US3371496A - Wash liquid production by heat exchange with low pressure liquid oxygen - Google Patents

Wash liquid production by heat exchange with low pressure liquid oxygen Download PDF

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US3371496A
US3371496A US385426A US38542664A US3371496A US 3371496 A US3371496 A US 3371496A US 385426 A US385426 A US 385426A US 38542664 A US38542664 A US 38542664A US 3371496 A US3371496 A US 3371496A
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liquid
oxygen
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low pressure
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Seidel Max
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Linde GmbH
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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
    • F25J3/04769—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
    • 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
    • F25J3/04242—Cold end purification of the feed air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/04418—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system with thermally overlapping high and low pressure columns
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/34—Processes or apparatus using separation by rectification using a side column fed by a stream from the low pressure column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/38—Processes or apparatus using separation by rectification using pre-separation or distributed distillation before a main column system, e.g. in a at least a double column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • 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
    • 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
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/40—One fluid being air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen

Definitions

  • the present invention relates to the production of gases containing high concentrations of oxygen. More particularly, it relates to the production of gaseous mixtures containing from 70 to 98% of elemental oxygen by the fractionation of air.
  • the condensate formed is then separated from the non-condensed portion of the oxygennitrogen mixture and is returned to the prewashing column for prewashing the air, while the non-condensed portion is delivered to the foot of the high pressure section (hereinafter designated alternatively as pressure column) of the double rectification column.
  • the washing fluid which has been enriched to about 43% oxygen content in the prewashing column, after being cleaned in adsorbers, is delivered to the low pressure rectification column below the outlet of the oxygen-rich mixture from the foot of the pressure column.
  • the above process has the disadvantage of a reduction in the economy of energy consumption as the oxygen content of the end product increases, as compared to the amount of energy required in the normal two column rectification process.
  • the above improvement is accomplished by withdrawing from the sump of the low pressure column a preliminary product containing a lower oxygen content than the end product, this preliminary product before its evaporation being brought to the oxygen content of the end product by intermediate evaporation with partial condensation of a further fraction passing from the prewashing column to a pressure column whereby the vapors obtained are returned to the foot of the low pressure column.
  • Another feature of the present invention resides in the fact that the intermediate concentration can be increased by enriching with oxygen the liquid preliminary product taken from'the low pressure column, this enrichment being effected by rectification by means of vapors formed during the concentration before the preliminary product is subjected to concentration.
  • the heaters used for the-intermediate concentration ice and for the vaporization of the end product are connected the head of the pressure column is condensed in a known manner.
  • the condensation pressure of this nitrogen depends on the pressure in the sump of the low pressure column and on the oxygen content of the liquid to be vaporized.
  • the liquid in the sump of the low pressure column has the same oxygen content as the preliminary product taken for concentration.
  • the boiling temperature at which the intermediate product is concentrated and at which the end product is vaporized is higher, because of the higher oxygen content, than the boiling temperature in the sump of the low pressure column.
  • Concentration of the intermediate product is continued until the liquid has an oxygen content equal to the oxygen content of the end product and under a pressure which, in case of the presence of an enriching rectification, is greater than the pressure over the sumpof the low pressure column by an amount equal to the resistance of the enriching rectification between the low pressure column and the intermediate vaporizer,
  • the intermediate concentration is higher than the boiling temperature of the liquid in the sump of the low pressure rectification-column.
  • an air. fraction having a low 0 content must be condensed and, in fact, according to the present invention, is in the form of the air to be fractionated which is being passed through the prewashing column.
  • the evaporating liquid acquires an oxygen content which will be in equilibrium with the vapors of the end product, eg in the following ratios:
  • oxygen in gaseous end product oxygen in gaseous end product: 98% oxygen in gaseous end product:
  • the air fraction coming from the prewashing column is first used to provide heat for the vaporization of the intermediate product and then, after separation of the oxygen-rich partial condensate, to effect vaporization of the end product by means of the remaining oxygen-poor vapors.
  • the heating is effected in the reverse order, first by vaporization of the end product and then with the remaining somewhat oxygen poor vapors by evaporation of the intermediate product.
