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DE1039079B - Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process - Google Patents

Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process

Info

Publication number
DE1039079B
DE1039079B DEG21772A DEG0021772A DE1039079B DE 1039079 B DE1039079 B DE 1039079B DE G21772 A DEG21772 A DE G21772A DE G0021772 A DEG0021772 A DE G0021772A DE 1039079 B DE1039079 B DE 1039079B
Authority
DE
Germany
Prior art keywords
oxygen
liquid
rectification
column
evaporator
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.)
Pending
Application number
DEG21772A
Other languages
German (de)
Inventor
Dr-Ing Ernst Karwat
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
Original Assignee
Gesellschaft fuer Lindes Eismaschinen AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to DEG21735A priority Critical patent/DE1033689B/en
Application filed by Gesellschaft fuer Lindes Eismaschinen AG filed Critical Gesellschaft fuer Lindes Eismaschinen AG
Priority to DEG21772A priority patent/DE1039079B/en
Priority to US721492A priority patent/US2975606A/en
Priority to GB8972/58A priority patent/GB851619A/en
Publication of DE1039079B publication Critical patent/DE1039079B/en
Pending legal-status Critical Current

Links

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
    • F25J3/04866—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.
    • F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
    • F25J3/0409—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • 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
    • F25J3/044—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 single pressure main column system only
    • 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
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • 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
    • F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Description

In der Patentanmeldung G 21735 Ia/17g ist ein Verfahren beschrieben zum Eindampfen von durch Rektifikation mk köhlenwasserstoffverunreinigter Luft in einer Rektifikationssäule gewonnenem, kohlenwasserstoffhaltigem, flüssigem Sauerstoff in einem aus einem Bündel parallel geschalteter Rohre bestehenden Verdampfer durch Wärmetausch mit einem außen an dem Rohrbündel kondensierenden Gas, welches dadurch gekennzeichnet ist, daß dem Verdampfer mehr flüssiger Sauerstoff zugeführt als darin verdampft wird und der entstehende gasförmige Sauerstoff im Gleichstrom mit der verdampfenden Flüssigkeit von oben nach unten oder umgekehrt strömt und der nicht verdampfte Teil in das Bad von flüssigem Sauerstoff an den Fuß der Rektifikationssäule zurückgeführt wird.In the patent application G 21735 Ia / 17g is a Process described for the evaporation of air contaminated with hydrocarbons by rectification Hydrocarbon-containing liquid oxygen obtained in a rectification column in one consisting of a bundle of tubes connected in parallel by exchanging heat with an evaporator outside of the tube bundle condensing gas, which is characterized in that the evaporator more liquid oxygen is supplied than is evaporated in it and the resulting gaseous oxygen flows in cocurrent with the evaporating liquid from top to bottom or vice versa and the unevaporated part is returned to the bath of liquid oxygen at the base of the rectification column will.

Gegenstand der Erfindung ist eine besonders zweckmäßige Ausführungsform des Verfahrens nach Anspruch 1 bis 3 der Hauptpatentanmeldung. Sie ist dadurch gekennzeichnet, daß im Gleichstromverdampfer so viel flüssiger Sauerstoff verdampft wird, daß zusammen mit der zu erzeugenden, zum Wärmeaustauscher abgeführten auch die zur Rektifikation erforderliche Menge Sauerstoffgas entsteht, die zur Rektifiziersäule zurückgeführt wird.The invention relates to a particularly useful embodiment of the method according to Claims 1 to 3 of the main patent application. It is characterized in that in the direct current evaporator so much liquid oxygen is evaporated that together with the to be generated, to The amount of oxygen gas required for rectification is also produced by the heat exchanger, which is returned to the rectification column.

Nach einer weiteren Ausbildung des Erfindungsgedankens werden Flüssigkeit und Dampf des Verdampfungskreislaufs mit Adsorptionsmitteln von den Kohlenwasserstoffen befreit.According to a further development of the inventive concept, the liquid and vapor of the evaporation circuit become freed from the hydrocarbons with adsorbents.

