US3257814A - Process for the manufacture of oxygen-enriched air - Google Patents

Process for the manufacture of oxygen-enriched air Download PDF

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US3257814A
US3257814A US249056A US24905663A US3257814A US 3257814 A US3257814 A US 3257814A US 249056 A US249056 A US 249056A US 24905663 A US24905663 A US 24905663A US 3257814 A US3257814 A US 3257814A
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air
oxygen
duct
nitrogen
exchanger
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Carbonell Emile
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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
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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
    • F25J3/04763—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
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • 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
    • F25J3/04278—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using external refrigeration units, e.g. closed mechanical or regenerative refrigeration units
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low pressure column
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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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    • F25J3/04284—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
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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
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    • 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
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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
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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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
    • F25J3/04624—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 integrated mass and heat exchange, so-called non-adiabatic rectification, e.g. dephlegmator, reflux exchanger
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
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    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2240/42—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 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
    • 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
    • F25J2240/46—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 oxygen
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    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream being air
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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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One 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
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    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen
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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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/14—External refrigeration with work-producing gas expansion loop
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle

Definitions

  • This invention relates to a method for the production of oxygen-enriched air through low-temperature liquefaction and rectification, in which a portion at least of the air to be separated is compressed, purified and cooled close to its dew point, then subjected to a fractionate condensation under reflux, and the liquid oxygen-enriched fraction is expanded, then vaporized through indirect heat exchange with the condensing air, while the residual nitrogen gas is also expanded, then warmed up close to room temperature and discharged.
  • An object of this invention is to allow the direct production of oxygen-enriched air containing 40% to 45% oxygen by volume, without a rectifying column and with a significantly smaller expense of refrigeration energy than through the preparation of essentially pure oxygen in rectifying columns or through the use of the back return apparatus of French Patent No. 324,460.
  • This is achieved through compressing the air to a comparatively low pressure, 2.3 to 3 absolute atmospheres, i.e. significantly less than in the known methods.
  • the equipment is extremely simple and comparatively cheap; besides the air compressor and heat exchangers, among which one reflux exchanger, it requires only one expanding machine, preferably a turbine, in view of the low differential pressure and of the high fiow rate of the gas to be expanded.
  • the method of the invention is characterised in that the oxygen-enriched fraction is supercooled, before it is expanded, through heat exchange with the previously expanded residual nitrogen.
  • the elimination of carbon dioxide from the air to be separated may be effected through any known means: chemically (absorption of carbon dioxide by a solution of sodium hydroxide), through freezing in an exchanger with recurrent defrosting, or through adsorption.
  • the preferred method is the elimination of carbon dioxide in a heat exchanger with recurrent permutation of gas streams (regenerator or reversing exchanger) through freezing of the carbon dioxide during cooling, followed by the vaporization of the latter in both separated fractions, the difference of temperatures at the cold end of the exchanger where the 3,257,814 Patented June 28, 1956 carbon dioxide deposits being kept sufiiciently low to allow the complete vaporization of the carbon dioxide by warming up an auxiliary stream of gas through countercurrent passage of the air to be cooled through an additional compartment of the said exchanger.
  • This auxiliary stream is advantageously constituted by a portion of the compressed nitrogen gas from the reflux condenser, which is then combined with the other portion before it is
  • it can also be a stream of nitrogen circulating through a closed circuit, which is warmed up in the additional compartment of the exchanger, then warmed up close to room temperature, compressed, cooled again close to its temperature at the outlet of the additional compartment, then expanded with external work and reintroduced into the cold end of the additional compartment.
  • this requires the use of an additional compressor and expanding machine, as well as of another exchanger, or the adjunction of addition exchange compartments to an existing exchanger.
  • the auxiliary gas stream can also be a fraction of the air to be separated, bled at the cold end'of the exchanger where the carbon dioxide deposits, then expanded after warming up and combined with the nitrogen separated at low pressure at the cold end of the said exchanger.
  • An installation for carrying out the method of the invention essentially includes a low-pressure air compressor (2.3 to 3 absolute atmospheres); a warm exchange device in the range between room temperature and about 180 C, a cold exchange device in the range between about 180 and the dew point of the air under the relevant pressure; a reflux condensing device ensuring the fractionate condensation of the air, thesupercooling and vaporization of the oxygen-enriched liquid; and an expansion turbine.