  • the oxygen content of the air fraction that is used for heating can be influenced.
  • the partial condensates in this case which are not returned to the fractionation column are returned to the pressure column together with the non-condensed portion of the air fraction used for heating.
  • the oxygen enrichment of the liquid drawn from the bottom of the pressure column and delivered to the low pressure column can be increased if a portion of the air fraction coming from the prewashing column is diverted from between the end product vaporizer and the intermediate vaporizer, or from ahead of both of the latter and after by-passing one or both Vaporizers, is introduced into the pressure column at a point below the inlet for the residual gases that were oxygen impoverished by partial condensation in the intermediate and final Vaporizers heated thereby.
  • FIGURES l, 2 and 3 show schematically three specific examples of systems operating in accordance with the present invention for obtaining oxygen of 80%, 90% and 98% purity. Those elements which are the same in the figures are designated by the same reference characters. In order to illustrate more clearly the novel features of the invention for the production of oxygen of difierent degrees of purity, minor details which are not critical to the invention have been omitted. It is understood, therefore, that minor variations from the procedures set forth in the specific examples below which would be obvious to one skilled in the art are regarded as a part of the present invention, so long as they do not depart from the basic concept of the invention disclosed herein.
  • FIG. 1 Production of ca. oxygen (FIGURE 1) Through conduit 1 were introduced 102,700 Nm. /h. of air under a pressure of approximately 4.0 atm. The air was cooled and freed from water vapor and carbon dioxide by passage first through regenerators 2, 4 and 6, and during the next switching period, through regenerators 3, 5 and 7. The remaining air, amounting to about 100,000 N /h., then passed through conduit 8 to the prewashing column 9 provided with rectification trays 10. In this column the remaining air was washed by the condensate produced during the heating of the final vaporizer 20 and intermediate vaporizer The washing liquid, amounting to about 35,000 Nm.
  • the cleansed liquid was then passed by conduit 13 through heat exchanger 14 and expansion valve 17 to the inlet 18 of low pressure column 16 where it was expanded to the pressure of about 1.3 atm. which prevailed in the column.
  • the cleansed gaseous air fraction flowing from the head of the prewashing column 9 had an oxygen content of about 14%.
  • a portion or this air fraction was delivered by conduit 19a to the final vaporizer 20 in which it was partially liquefied by heat exchange with the liquefied end product delivered by conduit 21 from rectification column 102, the partially liquefied air fraction being there delivered to the separator 22.
  • conduits 24a and 24b were passed by conduits 24a and 24b from the heads of the separators and delivered collectively by conduit 24 to pressure column 15 of the double rectifier which was under a pressure of about 3.7 atm.
  • a portion of the nitrogen which had been somewhat warmed in the heat exchanger 34 was delivered through conduit 40 to the heat exchanger 41 where it was warmed to room temperature countercurrently to itself while being compressed in a dry run compresser 42 to about atm. and then again cooled in heat exchanger 41 and liquefied in heat exchanger 34.
  • the liquid nitrogen was then passed through expansion valve 43 and through valve 445 to the high pressure column 15, and/ or was added via valve 44a to the liquid nitrogen flowing from the high pressure column 15 through heat exchanger 30 to the low pressure column 16.
  • the vapors produced in the intermediate vaporizer 100 were then delivered to the enrichment rectification column 102 in mass transfer with the outward flowing preliminary product, while gaseous residue containing about 53% oxygen taken from the head of this column was delivered by conduit 54 to the low pressure column 16.
  • the intermediate vaporizer 100 is represented as a circulating vaporizer.
  • the portion of the vaporizing liquid remaining after circulation was returned by conduit 53 to the preliminary product in the intermediate vaporizer.
  • the 90% oxygen liquid end product was delivered from the rectification column 102 through conduit 21 to the final vaporizer in which it was vaporized.
  • the liquid portion remaining after circulation of the vaporizing liquid having an oxygen content of about 97% in equilibrium with the vapors containing 90% oxygen, was separated and removed from the foot of the separator by conduit 46 for passage through the adsorber 47 which during continuous circulation was traversed by the vaporizing liquid.
  • the gaseous end product about 22,000 Nm. /h. 90% oxygen, consisting of 19,200 Nmfi/h. of pure oxygen and 2,800 Nm. /h. of air, was removed by conduit 48 from the head of the separator 45, to be warmed in the regenerator 7 to room temperature from which is escaped through conduit 49.
  • regenerator pairs 2/3, 4/5 and 6/7 The functioning of the regenerator pairs 2/3, 4/5 and 6/7 was reversed periodically in a known manner.
  • the settings of the valve groups 50a and 50c to the warm sides of the regenerators and of the groups of recoil valves 51a and 51c to the cold sides are indicated by the flow directions in the regenerators.
  • the compressed nitrogen to be passed through the expansion turbine 36 can be prewarmed in heating coils in the regenerator pairs, or a pair of regenerators is provided With a central pipe connection from which a portion of the air to be fractionated after being passed through one of the pair of transposable adsorbers is passed through an expansion turbine and then into the low pressure column.
