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EP0019905A1 - Apparatus for the separation of a gas mixture by rectification - Google Patents

Apparatus for the separation of a gas mixture by rectification Download PDF

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Publication number
EP0019905A1
EP0019905A1 EP80102953A EP80102953A EP0019905A1 EP 0019905 A1 EP0019905 A1 EP 0019905A1 EP 80102953 A EP80102953 A EP 80102953A EP 80102953 A EP80102953 A EP 80102953A EP 0019905 A1 EP0019905 A1 EP 0019905A1
Authority
EP
European Patent Office
Prior art keywords
liquid
heat exchanger
sump
rectification
bath
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.)
Granted
Application number
EP80102953A
Other languages
German (de)
French (fr)
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EP0019905B1 (en
Inventor
Wilhelm Rohde
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
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Linde GmbH
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Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to AT80102953T priority Critical patent/ATE2178T1/en
Publication of EP0019905A1 publication Critical patent/EP0019905A1/en
Application granted granted Critical
Publication of EP0019905B1 publication Critical patent/EP0019905B1/en
Expired legal-status Critical Current

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Classifications

    • 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
    • F25J3/04406—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
    • F25J3/04866—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.
    • F25J3/04884—Arrangement of reboiler-condensers
    • 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
    • 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
    • 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
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • Y10S62/902—Apparatus
    • Y10S62/903—Heat exchange structure
    • 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
    • Y10S62/902—Apparatus
    • Y10S62/908—Filter or absorber