Es ist zwar bekannt, in Luftzerlegungsapparaten zweistufiger Rektifikation, um an Bauhöhe zu sparen, die Drucksäule und die Niederdrucksäule nebeneinander (nicht wie üblich übereinander) zu bauen und den flüssigen Sauerstoff mit einer Pumpe vom Fuß der Niederdrucksäule auf den über der Drucksäule angeordneten Kondensatorverdampfer zu pumpen. Dabei war der Kondensatorverdampfer ebenfalls als Bündel parallel geschalteter Röhren ausgeführt, innerhalb deren der flüssige Sauerstoff durch an der Außenseite des Röhrenbündels kondensierenden Druckstickstoff verdampft wurde. Dabei wurde ferner dem oberen Ende des Rohrbündels mit der Pumpe ein größeres Gewicht flüssigen Sauerstoffs zugeführt, als Sauerstoff dämpfe erzeugt werden sollten; der Überschuß an flüssigem Sauerstoff wurde vom unteren Ende des Rohrbündels in das Bad flüssigen Sauerstoffs an den Fuß der Niederdrucksäule zurückgeführt. Although it is known to use two-stage rectification in air separation apparatus in order to save on structural height, to build the pressure column and the low pressure column next to each other (not on top of each other as usual) and the liquid oxygen with a pump from the foot of the low pressure column to the one above the pressure column arranged to pump condenser evaporator. The condenser evaporator was also used as Bundles of tubes connected in parallel, within which the liquid oxygen passes through to the Outside of the tube bundle condensing pressurized nitrogen was evaporated. It was also the A greater weight of liquid oxygen is supplied to the upper end of the tube bundle with the pump than Oxygen vapors should be generated; the excess of liquid oxygen was transferred from the lower end of the tube bundle into the liquid oxygen bath returned to the foot of the low pressure column.

Bei diesem bekannten Verfahren durchströmte jedoch — im Gegensatz zur Erfindung — der flüssige Sauerstoff das Rohrbündel von oben nach unten, während die erzeugten Dämpfe im Gegenstrom zur verdampfenden Flüssigkeit nach oben abzogen.In this known method, however - in contrast to the invention - the liquid flowed through Oxygen flows down the tube bundle from top to bottom, while the vapors generated go in countercurrent to the evaporating Liquid drawn off upwards.

Hierin liegt ein schwerer Nachteil des bekanntenThis is a serious disadvantage of the known

Verfahren zum Eindampfen
kohlenwasserstoffhaltigen, flüssigenProcess for evaporation
hydrocarbon-containing, liquid

Sauerstoffs und Einrichtung
zur Durchführung des VerfahrensOxygen and facility
to carry out the procedure

Zusatz zur Patentanmeldung G 21735 Ia/17 g
(Auslegeschrift 1 033 689)Addition to patent application G 21735 Ia / 17 g
(Interpretation document 1 033 689)

Anmelder:Applicant:

Gesellschaft für Linde's EismaschinenSociety for Linde's ice machines

Aktiengesellschaft,
Höllriegelskreuth bei MünchenCorporation,
Höllriegelskreuth near Munich

Dr.-Ing. Ernst Karwat, Pullach bei München,
ist als Erfinder genannt wordenDr.-Ing. Ernst Karwat, Pullach near Munich,
has been named as the inventor

Verfahrens für die Sicherheit des Lufttrenners. Unvermeidbare Beimengungen von Kohlenwasserstoffen in der Luft sammeln sich — auch wenn Vorreinigungsschritte gemacht werden — im Bad des flüssigen Sauerstoffs der Niederdrucksäule. Im Beharrungszustand müssen alle in die Niederdrucksäule eintretenden Kohlenwasserstoffe aus dem Trenner mit dem produzierten, gasförmigen Sauerstoff abgeführt werden, also mit dem Sauerstoff zusammen verdampft werden (Acetylenbilanz).Procedure for the safety of the air separator. Unavoidable admixtures of hydrocarbons in the air collect - even if precleaning steps are made - in the bath of the liquid Oxygen of the low pressure column. In the steady state, all entering the low-pressure column must Hydrocarbons are removed from the separator with the produced, gaseous oxygen be evaporated together with the oxygen (acetylene balance).