  • the gaseous end product was composed of 25,200 Nm. /l1. of 80% oxygen, consisting of 18,800 Nm. /h. of pure oxygen and 6,400 Nm. /h. of air.
  • a process for producing gas of 70-98% oxygen purity in a double rectifier having a high pressure column and a low pressure column comprising the steps of:
  • step (f) conducting partial vaporization of at least one of steps (c) and (e) in indirect heat exchange with washed cold gaseous air from step (b) to partially condense same;
  • step (g) instead of being delivered to the prewashing column, is delivered to the lower portion of the high pressure column at a point corresponding to its composition.
  • step (b) 4. The process of claim 1 wherein one portion of the washed cold gaseous air from the prewashing column, step (b), is passed directly to the foot of the high pressure column and another portion is used to furnish heat for the intermediate partial vaporization, and for the final partial vaporization of said second liquid fraction, and is then passed to the high pressure column at a point above that at which the first portion is introduced.
  • step (b) the liquid preliminary product from the sump of the low pressure column is enriched with oxygen by rectification by means of the first vapor fraction generated by the intermediate partial vaporization, before said preliminary product is subjected to intermediate partial vaporization, and one portion of the washed cold gaseous air from the prewashing column, step (b), is passed directly to the foot of the pressure column and another portion is used to furnish heat for the intermediate partial vaporization and for the final vaporization of the product, and is then passed to the high pressure column at a point above that at which the first portion is introduced.
  • step (f) is conducted by conducting partial vaporization of step (c), and resultant condensed air formed during the intermediate partial vaporization is separated from the non-condensed portion of the fractionated air and delivered as a washing liquid to the prewashing column.
  • step (g) instead of being delivered to the prewashing column, is delivered to the lower portion of the high pressure column at a point corresponding to its composition.
  • the intermediate partial vaporization is performed as a circulating vaporization wherein the non-vaporized liquid is separated during each circulation from its vapors, a portion of said liquid being further concentrated to produce said first liquid fraction which is to undergo said final partial vaporization, while the remainder of said liquid together with the preliminary product from the low pressure rectification column is admixed and subjected to further concentration.
  • An apparatus including a double rectifier in combination with regenerators for heat exchange between the air to be fractionated and the fractionation products and a final vaporizer for vaporization of the liquid products taken from the sump of the low pressure column by heat exchange with a partially condensing fraction taken in gaseous form from a prewashing column and its liquefied portion being returned as washing liquid to the prewashing column while the washing liquid which drains from the prewashing column is delivered to the low pressure column at a point below the point where the liquid from the sump of the high pressure column is introduced, the improvement which comprises an intermediate vaporizer distinct and separate from said final vaporizer and connected to the sump of the low pressure column to receive liquid therefrom to be concentrated while the vapors are returned to the column, means for heating said vaporizer by an air fraction taken from the head of a prewashing column, and means for returning at least a portion of said air fraction to the lower part of the said high pressure column.
  • the intermediate vaporizer is in the form of a circulating vaporizer with means for delivering its vapors to the low pressure column, in combination with means for delivering its liquid to the final vaporizer.
  • the apparatus of claim 16 comprising a condensate separator in the discharge conduit for the partly condensed air fraction from the intermediate or final vaporizer, the upper part of the separator being connected to the lower part of the high pressure column while the lower part is connected to the head of the prewashing column, the outlet conduit for the partly condensed air fraction from one of the two Vaporizers being connected directly to the lower part of the high pressure column.
  • the apparatus of claim 16 comprising a conduit with a throttle valve directly between the head of the 1G prewashing column and the foot of the high pressure column, and a parallel conduit having in its path the heating jackets of the intermediate vaporizer and final vaporizer.
  • the apparatus of claim 16 comprising a conduit with a throttle valve directly between the head of the prewashing column and the foot of the high pressure column, and a parallel conduit having in its path the heating jackets of the intermediate vaporizer and final vaporizer, the heating jackets of the intermediate vaporizer and final vaporizer being connected in parallel.
  • the apparatus of claim 16 comprising a conduit with a throttle valve directly between the head of the prewashing column and the foot of the high pressure column, and a parallel conduit having in its path the heating jackets of the intermediate vaporizer and final vaporizer, having heating jackets of the intermediate vaporizer and final vaporizer connected in series for countercurrent stagewise vaporization.
  • the apparatus of claim 16 comprising a conduit with a throttle valve directly between the head of the prewashing column and the foot of the high pressure column, and a parallel conduit having in its path the heating jackets of the intermediate vaporizer and final vaporizer, connected in series for unidirectional stagewise vaporization.
US385426A 1963-03-29 1964-07-27 Wash liquid production by heat exchange with low pressure liquid oxygen Expired - Lifetime US3371496A (en)