Definitions

  • the invention relates to a method and an apparatus for the separation of a gas mixture by rectification, wherein rectification liquid obtained in the sump of the rectification column is heated and partially evaporated, in which the rectification liquid is removed in the lower region of the liquid bath and fed back into the bath above the removal point.
  • German Patent 22 38 866 A method of this type has been described in German Patent 22 38 866.
  • a condenser-evaporator which is arranged in the sump of the rectification column and is partially covered by rectification liquid during operation of the column, the bottom liquid is heated and partly evaporated, with return liquid being generated on the condensation side of the evaporator-condenser for rectification.
  • return liquid being generated on the condensation side of the evaporator-condenser for rectification.
  • a disadvantage of this process is that the circulation is not carried out continuously.
  • the storage tank and the required switching valves mean additional equipment and increase the space requirement of the system.
  • the invention is therefore based on the object of developing a method of the type mentioned at the outset which enables continuous circulating operation and which can be carried out without considerable additional outlay.
  • the heat exchanger can be either the condenser evaporator which is present in any case during the rectification, or else one or more additional evaporators.
  • the heat exchanger which is arranged in such a way that it partially immerses in the sump liquid during operation of the rectification column, is closed on its side immersed in the liquid against the sump liquid. According to the invention, the removed part of the liquid is fed to the lower end of the heat exchanger and would theoretically rise to a height therein which corresponds to the liquid level of the sump liquid minus an amount corresponding to the pressure drop in the sampling pipes.
  • liquid is continuously removed from the lower region of the liquid bath and liquid is supplied to the liquid bath from above.
  • the continuous liquid circulation takes place without any special equipment. Total evaporation of the liquid in the heat exchanger should be avoided to prevent the heat exchanger surfaces from becoming encrusted.
  • At least some of the liquid removed is passed through an adsorber. Unwanted components are removed from the liquid in the adsorber.
  • gas bubbles are separated from the liquid before the liquid is fed to the heat exchanger. This measure increases the amount of liquid thrown over.
  • the method according to the invention is particularly suitable for the low-temperature separation of air. Since the circulation of the oxygen-rich liquid sump fraction formed during the air separation should not be carried out with the aid of a pump for safety reasons, the method according to the invention is particularly advantageous here. Gaseous air or gaseous nitrogen is advantageously used to evaporate the oxygen-rich liquid in the heat exchanger, the nitrogen being supplied under increased pressure to maintain the temperature difference required for the partial evaporation of the oxygen.
  • An apparatus for performing the method according to the invention comprises a rectification column, a heat exchanger arranged in the sump of the rectification column and a removal line, one end of which opens into the lower region of the rectification column and the other end of which is connected to the lower end of the heat exchanger.
  • a liquid level indicator connected in parallel with the heat exchanger is provided. This allows the liquid level in the heat exchanger to be checked from the outside and if necessary by throttling or S B of the circulated amount of liquid igerung change.
  • a further embodiment of the subject matter of the invention is particularly advantageous, in which a gas separator is connected to the extraction line opening into the heat exchanger.
  • the pipe runs in front of the connection point of the liquid level indicator in a vertical direction upwards and has a horizontal or downwardly inclined section between the connection point and the heat exchanger, while the gas separator is arranged essentially perpendicularly above the connection point. Gas bubbles contained in the liquid can rise freely into the gas separator.
  • Analog components have the same reference numbers in both figures.
  • 1 denotes a two-stage rectification column, as is used for the low-temperature separation of air.
  • the method according to the invention is also suitable for use in the rectification of another gas mixture.
  • a single-stage rectification column could just as well be used instead of the two-stage rectification column with a high-pressure stage 2 and a low-pressure stage 3 arranged above the high-pressure stage.
  • an oxygen-enriched liquid 4 collects during the air separation.
  • the head of the column 2 becomes a nitrogen-rich gaseous one Fraction removed (line 6) and fed to the condenser-evaporator 5, in which the gas is partially liquefied in the heat exchange with the oxygen-rich bottom liquid 4, with some of the bottom liquid 4 evaporating.
  • the condensed liquid is returned via line 7 to the high pressure stage 2.
  • the bottom liquid 4 still contains undesirable constituents, especially hydrocarbons such as acetylene
  • part of the liquid is circulated via an adsorber 8, in which these constituents are removed.
  • nitrogen is used, for example, which is supplied via line 9 and discharged via line 10.
  • the adsorber 8 is arranged at a lower level than the liquid bath 4.
  • a heat exchanger 11 which is arranged in the sump 4 of the rectification column and is partially immersed in the liquid bath during operation of the column, is used for liquid circulation.
  • the heat exchanger 11 for example a plate heat exchanger, is open at its upper end projecting over the liquid 4 to the inside of the low-pressure stage 3, its lower end immersed in the liquid is closed against the bottom liquid, for example with a header 12.
  • the heat exchanger is parallel to the Condenser-evaporator 5 connected to nitrogen lines 6, 7.
  • the heat exchanger can, as shown in the figure, be an additional evaporator, but it is also possible to form part of the heat exchange channels of the condenser-evaporator 5 in such a way that a direct connection between the heat exchange channels and the sump liquid is prevented.
  • a liquid extraction line 13 is provided, which is connected to the adsorber 8.
  • a flow meter 14 is arranged in the line 13.
  • the other end of the adsorber 8 is connected to a line 15 which opens into the header 12 of the heat exchanger 11.
  • liquid is removed from the column sump 4 via line 13, reaches the adsorber 8, where it is freed of hydrocarbons, and from there via line 15 into the header 12, from which it reaches the heat exchange channels of the heat exchanger 11.
  • the liquid rises in the heat exchanger 11 to a height which is equal to the liquid level of the bottom liquid 4 minus an amount which corresponds to the flow resistance in the liquid extraction line 13, 15 and in the adsorber 8.
  • Due to the warm nitrogen, the Line 6 is supplied, part of the liquid evaporates in the heat exchanger 11. Liquid is taken away by the withdrawing steam and thrown into the liquid bath via the upper edge of the heat exchanger 11. The evaporated amount of liquid is replaced by liquid flowing away from the rectification trays Bades by the fluid withdrawal had dropped again and the static liquid pressure in the pipeline 13 increased. The process therefore works continuously.
  • liquid is also thrown over in the evaporator condenser 5.
  • the liquid is through the connection that the evaporator-condenser 5 has on its underside with the liquid bath 4; added.
  • the liquid flows here via the pipes 13, 15 back into the heat exchanger until, according to the principle of the communicating tubes, a liquid level corresponding to the liquid level of the sump liquid 4 is reached. Since at the same time further liquid is evaporated from the heat exchanger and thrown over, the liquid level lags behind the state of equilibrium and a continuous liquid circuit is guaranteed.
  • the amount of liquid circulated through the adsorber 8 should correspond approximately to the amount of oxygen obtained during the rectification.
  • a bypass line 16 is provided parallel to the adsorber 8 and is provided with a control valve 17. With this bypass line 16, the level of the liquid level in the heat exchanger can also be influenced. A total evaporation of the liquid in the heat exchanger 11 must namely be avoided in order to prevent the heat exchanger surfaces from encrusting. There is also a risk of explosion if acetylene crystallizes out.
  • the heat exchanger should be filled to about 80% with liquid.
  • FIG. 2 shows essentially the same arrangement as FIG. 1.
  • a gas separator 18 is also provided here, which is connected in parallel to the heat exchanger 11.
  • the bypass line 16 and the line coming from the adsorber 15 run vertically upwards after their union below the connection point 19 of the gas separator 18, while the connecting piece 20 between the connection point 19 and the heat exchanger 11 runs horizontally at least over a short section.
  • the gas separator 18 is arranged vertically above the connection point 19. If gas bubbles are now contained in the liquid rising via the lines 15, 16, these rise from the connection point 19 into the gas separator 18 and are separated from the liquid which flows into the heat exchanger 11 via line 20.
  • the extraction line therefore does not have to be led exactly vertically upwards to the connection point 19 and the line 20 can, for example, have a section running downwards from the connection point 19.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

In the fractionation of a gaseous mixture, e.g., air, by rectification, wherein liquid in the sump of a rectifying column is heated and thereby partially vaporized; and simultaneously sump liquid is withdrawn from a lower zone of the sump liquid bath, and is recycled into the bath above the point of withdrawal, the improvement, prior to the recycle step, of passing the withdrawn sump liquid from the lower zone into a heat exchanger disposed in the sump, said heat exchanger having a substantially sealed bottom end at a level below the liquid level of the sump, and an open top end at a level higher than the liquid level of the sump; said withdrawn sump liquid being passed into the bottom end of said heat exchanger and partially vaporized therein, and removing resultant liquid-vapor mixture from the heat exchanger at the top end above the level of the liquid bath. This system provides pump-free circulation of the sump liquid and the use incorporates an on-line adsorber to remove deleterious impurities from the sump liquid, e.g., hydrocarbons from oxygen.