Die Verdampfung eines Kohlenwasserstoffs aus seiner Lösung im flüssigen Sauerstoff unterliegt dem Gesetz, daß das Verhältnis seiner Konzentration in der Flüssigkeit zu seiner Konzentration in der Gasphase eine für ihn charakteristische, konstante Zahl ist. Sie beträgt nach Messungen, z. B. für Acetylen, bei 90° K etwa 28. Dort, wo der produzierte, gasförmige Sauerstoff in der bekannten Vorrichtung das Rohrbüridel an dessen oberem Ende mit seinem durch die Acetylenbilanz geforderten Acetylengehalt verläßt, muß der auf das Bündel aufgegebene flüssige Sauerstoff also 28mal höhere Acetylenkonzentraition aufweisen als das Gas, sonst wäre die Bilanzforderung nicht erfüllbar. Im Abwärtssinken durch das Rohrbündel wird die Menge der Flüssigkeit kleiner. Ihr Gehalt am Acetylen steigt an und was bei der bekannten Arbeitsweise vom unteren Ende des Verdampferrohrbündels in die Niederdrucksäule zurückläuft, ist eine mk Acetylen stark angereicherte Flüssigkeit.The evaporation of a hydrocarbon from its solution in liquid oxygen is subject to this Law that the ratio of its concentration in the liquid to its concentration in the gas phase is a constant number characteristic of him. According to measurements, e.g. B. for acetylene, at 90 ° K about 28. Where the gaseous oxygen produced in the known device is the Leaves Rohrbüridel at its upper end with its acetylene content required by the acetylene balance, the liquid oxygen applied to the bundle must therefore have 28 times higher acetylene concentration than the gas, otherwise the balance sheet claim would not be achievable. Sinking down through the tube bundle the amount of liquid becomes smaller. Their acetylene content increases and what with the known Working method runs back from the lower end of the evaporator tube bundle into the low-pressure column, is a highly enriched mk acetylene liquid.

309 638/105309 638/105

Das Verfahren der vorliegenden Erfindung vermeidet diesen Nachteil. Indem es erstens die Gegenstromführung von Flüssigkeit und Dampf beim Eindampfen des kohlenwasserstoffhaltigen Sauerstoffs durch die Gleichstromführung ersetzt, braucht nunmehr nur der unverdampft gebliebene Teil der Flüssigkeit diejenige Konzentration an Kohlenwasserstoffen anzunehmen, die' dem Gleichgewicht mit dem Kohlen wasserstoff gehalt des abziehenden gasförmigen Sauerstoffs entspricht, also nicht melhr die ganze umlaufende Flüssigkeit wie bei dem bekannten Verfahren. Zweitens wird der rückgeführte unverdampfte Teil der Flüssigkeit durch Adsorption von seinem Gehalt an Kohlenwasserstoffen befreit, ehe er in die Niederdrucksäule zurückkehrt. Das gleiche gilt für den rückgeführten Teil des Gases. Infolgedessen verkehren in der Niederdrucksäule viel weniger Kohlenwasserstoffe. Da ferner ein großer Teil der Kohlenwasserstoffe mit den Adsorbern aus dem Kreislauf entnommen wird, braucht zur Aufrechterhaltung der Kohlenwasserstoffbilanz mit dem produzierten Sauerstoff nur mehr eine viel kleinere Menge Kohlenwasserstoffe abtransportiert zu werden.The method of the present invention avoids this disadvantage. First by doing the countercurrent flow of liquid and vapor during evaporation of the hydrocarbon-containing oxygen Replaced by direct current flow, only the part of the which has not been evaporated now needs To assume that concentration of hydrocarbons which is in equilibrium with the liquid Hydrogen content corresponds to the extracting gaseous oxygen, so not the whole circulating Liquid as in the known method. Second, the recycled unevaporated Part of the liquid is freed from its hydrocarbon content by adsorption before it enters the Low pressure column returns. The same applies to the recirculated part of the gas. As a result, run much fewer hydrocarbons in the low pressure column. There is also a large part of the hydrocarbons is removed from the circuit with the adsorbers, needs to maintain the Hydrocarbon balance with the produced oxygen only a much smaller amount of hydrocarbons to be transported away.

Die erfindungsgemäße Arbeitsweise bietet also einen viel höheren Grad von Sicherheit gegen Explosionen von Kohlenwasserstoffen im flüssigen Sauerstoff und ist in der Lage, wesentlich größere Mengen an Kohlenwasserstoffen im der verarbeiteten Luft gefahrlos zu verarbeiten.The method of operation according to the invention thus offers a much higher degree of security against Explosions of hydrocarbons in liquid oxygen and is capable of much larger ones Safe to process amounts of hydrocarbons in the processed air.

Wird die Arbeitsweise gemäß der Erfindung auf eine Einsäulenrektifikation angewendet, so befindet sich der Gleichstromverdampfer außerhalb und getrennt von der Rektifiziersäule, wie in Fig. 2 der Hauptpatentanmeldung dargestellt, wobei die Verdampferschlange im am Fuß der Säule befindlichen Bad entfällt. Der zur Beaufschlagung der Rektifiziersäule nötige gasförmige Sauerstoff geht von der vom Gleichstromverdampfer abgehenden Leitung für den erzeugten, gasförmigen Sauerstoff über die Abzweigleitung mit dem Ventil unter die Böden der Säule. Für den Fall, daß er relativ große Mengen von Kohlenwasserstoffen mit sich führen muß, wird er vor Rückkehr in die Säule mit einem Adsorptionsmittel gereinigt.If the method of operation according to the invention is applied to a one-column rectification, so is The direct current evaporator is outside and separate from the rectification column, as in Fig. 2 of the Main patent application shown, with the evaporator coil located at the foot of the column No bathroom. The gaseous oxygen required to act on the rectification column comes from the Direct current evaporator outgoing line for the generated, gaseous oxygen via the branch line with the valve under the bottoms of the column. In the event that he has relatively large amounts of Must carry hydrocarbons with it, it is before returning to the column with an adsorbent cleaned.