  • the various heat-exchange devices can be tubular exchangers of the usual type, regenerators or reversing exchangers.
  • the fractionated condensation of air can be carried out by means of a reflux condenser of the type described in French Patent No. 1,123,353 for another application (condensation of ethylene from furnace gases), or in British Patents Nos. 783,186 (September 18-, 1957) and 843,119 (August 4, 1960), or in British Patent No. 847,523 (September 7, 1960), the oxygenenriched liquid being super-cooled in a special exchanger. Both operations can also be carried out at once by means of a battery of three regenerators with circular permutation, each one being successively traversed by cold air under pressure, by the oxygen-enriched liquid (previously expanded), and by nitrogen (previously expanded with external work).
  • Another object of the invention is to allow the production of air with a higher oxygen content than by the above method, and more particularly of superoxygenated air with an oxygen content between and by volume, more especially suitable for some applications in iron metallurgy, particularly for enriching furnace blasts.
  • the French patent application No. P.V. 889,349 of February 27, 1962 already discloses a method for producing air with about 70% oxygen content from air compressed to 3.5-4 absolute atmospheres, thus with a notably smaller expense of energy than in air separation installations of the usual type.
  • the latter method requires much the same equipment as the known methods, notably two successive rectifying columns under difincludes, beside the reflux condenser described above,
  • An additional object of the invention is to make it possible to produce superoxyge'nated air, and incidentally a certain amount of pure oxygen, with a reduced expense of energy.
  • This embodiment is characterised in that the abovementioned oxygen-enriched vaporized fraction or part of that fraction is fed into the bottom of a rectifying column, into the top of which is fed the nitrogen separated in the reflux condensation, after liquefaction through heat exchang with liquid oxygen containing about 6070% 0 and expansion to a pressure close to the pressure of the oxygen-enriched vaporized fraction.
  • This embodiment of the invention also involves the following variations, taken together or separately:
  • the gas fraction subjected to expansion with external work is an air fraction compressed to a lower pressure than the air subjected to reflux condensation, and also cooled through heat exchange with the products of the separation through rectification;
  • a fraction of the liquid oxygen (about 70% 0 from the bottom of the rectifying column is separated in an auxiliary rectifying column into essentially pure liquid oxygen and a gas fraction which is returned to the main rectifying column;
  • a third line another portion of the air compressed to a comparatively low pressure is cooled through heat exchange with another portion of the nitrogen separated under low pressure.
  • Those three separate heat-exchange lines are provided because the flow rate of low-pressure nitrogen is considerably higher than the flow rate of intermediatepressure air, while the flow rate of low-pressure air is considerably higher than the flow rate'of low-pressure 60-70% oxygen.
  • the excess low-pressure air is therefore cooled through heat exchange with the excess low-pressure nitrogen.
  • the improvement defined hereafter is meant to make it possible to carry out the cooling and purifying of the bulk of the air in regenerators less costly than exchangers with recurrent inversion of the gas streams; it makes it possible to use one such exchanger only, which treats a small flow of air.
  • auxiliary air fraction is cooled and purified counter-current to the gas containing 60-70% 0 in a first heat-exchange line made of a first battery of regenerators; the air fraction to be condensed under reflux is cooled and purified counter-current to the nitrogen separated in a second heat-exchange line made of a second battery of regenerators, while another auxiliary air fraction, purified separately from its cooling, is cooled in a third heat-exchange line, counter-current to a portion of the separated nitrogen, taken from the excess nitrogen over and above the air fraction to be condensed under reflux, in the middle zone of the second battery of regenerators, and is afterwards fed in the gaseous state into the middle zone of the rectifying column; part of the first auxiliary air fraction is bled from the middle zone of the first battery of regenerators, with such a flow rate that the residual air flow is lower than the flow of 6070'% oxygen gas in the coldest zone of the first battery of regenerators, then purified and also fed in the gaseous state into
  • FIG. 1 of the drawing shows an installation in which the complete sublimation of the carbon dioxide deposited in the reversing heat exchangers is ensured through the circulation, in a special compartment of those exchangers, of a nitrogen fraction taken from the outlet of the reflux condenser, then warmed up and combined with the main nitrogen fraction under pressure at the inlet of the expansion turbine.