Description

Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Zerlegung eines Gasgemisches durch Rektifikation, wobei im Sumpf der Rektifiziersäule anfallende Rektifizierflüssigkeit erwärmt und dabei teilweise verdampft wird, bei dem die Rektifizierflüssigkeit im unteren Bereich des Flüssigkeitsbades entnommen und oberhalb der Entnahmestelle dem Bad wieder zugeführt wird.The invention relates to a method and an apparatus for the separation of a gas mixture by rectification, wherein rectification liquid obtained in the sump of the rectification column is heated and partially evaporated, in which the rectification liquid is removed in the lower region of the liquid bath and fed back into the bath above the removal point.

Ein Verfahren dieser Art ist in der deutschen Patentschrift 22 38 866 beschrieben worden. Durch einen Kondensator-Verdampfer,wder im Sumpf der Rektifiziersäule angeordnet und beim Betrieb der Säule teilweise von Rektifizierflüssigkeit bedeckt ist, wird die Sumpfflüssigkeit erwärmt und dabei teilweise verdampft, wobei auf der Kondensationsseite des Verdampfer-Kondensators Rücklaufflüssigkeit für die Rektifikation erzeugt wird. Bei der Rektifikation eines Gasgemisches erweist es sich oft erforderlich, die sich im Sumpf der Rektifiziersäule ansammelnde Flüssigkeit umzuwälzen, beispielsweise um auf diese Weise unerwünschte Bestandteile aus der Flüssigkeit zu entfernen. Da die Verwendung von Umwälzpumpen nicht nur apparativ und energetisch aufwendige sondern etwa bei der Luftzerlegung zum Umwälzen von flüssigem Sauerstoff wegen der Explosionsgefahr auch nicht ganz unproblematisch ist, wurde in der genannten Veröffentlichung vorgeschlagen, die Rektifizierflüssigkeit dadurch umzuwälzen, daß Flüssigkeit aus dem Sumpf der Säule durch die bestehende Druckdifferenz zwischen der Flüssigkeitsentnahmestelle und der Produktaustrittsleitung in einen über der Sumpfflüssigkeit angeordneten Speicherbehälter gefördert und von dort unter Ausnutzung des Gefälles in den Säutehsumpf zurückgeleitet wird. In einer ersten Schaltphase ist der Speicherbehälter mit der Produktleitung verbunden und es wird Flüssigkeit in den Behälter gefördert. In einer zweiten Schaltphase wird die Verbindung zur Produktleitung unterbrochen und die Flüssigkeit fließt aus dem Speicherbehälter in den Säulensumpf zurück. Mit der beschriebenen Anordnung kann somit Flüssigkeit ohne die Verwendung einer Pumpe umgewälzt werden.A method of this type has been described in German Patent 22 38 866. By means of a condenser-evaporator, which is arranged in the sump of the rectification column and is partially covered by rectification liquid during operation of the column, the bottom liquid is heated and partly evaporated, with return liquid being generated on the condensation side of the evaporator-condenser for rectification. When a gas mixture is rectified, it often proves necessary to circulate the liquid accumulating in the sump of the rectification column, for example in order to remove undesired constituents from the liquid in this way. Since the use of Circulation pumps are not only expensive in terms of equipment and energy, but are also not entirely unproblematic when it comes to air separation for circulating liquid oxygen because of the risk of explosion the liquid tapping point and the product outlet line are conveyed into a storage container arranged above the sump liquid and from there is returned to the sump by using the slope. In a first switching phase, the storage container is connected to the product line and liquid is conveyed into the container. In a second switching phase, the connection to the product line is interrupted and the liquid flows back from the storage tank into the column sump. With the arrangement described, liquid can thus be circulated without the use of a pump.

Nachteilig bei diesem Verfahren ist, daß das Umwälzen nicht kontinuierlich erfolgt. Außerdem bedeuten der Speicherbehälter sowie die erforderlichen Schaltventile einen zusätzlichen apparativen Aufwand und erhöhen den Platzbedarf der Anlage.A disadvantage of this process is that the circulation is not carried out continuously. In addition, the storage tank and the required switching valves mean additional equipment and increase the space requirement of the system.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art zu entwickeln, das einen kontinuierlichen Umwälzbetrieb ermöglicht und das ohne erheblichen Mehraufwand durchführbar ist.The invention is therefore based on the object of developing a method of the type mentioned at the outset which enables continuous circulating operation and which can be carried out without considerable additional outlay.

Diese Aufgabe wird erfindungsgemäß dadurch gelöst, daß die entnommene Rektifizierflüssigkeit, vor sie der im Sumpf befindlichen Rektifizierflüssigkeit wieder zugemischt wird, dem Wärmetauscher an seinem unteren Ende zugeführt und darin teilweise verdampft und das entstehende Flüssigkeits-Dampf-Gemisch oberhalb des Flüssigkeitsbades aus dem Wärmetauscher entnommen wird.This object is achieved in that the removed rectifying liquid, before it is mixed again with the rectifying liquid located in the sump, is fed to the heat exchanger at its lower end and partially evaporated therein, and the liquid-vapor produced Mixture above the liquid bath is removed from the heat exchanger.