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DEG37391A DE1187248B (de) 1963-03-29 1963-03-29 Verfahren und Einrichtung zur Gewinnung von Sauerstoffgas mit 70 bis 98% O-Gehalt

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DE (1) DE1187248B (de)
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NL (1) NL6407747A (de)

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US4072023A (en) * 1975-10-03 1978-02-07 Linde Aktiengesellschaft Air-rectification process and apparatus
US5220796A (en) * 1991-07-15 1993-06-22 The Boc Group, Inc. Adsorption condensation solvent recovery system
US5265429A (en) * 1992-02-21 1993-11-30 Praxair Technology, Inc. Cryogenic air separation system for producing gaseous oxygen
DE102007031765A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren zur Tieftemperaturzerlegung von Luft
DE102007031759A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren und Vorrichtung zur Erzeugung von gasförmigem Druckprodukt durch Tieftemperaturzerlegung von Luft
DE102009034979A1 (de) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von gasförmigem Drucksauerstoff
EP2312248A1 (de) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Verfahren und Vorrichtung Gewinnung von Drucksauerstoff und Krypton/Xenon
EP2458311A1 (de) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102010052544A1 (de) 2010-11-25 2012-05-31 Linde Ag Verfahren zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2520886A1 (de) 2011-05-05 2012-11-07 Linde AG Verfahren und Vorrichtung zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2568242A1 (de) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von Stahl
EP2600090A1 (de) 2011-12-01 2013-06-05 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von Drucksauerstoff durch Tieftemperaturzerlegung von Luft
DE102011121314A1 (de) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Verfahren zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102013017590A1 (de) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Verfahren zur Gewinnung eines Krypton und Xenon enthaltenden Fluids und hierfür eingerichtete Luftzerlegungsanlage
DE102012017488A1 (de) 2012-09-04 2014-03-06 Linde Aktiengesellschaft Verfahren zur Erstellung einer Luftzerlegungsanlage, Luftzerlegungsanlage und zugehöriges Betriebsverfahren
EP2784420A1 (de) 2013-03-26 2014-10-01 Linde Aktiengesellschaft Verfahren zur Luftzerlegung und Luftzerlegungsanlage
WO2014154339A2 (de) 2013-03-26 2014-10-02 Linde Aktiengesellschaft Verfahren zur luftzerlegung und luftzerlegungsanlage
EP2801777A1 (de) 2013-05-08 2014-11-12 Linde Aktiengesellschaft Luftzerlegungsanlage mit Hauptverdichterantrieb
EP2963369A1 (de) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
EP2963367A1 (de) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Tieftemperaturzerlegung von Luft mit variablem Energieverbrauch
EP2963370A1 (de) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Verfahren und vorrichtung zur tieftemperaturzerlegung von luft
EP2963371A1 (de) 2014-07-05 2016-01-06 Linde Aktiengesellschaft Verfahren und vorrichtung zur gewinnung eines druckgasprodukts durch tieftemperaturzerlegung von luft