  • FIG. 2 shows an installation in which the sublimation is replaced by a set of three regenerators with circular permutation.
  • FIG. 5 shows an installation for the production of oxygen containing about 6070% 0 in which a rectifying column is added to the reflux condenser.
  • FIG. 6 shows an installation for the production of oxygen containing about 60-70% 0 similar to the installation shown on FIG. 5, but with an additional auxiliary rectifying column for the production of a small amount of 99.5% oxygen.
  • FIG. 7 shows an installation for the production of oxygen containing about 6070% 0 similar to the installation shown on FIG. 5, but where the air is cooled through heat exchange with the separated nitrogen and oxygen in two separate batteries of regenerators.
  • the air to be separated is raised by turbo-compressor 10 to 2.7 absolute atmospheres. It is fed through duct 11 into reversing heat exchanger 1, where it is cooled to about 95 C., exchanging heat with the separated enriched air and nitrogen, and where the moisture is deposited as ice. It then goes through duct 14 to exchanger 2, with ternary permutation of the air, nitrogen and oxygen circuits, where it is cooled to about 180 C., and through duct 17 to exchanger 3 where it is cooled to approximately 183 C., close to its dew' point.
  • the cooled and purified air is then fed through duct 22 into the bottom of reflux condenser 4, where it is cooled through indirect contact counter-current to the oxygen-rich liquid separated in this condenser, supercooled and expanded; it condenses progressively while flowing upwards in the exchanger, and the liquid thus formed runs down counter-current to the ascending gas.
  • a liquid containing 40-45% 0 is collected in vessel 30; the gases from that liquid are returned through duct 31 to the bottom of condenser 4.
  • the second fraction of nitrogen under pressure is sent through duct 25, with flow regulation by valve 35, to a special compartment of exchanger 3, where it warms up countercurrent to the separated enriched air and nitrogen. It emerges from the warm end of this exchanger through duct 26; one portion is directly combined through valve 37 with the first nitrogen fraction from valve 36; another portion is sent through duct to a special compartment of exchanger 2, where it warms up again; it is then returned through duct 21 to a special tube nest of exchanger 3, where it cools down again before it is combined through duct 50 with the nitrogen fraction fed through duct 51 into turbine 41.
  • the oxygen-enriched liquid collected in vessel 30 is sent through duct 32 to exchanger 5, where it is supercooled to approximately -189 C. through heat exchange with the cold nitrogen expanded with .external work (see above). It is then expanded in valve 33 whose down- This nitrogen is divided into two fractions.
  • the installation shown on FIG. 2 is largely similar to the installation shown on FIG. 1, but the difference of temperatures at the cold end of the exchangers where carbon dioxide deposits is maintained, not through warming up a fraction of the nitrogen separated under pressure, but through a closed cycle of nitrogen.
  • a stream of nitrogen, compressed by turbo-compressor to a pressure between 5 and 15 kg./sq. cm., is sent through duct 51 to exchanger 1, where it cools down counter-current to the air to be separated, then through duct 52 to turbine 53, where it expands.
  • exchanger 2 a flow of cold gas higher than the flow of the air to be cooled, since the nitrogen expanded in turbine 53 has not been previously cooled in that exchanger.
  • exchanger 3 the excess flow of cold gas is maintained as in the installation shown in FIG. 1, through warming up in a special compartment of that exchanger a fraction of the nitrogen under pressure separated in the reflux condenser.
  • the installation shown in FIG. 3 is also similar to the installation shown in FIG. 1, but the excess flow of cold gas inside exchanger 2 is maintained through bleeding at the cold end of that exchanger 21 small fraction of the cooled air under pressure, which is introduced through expanding valve into a special compartment of that exchanger; after having warmed up, this air fraction is combined, through duct 61 and valve 62, with the low-pressure nitrogen introduced into the cold end of that exchanger through duct 18; part of it may also be diverted and combined, through duct 63 and valve 64, with the low-pressure nitrogen introduced through duct 23 into the cold end of exchanger 3.
  • the above installations involve the use of exchangers with recurrent inversion of the air and nitrogen circuits
  • the latter may be replaced by regenerators, provided with internal tube nests to carry the nitrogen under pressure to be expanded with external work, which must not be polluted by the carbon dioxide deposited from the air.