Bei dem Wärmetauscher kann es sich sowohl um den bei der Rektifikation ohnehin vorhandenen Kondensator-Verdampfer oder aber um einen oder mehrere zusätzliche Verdampfer handeln. Der Wärmetauscher, der so angeordnet ist, daß er beim Betrieb der Rektifiziersäule teilweise in die Sumpfflüssigkeit eintaucht, ist an seiner in die Flüssigkeit eintauchenden Seite gegen die Sumpfflüssigkeit verschlossen. Der entnommene Teil der Flüssigkeit wird erfindungsgemäß dem unteren Ende des Wärmetauschers zugeführt und würde darin theoretisch bis zu einer Höhe ansteigen, die dem Flüssigkeitsspiegel der Sumpfflüssigkeit abzüglich eines dem Druckabfall in den Entnahmerohren entsprechenden Betrages entspricht. Dadurch, daß in dem Wärmetauscher ein Teil der Flüssigkeit verdampft wird, werden von der verdampfenden Flüssigkeit auch flüssige Anteile mitgerissen und über den oberen Rand des Wärmetauschers, der zum Innenraum der Rektifiziersäule hin offen ist, in die den Wärmetauscher umgebende Sumpfflüssigkeit überworfen.The heat exchanger can be either the condenser evaporator which is present in any case during the rectification, or else one or more additional evaporators. The heat exchanger, which is arranged in such a way that it partially immerses in the sump liquid during operation of the rectification column, is closed on its side immersed in the liquid against the sump liquid. According to the invention, the removed part of the liquid is fed to the lower end of the heat exchanger and would theoretically rise to a height therein which corresponds to the liquid level of the sump liquid minus an amount corresponding to the pressure drop in the sampling pipes. Because part of the liquid is evaporated in the heat exchanger, liquid parts are also carried away by the evaporating liquid and are thrown over the upper edge of the heat exchanger, which is open to the interior of the rectification column, into the sump liquid surrounding the heat exchanger.

Auf diese Weise wird beim erfindungsgemäßen Verfahren kontinuierlich Flüssigkeit vom unteren Bereich des Flüssigkeitsbades entnommen und dem Flüssigkeitsbad von oben Flüssigkeit zugeführt. Die kontinuierliche Flüssigkeitsumwälzung erfolgt dabei ohne besonderen apparativen Aufwand. Eine Totalverdampfung der Flüssigkeit im Wärmetauscher ist zu vermeiden, um ein Verkrusten der Wärmetauscherflächen zu verhindern.In this way, in the method according to the invention, liquid is continuously removed from the lower region of the liquid bath and liquid is supplied to the liquid bath from above. The continuous liquid circulation takes place without any special equipment. Total evaporation of the liquid in the heat exchanger should be avoided to prevent the heat exchanger surfaces from becoming encrusted.

In vorteilhafter Weiterbildung des erfindungsgemäßen Verfahrens wird mindestens ein Teil der entnommenen Flüssigkeit über einen Adsorber geleitet. In dem Adsorber werden unerwünschte Bestandteile aus der Flüssigkeit entfernt.In an advantageous development of the method according to the invention, at least some of the liquid removed is passed through an adsorber. Unwanted components are removed from the liquid in the adsorber.

Es ist zweckmäßig, wenn ein regelbarer Teil der entnommenen Flüssigkeit über einen Bypass am Adsorber vorbeigeführt wird. Die über den Adsorber geführte Flüssigkeitsmenge kann dadurch unabhängig von der umgewälzten Flüssigkeitsmenge eingestellt werden.It is expedient if a controllable part of the liquid removed is bypassed the adsorber. The amount of liquid passed through the adsorber can thus be set independently of the amount of liquid circulated.

Bei einer vorteilhaften Ausführungsform des Erfindungsgegenstandes werden vor der Zuführung der Flüssigkeit zum Wärmetauscher Gasblasen aus der Flüssigkeit abgetrennt. Mit dieser Maßnahme wird die Menge der überworfenen Flüssigkeit vergrößert.In an advantageous embodiment of the subject matter of the invention, gas bubbles are separated from the liquid before the liquid is fed to the heat exchanger. This measure increases the amount of liquid thrown over.

Das erfindungsgemäße Verfahren eignet sich besonders bei der Tieftemperaturzerlegung von Luft. Da die Umwälzung der bei der Luftzerlegung entstehenden sauerstoffreichen flüssigen Sumpffraktion aus Sicherheitsgründen nicht mit Hilfe einer Pumpe durchgeführt werden soll, ist das erfindungsgemäße Verfahren hierbei besonders vorteilhaft. Zum Verdampfen der sauerstoffreichen Flüssigkeit im Wärmetauscher wird mit Vorteil gasförmige Luft oder gasförmiger Stickstoff verwendet, wobei der Stickstoff zur Einhaltung der zur teilweisen Verdampfung des Sauerstoffs benötigten Temperaturdifferenz unter erhöhtem Druck zugeführt wird.The method according to the invention is particularly suitable for the low-temperature separation of air. Since the circulation of the oxygen-rich liquid sump fraction formed during the air separation should not be carried out with the aid of a pump for safety reasons, the method according to the invention is particularly advantageous here. Gaseous air or gaseous nitrogen is advantageously used to evaporate the oxygen-rich liquid in the heat exchanger, the nitrogen being supplied under increased pressure to maintain the temperature difference required for the partial evaporation of the oxygen.

Eine Vorrichtung zur Durchführung des erfindungsgemäßen Verfahrens umfaßt eine Rektifiziersäule, einen im Sumpf der Rektifiziersäule angeordneten Wärmetauscher sowie eine Entnahmeleitung, deren eines Ende in den unteren Bereich der Rektifiziersäule mündet und deren anderes Ende mit dem unteren Ende des Wärmetauschers verbunden ist.An apparatus for performing the method according to the invention comprises a rectification column, a heat exchanger arranged in the sump of the rectification column and a removal line, one end of which opens into the lower region of the rectification column and the other end of which is connected to the lower end of the heat exchanger.