Bei einer Zweisäulenrektifikation zur Luftzerlegung ist die erfindungsgemäße Arbeitsweise immer dann anwendbar, wenn das am Fuß der Niederdrucksäule befindliche Bad von flüssigem Sauerstoff aus baulichen Gründen getrennt ist von dem zur Bildung von Waschflüssigkeit für die Vorrektifikationsdrucksäule vorgesehenen Druckstickstoffkondens-ator, in welchem gasförmiger Druckstickstoff durch Verdampfen flüssigen, aus der Niederdrucksäule entnommenen Sauerstoffs kondensiert wird. Das ist z. B. der Fall, wenn l)eide Säulen nebeneinander stehen.In the case of a two-column rectification for air separation, the method of operation according to the invention is always then applicable when the bath of liquid oxygen at the foot of the low pressure column is structural Reasons is separate from that for the formation of washing liquid for the pre-rectification pressure column provided pressurized nitrogen condenser, in which gaseous pressurized nitrogen evaporates liquid, is condensed oxygen removed from the low pressure column. This is e.g. B. the case if l) both pillars stand side by side.

An Hand der Fig. 1 und 2 wird je ein Verfahrensl«ispiel hierfür beschrieben.A procedural game is shown on the basis of FIGS. 1 and 2 described for this.

Das Beispiel nach Fig. 1 bezieht sich auf einen Gleichstroinverdampfer, in dem Flüssigkeit und Dämpfe gemeinsam von unten nach oben steigen, das Beispiel nach Fig. 2 auf einen solchen mit Fallgleichstromverdampfung. The example according to FIG. 1 relates to a co-flow evaporator in which liquid and Vapors rise together from bottom to top, the example according to FIG. 2 to one with falling cocurrent evaporation.

In Fig. 1 tritt im nicht gezeichneten Wärmeaustauscher vorgekühlte Druckluft bei 0 in die Druckrektifiziersäule 1 ein; die hier erzeugte sauerstoffreiche Flüssigkeit geht über Ventil 2 und Silicagel-Adsorber 3 bei 4 in die Niederdrucksäule 5. Bei 6 der Drucksäule entnommener, flüssiger Stickstoff beaufschlagt hinter Ventil 7 den Kopf der Niederdruckrektifiziersäule 5. Der in der Niederdrucksäule durch Rektifikation gebildete flüssige kohlenwasserstoffhaltige Sauerstoff wird am Fuß der Niederdrucksäule bei 8 entnommen und von der Pumpe 9 dem auf den Kopf der Drucksäule 1 gesetzten Verdampfer 10 unten zugeführt, strömt im Rohrbündel 11 nach oben und wird währenddessen durch Kondensieren von im Oberteil 12 der Drucksäule 1 strömenden Stickstoff zum Teil verdampft. Der verdampfte Sauerstoff verläßt den über dem Gleichstromverdampfer 1 angeordneten Abscheideraum 17 bei 13 und teilt sich bei 14 in zwei Ströme. Die der Produktion gleiche Sauerstoff menge geht in Richtung 15 zum nicht gezeichneten Wärmeaustauscher. Die zur Beaufschlagung der Niederdrucksäule nötige Sauerstoffmenge, ungefahr das Vierfache der Produktionsmenge, geht bei 16 über dem Bad flüssigen Sauerstoffs in die Niederdrucksäule 5; sie kann von Kohlenwasserstoffen in einem nicht gezeichneten Adsorber gereinigt werden. Von der Pumpe 9 wird mehr flüssiger Sauerstoff inIn Fig. 1 precooled compressed air enters the pressure rectification column at 0 in the heat exchanger (not shown) 1 a; the oxygen-rich liquid produced here passes through valve 2 and silica gel adsorber 3 at 4 in the low-pressure column 5. At 6, liquid nitrogen removed from the pressure column is applied behind valve 7 the head of the low-pressure rectification column 5. The one in the low-pressure column Rectification formed liquid hydrocarbonaceous Oxygen is taken from the foot of the low pressure column at 8 and from the pump 9 to the Head of the pressure column 1 set evaporator 10 is supplied below, flows in the tube bundle 11 upwards and is meanwhile by condensing nitrogen flowing in the upper part 12 of the pressure column 1 partly evaporated. The evaporated oxygen leaves the one arranged above the direct current evaporator 1 Separation space 17 at 13 and divides at 14 into two streams. The same as in production Oxygen amount goes in the direction of 15 to the not shown Heat exchanger. The amount of oxygen required to act on the low pressure column, approx four times the production amount, goes at 16 above the bath of liquid oxygen in the low pressure column 5; it can be from hydrocarbons in be cleaned with an adsorber not shown. From the pump 9 more liquid oxygen is in