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Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4072023A (en) * 1975-10-03 1978-02-07 Linde Aktiengesellschaft Air-rectification process and apparatus
US5220796A (en) * 1991-07-15 1993-06-22 The Boc Group, Inc. Adsorption condensation solvent recovery system
US5265429A (en) * 1992-02-21 1993-11-30 Praxair Technology, Inc. Cryogenic air separation system for producing gaseous oxygen
DE102007031765A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren zur Tieftemperaturzerlegung von Luft
DE102007031759A1 (de) 2007-07-07 2009-01-08 Linde Ag Verfahren und Vorrichtung zur Erzeugung von gasförmigem Druckprodukt durch Tieftemperaturzerlegung von Luft
EP2015013A2 (de) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von gasförmigem Druckprodukt durch Tieftemperaturzerlegung von Luft
EP2015012A2 (de) 2007-07-07 2009-01-14 Linde Aktiengesellschaft Verfahren zur Tieftemperaturzerlegung von Luft
DE102009034979A1 (de) 2009-04-28 2010-11-04 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von gasförmigem Drucksauerstoff
EP2312248A1 (de) 2009-10-07 2011-04-20 Linde Aktiengesellschaft Verfahren und Vorrichtung Gewinnung von Drucksauerstoff und Krypton/Xenon
EP2458311A1 (de) 2010-11-25 2012-05-30 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102010052544A1 (de) 2010-11-25 2012-05-31 Linde Ag Verfahren zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102010052545A1 (de) 2010-11-25 2012-05-31 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung eines gasförmigen Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2466236A1 (de) 2010-11-25 2012-06-20 Linde Aktiengesellschaft Verfahren zur Gewinnung eines gasförmigen Druckprodukts durch Tiefemperaturzerlegung von Luft
EP2520886A1 (de) 2011-05-05 2012-11-07 Linde AG Verfahren und Vorrichtung zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
EP2568242A1 (de) 2011-09-08 2013-03-13 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von Stahl
DE102011112909A1 (de) 2011-09-08 2013-03-14 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von Stahl
EP2600090A1 (de) 2011-12-01 2013-06-05 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von Drucksauerstoff durch Tieftemperaturzerlegung von Luft
DE102011121314A1 (de) 2011-12-16 2013-06-20 Linde Aktiengesellschaft Verfahren zur Erzeugung eines gasförmigen Sauerstoff-Druckprodukts durch Tieftemperaturzerlegung von Luft
DE102012017488A1 (de) 2012-09-04 2014-03-06 Linde Aktiengesellschaft Verfahren zur Erstellung einer Luftzerlegungsanlage, Luftzerlegungsanlage und zugehöriges Betriebsverfahren
EP2784420A1 (de) 2013-03-26 2014-10-01 Linde Aktiengesellschaft Verfahren zur Luftzerlegung und Luftzerlegungsanlage
WO2014154339A2 (de) 2013-03-26 2014-10-02 Linde Aktiengesellschaft Verfahren zur luftzerlegung und luftzerlegungsanlage
EP2801777A1 (de) 2013-05-08 2014-11-12 Linde Aktiengesellschaft Luftzerlegungsanlage mit Hauptverdichterantrieb
DE102013017590A1 (de) 2013-10-22 2014-01-02 Linde Aktiengesellschaft Verfahren zur Gewinnung eines Krypton und Xenon enthaltenden Fluids und hierfür eingerichtete Luftzerlegungsanlage
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Also Published As

Publication number Publication date
GB1023055A (en) 1966-03-16
DE1187248B (de) 1965-02-18
FR1426146A (fr) 1966-01-28
NL6407747A (de) 1966-01-10

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