Bei einer weiteren erfindungsgemäßen Ausführungsform ist ein dem Wärmetauscher parallel geschalteter Flüssigkeitsstandsanzeiger vorgesehen. Damit läßt sich der Flüssigkeitsstand im Wärmetauscher von außen kontrollieren und gegebenenfalls durch Drosselung oder SBigerung der umgewälzten Flüssigkeitsmenge verändern.In a further embodiment according to the invention, a liquid level indicator connected in parallel with the heat exchanger is provided. This allows the liquid level in the heat exchanger to be checked from the outside and if necessary by throttling or S B of the circulated amount of liquid igerung change.

Besonders vorteilhaft ist eine weitere Ausgestaltung des Erfindungsgegenstandes, bei der mit der in dem Wärmetauscher mündenden Entnahmeleitung ein Gasabscheider verbunden ist. Zu diesem Zweck verläuft die Rohrleitung vor der Anschlußstelle des Flüssigkeitsstandsanzeigers in vertikalter Richtung nach oben und weist zwischen Anschlußstelle und Wärmetauscher mindestens kurzzeitig einen waagerechten oder abwärts geneigten Abschnitt auf, während der Gasabscheider im wesentlichen lotrecht über der Anschlußstelle angeordnet ist. In der Flüssigkeit enthaltene Gasblasen können so unbehindert in den Gasabscheider aufsteigen.A further embodiment of the subject matter of the invention is particularly advantageous, in which a gas separator is connected to the extraction line opening into the heat exchanger. For this purpose, the pipe runs in front of the connection point of the liquid level indicator in a vertical direction upwards and has a horizontal or downwardly inclined section between the connection point and the heat exchanger, while the gas separator is arranged essentially perpendicularly above the connection point. Gas bubbles contained in the liquid can rise freely into the gas separator.

Weitere Einzelheiten der Erfindung werden anhand eines schematisch dargestellten Ausführungsbeispiels beschrieben.Further details of the invention are described with reference to a schematically illustrated embodiment.

Hierbei zeigen:

  • Figur 1 eine Rektifiziersäule zur Durchführung des erfindungsgemäßen Verfahrens
  • Figur 2 eine modifizierte Anordnung gemäß Figur 1
Here show:
  • Figure 1 shows a rectification column for performing the method according to the invention
  • FIG. 2 shows a modified arrangement according to FIG. 1

Analoge Bauteile tragen in beiden Figuren dieselben Bezugszeichen. Mit 1 ist.eine zweistufige Rektifiziersäule bezeichnet, wie sie zur Tieftemperaturzerlegung von Luft verwendet wird. Das erfindungsgemäße Verfahren eignet sich jedoch ebenso zur Anwendung bei der Rektifikation eines anderen Gasgemisches. Genausogut könnte statt der dargestellten zweistufigen Rektifiziersäule mit einer Hochdruckstufe 2 und einer oberhalb der Hochdruckstufe angeordneten Niederdruckstufe 3 eine einstufige Rektifiziersäule verwendet werden.Analog components have the same reference numbers in both figures. 1 denotes a two-stage rectification column, as is used for the low-temperature separation of air. However, the method according to the invention is also suitable for use in the rectification of another gas mixture. A single-stage rectification column could just as well be used instead of the two-stage rectification column with a high-pressure stage 2 and a low-pressure stage 3 arranged above the high-pressure stage.

Im Sumpf der Niederdrucksäule 3 sammelt sich während der Luftzerlegung eine mit Sauerstoff angereicherte Flüssigkeit 4. Ein Kondensator-Verdampfer 5, der in der Sumpfflüssigkeit angeordnet ist, erzeugt-Rücklaufflüssigkeit für die Hochdrucksäule 2. Zu diesem Zweck wird vom Kopf der Säule 2 eine stickstoffreiche gasförmige Fraktion entnommen (Leitung 6) und dem Kondensator-Verdampfer 5 zugeführt, in dem das Gas teilweise im Wärmetausch mit der sauerstoffreichen Sumpfflüssigkeit 4 verflüssigt wird, wobei ein-Teil der Sumpfflüssigkeit 4 verdampft. Die kondensierte Flüssigkeit wird über Leitung 7 in die Hochdruckstufe 2 zurückgeleitet.In the sump of the low-pressure column 3, an oxygen-enriched liquid 4 collects during the air separation. A condenser-evaporator 5, which is arranged in the sump liquid, produces return liquid for the high-pressure column 2. For this purpose, the head of the column 2 becomes a nitrogen-rich gaseous one Fraction removed (line 6) and fed to the condenser-evaporator 5, in which the gas is partially liquefied in the heat exchange with the oxygen-rich bottom liquid 4, with some of the bottom liquid 4 evaporating. The condensed liquid is returned via line 7 to the high pressure stage 2.