  • the reflux condenser may be replaced by a set of three regenerators, successively traversed by the air to be condensed, by the nitrogen expanded with external work, and by the oxygenenriched liquid, counter-current to the above air.
  • FIG. 4 shows only the three regenerators 4A, 4B and 4C, which replace the reflux condenser and ensure the supercooling of the oxygen-enriched liquid.
  • regenerator 4A The essentially pure nitrogen separated at the top of regenerator 4A through duct 34 is warmed up, expanded with external work in a turbine (not shown), then warmed up by passing through regenerator 4B and discharged through duct 23.
  • regenerator 4A When regenerator 4A has warmed up to such an extent that the separation of the air becomes inadequate, the regenerators undergo a circular permutation: air is introduced into regenerator 4B, while regenerator 4A is cooled by the expanded oxygen-enriched liquid, and regenerator 4C by the nitrogen expanded with external work (FIG. 4b).
  • regenerator 4C air at the dew point is introduced into regenerator 4C, while regenerators 4A and 4B are cooled respectively by low-pressure nitrogen and by oxygen-enriched liquid.
  • the air to be separated is introduced through duct 11 into turbo-compressor 12, which discharges it under 2.4 absolute atmospheres into duct 13. It is then divided into two fractions.
  • the first fraction which makes up about 67% of the whole, is compressed again by turbo-compressor 15 to 4.3 absolute atmospheres, then through duct 16, counter-current to a portion of the nitrogen separated under low pressure, into exchangers 1C and 2C, with recurrent inversion of the air and nitrogen streams by means of two sets of valves (21A, 21B, 22A, 22B, and 71A, 71B, 72A, 723).
  • exchangers can be for instance compact weldedalu-minum exchangers of the type sold by Compagnie Europenne de Matriels Thermiques.
  • the air cools down in these exchangers, and deposits its moisture and carbon dioxide in the solid state.
  • a portion (about 18%) of the cooled air is bled through duct 80, with flow control by valve 8-1, and returned counter-current to the air to be cooled into a special compartment of the exchanger, so as to reduce the difference of temperatures between air and nitrogen at the cold end of the exchanger.
  • the main portion of the air is combined through valve 82 with the warmed-up portion, and the combined streams are fed through duct 83 into exchanger 3, where they are cooled down close to the dew point through heat exchange with the nitrogen separated in rectifying column 6, and with part of the nitrogen from expansion turbine 7, as described below.
  • the first air fraction under higher pressure, close to its dew point, is fed through duct 84 into the bottom of reflux condenser 4, where it rises with progressive condensation through indirect contact counter-current to the oxygen-enriched liquid separated in the same condenser, then supercooled and expanded; there emerges at the bottom of the said condenser, through duct 32, a liquid containing to 0 which is collected in vessel 33; the gases from that liquid are returned through duct 34 to the condenser.
  • the oxygen-enriched liquid from vessel 33 is sent through duct 35 to exchanger 5, where it is supercooled countercurrent to pure nitrogen from the rectifying column, as described below; it then goes through duct 36 to expanding valve 37 (2.4 atmospheres) and is returned to reflux condenser 4, where it is vaporized through indirect heat exchange with the air under pressure being condensed. It is then fed through duct 38 into the bottom of rectifying column 6.
  • the nitrogen emerging from the top of reflux condenser still contains about 1% to 5% oxygen.
  • This nitrogen goes through duct 39 to exchanger 40, where it is condensed through heat exchange with superoxygenated air (-70% 0 separated in rectifying column 6, as described below. It then goes through duct 41 to exchanger 42, where it is supercooled through heat exchange with nitrogen expanded in turbine 7, and is fed through duct 43 into the top of rectifying column 6, as reflux liquid, after having been expanded to 2.4 atmospheres in valves 44.
  • the second air fraction under 2.4 atmospheres, is divided in two portions at the outlet of duct 14.
  • the first portion is cooled and purified, counter-current to oxygen, in reversing exchangers 1A and 2A, fitted with valve sets 17A, 17B, 18A, 18B and 63A, 63B, 64A, 6413, which ensure the recurrent inversions between air and oxygen.
  • exchanger 2C complete sublimation of the deposited carbon dioxide is ensured by returning a portion of the cooled air, bled through duct 73 and warmed up counter-current to the incoming air, with flow control by valve 74.
