseous oxygen under pressure Revoked EP0605262B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR9215925A FR2699992B1 (en) 1992-12-30 1992-12-30 Process and installation for producing gaseous oxygen under pressure.
FR9215925 1992-12-30

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EP0605262A1 EP0605262A1 (en) 1994-07-06
EP0605262B1 true EP0605262B1 (en) 2000-06-28

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EP (1) EP0605262B1 (en)
JP (1) JPH06229668A (en)
CA (1) CA2112499A1 (en)
DE (1) DE69328922T2 (en)
FR (1) FR2699992B1 (en)

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EP0605262A1 (en) 1994-07-06
CA2112499A1 (en) 1994-07-01
JPH06229668A (en) 1994-08-19
DE69328922T2 (en) 2000-11-16
US5408831A (en) 1995-04-25
FR2699992A1 (en) 1994-07-01
DE69328922D1 (en) 2000-08-03
FR2699992B1 (en) 1995-02-10

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