Da in der Sumpfflüssigkeit 4 noch unerwünschte Bestandteile, vor allem Kohlenwasserstoffe wie Acetylen, enthalten sind, wird ein Teil der Flüssigkeit über einen Adsorber 8 umgewälzt, in dem diese Bestandteile entfernt werden. Zum Regenerieren der Adsorber wird beispielsweise Stickstoff verwendet, der über Leitung 9 zu- und über Leitung 10 abgeführt wird. Der Adsorber 8 ist auf tieferem Niveau angeordnet als das Flüssigkeitsbad 4.Since the bottom liquid 4 still contains undesirable constituents, especially hydrocarbons such as acetylene, part of the liquid is circulated via an adsorber 8, in which these constituents are removed. To regenerate the adsorber, nitrogen is used, for example, which is supplied via line 9 and discharged via line 10. The adsorber 8 is arranged at a lower level than the liquid bath 4.

Erfindungsgemäß dient zur Flüssigkeitsumwälzung ein im Sumpf 4 der Rektifiziersäule angeordneter Wärmetauscher 11, der beim Betrieb der Säule teilweise in das Flüssigkeits- - bad eintaucht. Der Wärmetauscher 11, z.B. ein Plattenwärmetauscher, ist an seinem über die Flüssigkeit 4 ragenden oberen Ende zur Innenseite der Niederdruckstufe 3 hin offen, sein in die Flüssigkeit eintauchendes unteres Ende ist gegen die Sumpfflüssigkeit verschlossen, beispielsweise mit einem Header 12. Der Wärmetauscher ist parallel zum Kondensator-Verdampfer 5 an die Stickstoffleitungen 6, 7 angeschlossen. Der Wärmetauscher kann, wie in der Figur dargestellt, ein zusätzlicher Verdampfer sein, es ist aber auch möglich, einen Teil der Wärmetauschkanäle des Kondensator-Verdampfers 5 derart auszubilden, daß eine direkte Verbindung zwischen den Wärmetauschkanälen und der Sumpfflüssigkeit verhindert wird. Am unteren Ende der Niederdruckstufe 3 ist eine Flüssigkeitsentnahmeleitung 13 vorgesehen, die mit dem Adsorber 8 verbunden ist. In der Leitng 13 ist ein Strömungsmesser 14 angeordnet. Das andere Ende des Adsorbers 8 ist an eine Leitung 15 angeschlossen, die in den Header 12 des Wärmetauschers 11 mündet.According to the invention, a heat exchanger 11, which is arranged in the sump 4 of the rectification column and is partially immersed in the liquid bath during operation of the column, is used for liquid circulation. The heat exchanger 11, for example a plate heat exchanger, is open at its upper end projecting over the liquid 4 to the inside of the low-pressure stage 3, its lower end immersed in the liquid is closed against the bottom liquid, for example with a header 12. The heat exchanger is parallel to the Condenser-evaporator 5 connected to nitrogen lines 6, 7. The heat exchanger can, as shown in the figure, be an additional evaporator, but it is also possible to form part of the heat exchange channels of the condenser-evaporator 5 in such a way that a direct connection between the heat exchange channels and the sump liquid is prevented. At the lower end of the low-pressure stage 3, a liquid extraction line 13 is provided, which is connected to the adsorber 8. A flow meter 14 is arranged in the line 13. The other end of the adsorber 8 is connected to a line 15 which opens into the header 12 of the heat exchanger 11.

Bei"der Durchführung des erfindungsgemäßen Verfahrens wird über Leitung 13 Flüssigkeit aus dem Säulensumpf 4 entnommen, gelangt in den Adsorber 8, wo sie von Kohlenwasserstoffen befreit wird, und von dort über Leitung 15 in den Header 12, von dem sie auf die Wärmetauschkanäle des Wärmetauschers 11 verteilt wird. Die Flüssigkeit steigt im Wärmetauscher 11 bis in eine Höhe, die gleich ist dem Flüssigkeitspiegel der Sumpfflüssigkeit 4 abzüglich eines.Betrags, der dem Strömungswiderstand in der Flüssigkeitsentnahmeleitung 13, 15 und im Adsorber 8 entspricht. Durch den warmen Stickstoff, der über Leitung 6 zugeführt wird, verdampft ein Teil der Flüssigkeit im Wärmetauscher 11. Vom abziehenden Dampf wird Flüssigkeit mitgenommen und über den oberen Rand des Wärmetauschers 11 in das Flüssigkeitsbad übergeworfen. Die verdampfte Flüssigkeitsmenge wird durch von den Rektifizierböden abfließende Flüssigkeit ersetzt. Damit steigt der Flüssigkeitsspiegel des Bades, der durch die Flüssigkeitsentnahme abgesunken war, wieder an und der statische Flüssigkeitsdruck in der Rohrleitung 13 erhöht sich. Das Verfahren arbeitet somit kontinuierlich.When "carrying out the method according to the invention, liquid is removed from the column sump 4 via line 13, reaches the adsorber 8, where it is freed of hydrocarbons, and from there via line 15 into the header 12, from which it reaches the heat exchange channels of the heat exchanger 11. The liquid rises in the heat exchanger 11 to a height which is equal to the liquid level of the bottom liquid 4 minus an amount which corresponds to the flow resistance in the liquid extraction line 13, 15 and in the adsorber 8. Due to the warm nitrogen, the Line 6 is supplied, part of the liquid evaporates in the heat exchanger 11. Liquid is taken away by the withdrawing steam and thrown into the liquid bath via the upper edge of the heat exchanger 11. The evaporated amount of liquid is replaced by liquid flowing away from the rectification trays Bades by the fluid withdrawal had dropped again and the static liquid pressure in the pipeline 13 increased. The process therefore works continuously.