  • the air thus warmed up is then mixed again with the main fraction going through valve 75, and the combined streams go through duct A.
  • the second portion of the low pressure air is cooled and purified counter-current to a portion of the lowpressure nitrogen in reversing exchanger 18, fitted with two sets of valves 19A, 19B, 20A, 20B and 67A, 67B, 63A, 68B.
  • Exchanger 2B also contains a tube nest for the return of the air bled through duct 76 with flow control by valve 77. After this air has been combined by valve 78 to the main stream of air, the second portion of cooled low-pressure air goes through duct 79.
  • Complete sublimation of the deposited carbon dioxide may of course be obtained by means of a closed circuit of nitrogen, or of air bleeding warmed up in special tube nests, then combined with separated nitrogen or oxygen, according to the variations shown in FIGS. 2 and 3.
  • the low-pressure air and the oxygen-enriched gas fed in the gaseous state into that column through duct 38 are separated therein into a liquid containing about 60% to 70% oxygen, essentially in equilibrium with the gas fed in the gaseous state through duct 38, and into essentially pure nitrogen.
  • the superoxygenated liquid air is sent through duct 45 and expanding valve 46, under approximately 1.2 atmospheres, to exchanger 40, where it is vaporized through heat exhange with the nitrogen issuing from reflux condenser 4; it then goes through ducts 47 and 62 to heat exchangers 2A and 1A, where it warms up close to room temperature, before it is sent to use by duct 90.
  • the essentially pure nitrogen emerging from the head of column 6 is sent through duct 48 to exchange 5, where it warms up through heat exchange with the oxygen-enriched liquid separated in reflux condenser 4, then through duct 49 to exchanger 3, where it warms up again, and is then fed through duct 50 into expansion turbine 7 under approximately 1.2 atmospheres. It then ensures in exchanger 42 the supercooling of the liquid nitrogen sent to column 6, then goes through ducts 51, 52 and 53 respectively to heat exchangers 3 and 2C, 1C or 2B, 1B, before it is discharged through ducts 26 or 28, then 29.
  • the pressures of both air fractions are slightly higher than those of FIG. 5: 2.5 to 3 absolute atmospheres for the low-pressure fraction and 4.5 to 5 absolute atmospheres for the high-pressure fraction.
  • Cold is produced by expanding the low-pressure air fraction with external work in turbine 7 before it is fed into the main rectifying column 6, which works under approximately 1.2 atmospheres.
  • a portion only of the high-pressure air fraction is fed into reflux condenser 4, as above.
  • Another portion is sent through duct 60 to exchanger 61, where it condenses through heat exchange with 60-70% liquid oxygen, bled from the bottom of main column 6 through duct 45 and already partly vaporized in exchanger 40. It then goes through duct 62 to expanding valve 63 (1.2 atmospheres), and is then fed through duct 64 into column 6.
  • a third portion is sent through duct 65 to coil 66, laid inside the sump of auxiliary rectifying column 8, where it condenses by warming up the bottom of that column. It then goes through duct 67 to expanding valve 68 (1.2 atmospheres), and is then fed, also through duct 64, into column 6.
  • the low-pressure air introduced through duct 14 is divided into a first auxiliary fraction going through duct 114 and another auxiliary fraction, with a much lower flow rate, going through duct 214.
  • the first auxiliary fraction is cooled and purified in regenerators 191A and 191B, through which the streams of air and of 6070% oxygen are circulated alternatively, by means of a set of valves 192A, 192B, 193A, 193B, and of the valve boxes shown schematically in 194A, 194B.
  • valves 192A and 19313 are open, valves 1923 and 193A are closed, and the valve boxes have the arrangement shown, so that the air goes through regenerator 191A and coo-ls down through contact with the latters packing, while depositing its carbon dioxide in the solid state in the coldest zone of the regenerator; on the other hand, the oxygen at 60-70% 0 warms up through contact with the packing of regenerator 1918.
  • the cooled and purified air then goes through ducts 115 and 75A to exchanger 3, then through duct 31 to the rectifying column.