Es sei noch darauf hingewiesen, daß ein Überwerfen von Flüssigkeit auch im Verdampfer-Kondensator 5 erfolgt. Die Flüssigkeit wird über die Verbindung, die der Verdampfer-Kondensator 5 an seiner Unterseite mit dem Flüssigkeitsbad 4 besitzt; ergänzt. Dagegen ist beim Wärmetauscher 11 ein direktes Rückströmen von Flüssigkeit durch den Header 12 verhindert. Die Flüssigkeit strömt hier über die Rohrleitungen 13, 15 in den Wärmetauscher zurück, bis nach dem Prinzip der kommunizierenden Röhren ein dem Flüssigkeitsspiegel der Sumpfflüssigkeit 4 entsprechender Flüssigkeitsstand erreicht wird. Da gleichzeitig weitere Flüssigkeit aus dem Wärmetauscher verdampft und übergeworfen wird, hinkt der Flüssigkeitsspiegel dem Gleichgewichtszustand nach und es ist ein kontinuierlicher Flüssigkeitskreislauf gewährleistet. Es ist denkbar, den Verdampfer 11 - anstelle des einen gezeichneten können ebensogut auch mehrere Verdampfer vorgesehen sein - statt mit Stickstoff mit Luft zu beheizen.It should also be pointed out that liquid is also thrown over in the evaporator condenser 5. The liquid is through the connection that the evaporator-condenser 5 has on its underside with the liquid bath 4; added. In contrast, there is a direct backflow of liquid through the header 12 in the heat exchanger 11 prevented. The liquid flows here via the pipes 13, 15 back into the heat exchanger until, according to the principle of the communicating tubes, a liquid level corresponding to the liquid level of the sump liquid 4 is reached. Since at the same time further liquid is evaporated from the heat exchanger and thrown over, the liquid level lags behind the state of equilibrium and a continuous liquid circuit is guaranteed. It is conceivable to heat the evaporator 11 - instead of the one shown, it is also possible to provide a plurality of evaporators - instead of heating it with air using nitrogen.

Die über den Adsorber 8 umgewälzte Flüssigkeitsmenge sollte etwa der Menge des bei der Rektifikation gewonnenen Sauerstoffs entsprechen. Um die Flüssigkeitsmenge unabhängig - von der umgewälzten Menge regeln zu können, ist parallel zum Adsorber 8 eine Bypassleitung 16 vorgesehen, die mit einem Regelventil 17 versehen ist. Mit dieser Bypassleitung 16 kann zugleich die Höhe des-Flüssigkeitsstandes im Wärmetauscher beeinflußt werden. Eine Totalverdampfung der Flüssigkeit im Wärmetauscher 11 muß nämlich vermieden werden, um eine Verkrustung der Wärmetauscherflächen zu verhindern. Außerdem besteht bei Auskristallisieren von Acetylen Explosionsgefahr. Der Wärmetauscher soll etwa zu 80 % mit Flüssigkeit gefüllt sein.The amount of liquid circulated through the adsorber 8 should correspond approximately to the amount of oxygen obtained during the rectification. In order to be able to regulate the amount of liquid independently of the circulated amount, a bypass line 16 is provided parallel to the adsorber 8 and is provided with a control valve 17. With this bypass line 16, the level of the liquid level in the heat exchanger can also be influenced. A total evaporation of the liquid in the heat exchanger 11 must namely be avoided in order to prevent the heat exchanger surfaces from encrusting. There is also a risk of explosion if acetylene crystallizes out. The heat exchanger should be filled to about 80% with liquid.

Figur 2 zeigt im wesentlichen dieselbe Anordnung wie Figur 1. Zusätzlich ist hier noch ein Gasabscheider 18 vorgesehen, der parallel zum Wärmetauscher 11 geschaltet ist. Mit Hilfe von Flüssigkeitsstandsanzeigern 21, 22 läßt sich die Höhe des Flüssigkeitsstandes im Säulensumpf und im Wärmetauscher 11 von außen leicht kontrollieren und somit stets die optimale Flüssigkeitshöhe einregulieren.FIG. 2 shows essentially the same arrangement as FIG. 1. In addition, a gas separator 18 is also provided here, which is connected in parallel to the heat exchanger 11. With the help of liquid level indicators 21, 22, the height of the liquid level in the column sump and in the heat exchanger 11 can be easily checked from the outside and thus always regulate the optimal liquid level.

Die Bypassleitung 16 und die vom Adsorber kommende Leitung 15 verlaufen nach ihrer Vereinigung unterhalb der Anschlußstelle 19 des Gasabscheiders 18 vertikal nach oben, während das Verbindungstück 20 zwischen der Anschlußstelle 19 und dem Wärmetauscher 11 zumindest auf einem kurzen Abschnitt waagrecht verläuft. Der Gasabscheider 18 ist lotrecht über der Anschlußstelle 19 angeordnet. Falls nun in der über die Leitungen 15, 16 aufsteigenden Flüssigkeit Gasblasen enthalten sind, so steigen diese von der Anschlußstelle 19 in den Gasabscheider 18 nach oben und werden von der Flüssigkeit abgetrennt, die über Leitung 20 in den Wärmetauscher 11 strömt. Selbstverständlich läßt sich die beschriebene und gezeigte Anordnung abändern, ohne das Prinzip der Gasabscheidung abzuändern. Die Entnahmeleitung muß demnach nicht genau vertikal zur Anschlußstelle 19 nach oben geführt sein und die Leitung 20 kann zum Beispiel einen von der Anschlußstelle 19 nach abwärts verlaufenden Abschnitt aufweisen.The bypass line 16 and the line coming from the adsorber 15 run vertically upwards after their union below the connection point 19 of the gas separator 18, while the connecting piece 20 between the connection point 19 and the heat exchanger 11 runs horizontally at least over a short section. The gas separator 18 is arranged vertically above the connection point 19. If gas bubbles are now contained in the liquid rising via the lines 15, 16, these rise from the connection point 19 into the gas separator 18 and are separated from the liquid which flows into the heat exchanger 11 via line 20. Of course, the arrangement described and shown can be changed without changing the principle of gas separation. The extraction line therefore does not have to be led exactly vertically upwards to the connection point 19 and the line 20 can, for example, have a section running downwards from the connection point 19.

Claims (8)

1. Verfahren zur Zerlegung eines Gasgemisches durch Rektifikation, wobei im Sumpf der Rektifiziersäule anfallende Rektifizierflüssigkeit erwärmt und dabei teilweise verdampft wird, bei dem die Rektifizierflüssigkeit im unteren Bereich des Flüssigkeitsbades entnommen und oberhalb der Entnahmestelle dem Bad wieder zugeführt wird, dadurch gekennzeichnet, daß die entnommene Rektifizierflüssigkeit bevor sie der im Sumpf befindlichen Rektifizierflüssigkeit (4) wieder zugemischt wird, dem Wärmetauscher (11) an seinem unteren Ende zugeführt und darin teilweise verdampft und das entstehende Flüssigkeits-Dampf-Gemisch oberhalb des Flüssigkeitsbades (4) aus dem Wärmetauscher (11) entnommen wird.1. Process for the decomposition of a gas mixture by rectification, the rectifying liquid obtained in the sump of the rectifying column being heated and partially evaporated, in which the rectifying liquid is removed from the lower region of the liquid bath and fed back into the bath above the removal point, characterized in that the removed Rectifying liquid before it is mixed again with the rectifying liquid (4) in the sump, fed to the heat exchanger (11) at its lower end and partially evaporated therein and the liquid-steam mixture formed above the liquid bath (4) is removed from the heat exchanger (11) becomes. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß mindestens ein Teil der entnommenen Flüssigkeit über einen Adsorber (8) geleitet wird.2. The method according to claim 1, characterized in that at least part of the liquid withdrawn is passed through an adsorber (8). 3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß ein regelbarer Teil der entnommenen Flüssigkeit über einen Bypass (16) am'Adsorber (8) vorbeigeführt wird.3. The method according to claim 1 or 2, characterized in that a controllable part of the liquid withdrawn via a bypass (16) past the adsorber (8). 4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß vor der Zuführung der Flüssigkeit zum Wärmetauscher (11) Gasblasen aus der Flüssigkeit abgetrennt werden.4. The method according to any one of claims 1 to 3, characterized in that gas bubbles are separated from the liquid before the supply of the liquid to the heat exchanger (11). 5. Anwendung des Verfahrens nach einem der Ansprüche 1 bis 4 bei der Tieftemperaturzerlegung von Luft.5. Application of the method according to one of claims 1 to 4 in the low-temperature separation of air. 6. Vorrichtung zur Durchführung des Verfahrens nach einem der Ansprüche 1 bis 4 mit einer Rektifiziersäule, einem im Sumpf der Rektifiziersäule angeordneten Wärmetauscher, sowie einer Entnahmeleitung, deren eines Ende in den unteren Bereich der Rektifiziersäule mündet, dadurch gekennzeichnet, daß das andere Ende (20) der Entnahmeleitung mit dem unteren Ende des Wärmetauschers (11) verbunden ist.6. Apparatus for carrying out the method according to one of claims 1 to 4 with a rectification column, a heat exchanger arranged in the sump of the rectification column, and a removal line, one end of which opens into the lower region of the rectification column, characterized in that the other end (20 ) the sampling line is connected to the lower end of the heat exchanger (11). 7. Vorrichtung nach Anspruch 6, dadurch gekennzeichnet, daß parallel zu dem Wärmetauscher (11) ein Flüssigkeitsstandsanzeiger (22) angeordnet ist.7. The device according to claim 6, characterized in that a liquid level indicator (22) is arranged parallel to the heat exchanger (11). 8. Vorrichtung nach Anspruch 6 oder 7, dadurch gekennzeichnet, daß mit der in den Wärmetauscher (11) mündenden Entnahmeleitung (20) ein Gasabscheider (18) verbunden ist.8. Apparatus according to claim 6 or 7, characterized in that a gas separator (18) is connected to the discharge line (20) opening into the heat exchanger (11).
EP80102953A 1979-05-30 1980-05-27 Apparatus for the separation of a gas mixture by rectification Expired EP0019905B1 (en)

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US4337070A (en) 1982-06-29
DE3061536D1 (en) 1983-02-10
ATE2178T1 (en) 1983-01-15
EP0019905B1 (en) 1983-01-05
AU5864580A (en) 1980-12-04
DE2922028A1 (en) 1980-12-11

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