  • valve 195A which opens into the middle zone of regenerator 191A (average temperature: approximately 120 C.), and is combined through duct 196 (the corresponding valve 195B, linked to regenerator 191B, being closed) to the other auxiliary air fraction, previously cooled in reversing exchanger 1A, at the inlet of adsorbing body 104, which may be made of silica gel, and which ensures the purification of the air going through it; the stream is then combined through duct 215 with the air issuing through duct 115 from the cold ends of regenerators 191A and 191Bv
  • one absorbing body 104 only is shown, for the sake of clearness, two such bodies are usually provided in parallel, one in the working stage and the other in the regeneration stage.
  • auxiliary air fraction which has a comparatively low flow rate, so computed as to allow the recovery of cold from the low-pressure nitrogen bled from the middle zone of regenerators 91A and 91B, goes through duct 214 to reversing exchanger 1A, which is provided with two sets of reversing valves A, 100B, 101A, 101B and 102A, 102B, 103A, 103B. In the working stage shown, valves 100A, 101B, 103A and 102B are open, and the other valves are closed.
  • the air is fed into the exchanger through valve 100A and leaves it through valve 103A, while the nitrogen issuing from the middle zone of regenerator 91B through valve 95B and duct 96 is fed through valve 102B into exchanger 1A and leaves it through valve 101B; the warmed-up nitrogen is combined through duct 98 with the nitrogen issuing from the warm end of regenerator 913.
  • the air cooled down to approximately l00 C. in the exchanger is combined, at the inlet of adsorbing body 104, with the air from the middle zones of regenerators A and 195B; the combined air streams are decarbonated, then go through ducts 75A to exchanger 3 and through duct 31 to rectifying column 6.
  • a method for the production of oxygen-enriched air through low-temperature liquefaction and rectification comprising the steps of:
  • auxiliary air stream is cooled and purified countercurrent to the gas of about 60% to 70% oxygen obtained after the liquefaction of said residual nitrogen gas in a first heat-exchange line made of a first set of regenerators
  • said air stream is cooled and purified countercurrent to said separated nitrogen stream in a second heat-exchange line made of a second set of regenerators
  • a second auxiliary air stream purified independently from its cooling, is cooled in a third heat-exchange line countercurrent to a portion of the separated nitrogen taken from the excess nitrogen separated over and above said air stream and bled from the middle zone of said second set of regenerators
  • said second auxiliary air stream is also fed in the gaseous state into the middle zone of said rectifying column, and part of the first auxiliary air stream is bled from the middle zone of said first set of regenerators with such a flow rate that the residual flow of air is lower than the flow of gas of about 60% to 70% oxygen in the coldest zone of said first set of regenerators and is then purified

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FR883934A FR1322843A (fr) 1962-01-05 1962-01-05 Procédé de fabrication d'air enrichi en oxygène
FR894365A FR82408E (fr) 1962-01-05 1962-04-13 Procédé de fabrication d'air enrichi en oxygène
FR913755A FR82626E (fr) 1962-01-05 1962-10-29 Procédé de fabrication d'air enrichi en oxygène

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Cited By (9)

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US3392536A (en) * 1966-09-06 1968-07-16 Air Reduction Recompression of mingled high air separation using dephlegmator pressure and compressed low pressure effluent streams
US3401531A (en) * 1965-05-19 1968-09-17 Linde Ag Heat exchange of compressed nitrogen and liquid oxygen in ammonia synthesis feed gas production
US3416323A (en) * 1966-01-13 1968-12-17 Linde Ag Low temperature production of highly compressed gaseous and/or liquid oxygen
US3421333A (en) * 1964-08-28 1969-01-14 Linde Ag Thawing technique for a single air separation plant
US3490246A (en) * 1965-08-20 1970-01-20 Linde Ag Split pressure low temperature process for the production of gases of moderate purity
US3500651A (en) * 1966-01-13 1970-03-17 Linde Ag Production of high pressure gaseous oxygen by low temperature rectification of air
US3699695A (en) * 1965-10-29 1972-10-24 Linde Ag Process of separating air into an oxygen-rich fraction suitable for blast furnace operation
US4308043A (en) * 1980-08-15 1981-12-29 Yearout James D Production of oxygen by air separation
EP1239247A1 (en) * 2001-03-08 2002-09-11 Air Products And Chemicals, Inc. Method for providing refrigeration to parallel heat exchangers

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US2673456A (en) * 1949-06-16 1954-03-30 Standard Oil Dev Co Separation of low boiling gas mixtures
US2715323A (en) * 1948-09-11 1955-08-16 Hydrocarbon Research Inc Production of oxygen by liquefaction and rectification of air
US2753698A (en) * 1952-03-05 1956-07-10 Linde Eismasch Ag Method and apparatus for fractionating air and power production
US2802349A (en) * 1951-08-25 1957-08-13 Kellogg M W Co Removing impurities from a gas liquefaction system with aid of extraneous gas stream
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FR324460A (fr) * 1902-09-15 1903-04-01 Claude Georges Perfectionnements dans la fabrication de l'oxygène à l'aide de l'air liquide
DE589916C (de) * 1932-07-21 1933-12-20 Linde Eismasch Ag Verfahren zur Gewinnung von an Sauerstoff angereicherten Gemischen aus Luft
DE1112095B (de) * 1959-11-17 1961-08-03 Linde Eismasch Ag Verfahren und Einrichtung zur Erzeugung fluessiger Gaszerlegungs-produkte

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US1945367A (en) * 1931-06-13 1934-01-30 Air Liquide Process for the separation of gaseous mixtures
US2000992A (en) * 1934-01-31 1935-05-14 Air Reduction Separation of constituents of gaseous mixtures
GB632329A (en) * 1947-05-14 1949-11-21 British Oxygen Co Ltd Improvements in or relating to the separation of air
US2626510A (en) * 1947-06-18 1953-01-27 Air Prod Inc Air fractionating cycle and apparatus
US2650481A (en) * 1948-01-27 1953-09-01 Kellogg M W Co Separation of gaseous mixtures
US2715323A (en) * 1948-09-11 1955-08-16 Hydrocarbon Research Inc Production of oxygen by liquefaction and rectification of air
US2673456A (en) * 1949-06-16 1954-03-30 Standard Oil Dev Co Separation of low boiling gas mixtures
US2664719A (en) * 1950-07-05 1954-01-05 Union Carbide & Carbon Corp Process and apparatus for separating gas mixtures
US2802349A (en) * 1951-08-25 1957-08-13 Kellogg M W Co Removing impurities from a gas liquefaction system with aid of extraneous gas stream
US2753698A (en) * 1952-03-05 1956-07-10 Linde Eismasch Ag Method and apparatus for fractionating air and power production
US2850880A (en) * 1955-01-05 1958-09-09 Linde Eismasch Ag Process and an apparatus for the separation of compressed air
US2918802A (en) * 1956-09-27 1959-12-29 Air Liquide Process of separation of air into its elements
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Cited By (9)

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Publication number Priority date Publication date Assignee Title
US3421333A (en) * 1964-08-28 1969-01-14 Linde Ag Thawing technique for a single air separation plant
US3401531A (en) * 1965-05-19 1968-09-17 Linde Ag Heat exchange of compressed nitrogen and liquid oxygen in ammonia synthesis feed gas production
US3490246A (en) * 1965-08-20 1970-01-20 Linde Ag Split pressure low temperature process for the production of gases of moderate purity
US3699695A (en) * 1965-10-29 1972-10-24 Linde Ag Process of separating air into an oxygen-rich fraction suitable for blast furnace operation
US3416323A (en) * 1966-01-13 1968-12-17 Linde Ag Low temperature production of highly compressed gaseous and/or liquid oxygen
US3500651A (en) * 1966-01-13 1970-03-17 Linde Ag Production of high pressure gaseous oxygen by low temperature rectification of air
US3392536A (en) * 1966-09-06 1968-07-16 Air Reduction Recompression of mingled high air separation using dephlegmator pressure and compressed low pressure effluent streams
US4308043A (en) * 1980-08-15 1981-12-29 Yearout James D Production of oxygen by air separation
EP1239247A1 (en) * 2001-03-08 2002-09-11 Air Products And Chemicals, Inc. Method for providing refrigeration to parallel heat exchangers

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GB913755A (en) 1962-12-28
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DE1266773B (de) 1968-04-25
FR82626E (fr) 1964-03-20
GB1033931A (en) 1966-06-22
NL287429A (xx)
BE626588A (xx)
FR82408E (fr) 1964-02-07

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