ao den Verdampfer 10 von unten eingeführt als verdampft wird. Der Überschuß an flüssigem Sauerstoff, angereichert mit Kohlenwasserstoffen, trennt sich im Abscheideraum 17 vom gasförmigen Sauerstoff, läuft über Ventil 18 und, im Silicagel-Adsorber 19 gereinigt, zurück in die Saugleitung der Pumpe 9. Bei Ventil 20 ist ein Auslaß ins Freie vorgesehen, durch den notfalls eine kleine Menge verunreinigter Flüssigkeit abgelassen werden kann.ao the evaporator 10 is introduced from below when it is evaporated. The excess of liquid oxygen, enriched with hydrocarbons, separates from gaseous oxygen in separation space 17, runs via valve 18 and, cleaned in the silica gel adsorber 19, back into the suction line of the pump 9 Valve 20 is provided with an outlet to the open air through which a small amount of contaminated liquid can be removed if necessary can be drained.

In Fig. 2 ist ein Gleicbstromverdampfer gezeigt, welcher von dem zu verdampfenden Sauerstoff zusammen mit den entstehenden Dämpfen von oben nach unten durchströmt wird. In der Zeichnung bezeichnen gleiche Zahlen die gleichen Teile und Funktionen der Apparatur wie in Fig. 1. Es wird daher davon abgesehen, ihre Bedeutung nochmals zu beschreiben.In Fig. 2, a co-flow evaporator is shown, which is composed of the oxygen to be evaporated is flowed through with the resulting vapors from top to bottom. Mark in the drawing the same numbers the same parts and functions of the apparatus as in Fig. 1. It is therefore refrained from to describe their meaning again.

Abweichend von dem in Fig. 1 geschilderten Verfahren wird hier der bei 8 aus der Niederdrucksäule entnommene, flüssige Sauerstoff mit der Pumpe 9 bei 25 auf das obere Ende des Gleichstromverdampfers geführt, in welchem flüssiger Sauerstoff und der entstehende Dampf nach unten zum Abscheider 26 gehen, von wo aus die gebildeten Dämpfe in die Rohrleitung 27 zur Verteilungsstelle 28 gehen.Deviating from the method outlined in FIG. 1, that at 8 is here from the low-pressure column withdrawn, liquid oxygen with the pump 9 at 25 on the upper end of the direct current evaporator out, in which liquid oxygen and the resulting vapor go down to the separator 26, from where the vapors formed go into the pipeline 27 to the distribution point 28.

Die der Produktion entsprechende Sauer stoff menge geht in Richtung 29 zum Wärmeaustauscher, während die zur Beaufschlagung der Rektifikationssäule erforderliche Sauerstoffmenge — gegebenenfalls im Adsorber 30 gereinigt — bei 31 unter die Böden der Niederdrucksäule tritt.The amount of oxygen corresponding to the production goes in the direction of 29 to the heat exchanger, while the amount of oxygen required to act on the rectification column - if necessary in Adsorber 30 cleaned - enters at 31 under the bottoms of the low pressure column.

Die im Abscheider 26 angefallene Flüssigkeit wird bei 32 entnommen, über die Ventile 37 und 36 und über den Adsorber 34 bei 35 in das Bad von flüssigem Sauerstoff am Fuße der Niederdrucksäule zurückgeführt. 33 l>ezeichnet das Auslaßventil für die Entnähme kleiner Flüssigkeitsmengen zum Zwecke der Verminderung der im System befindlichen Mengen Kohlenwasserstoffe. Zur Desorption des Adsorbers 34 sind in an sich bekannter Weise die Ventile 36, 37, 39, 40 und 41 vorgesehen.The liquid that has accumulated in the separator 26 is withdrawn at 32, via the valves 37 and 36 and returned via adsorber 34 at 35 into the bath of liquid oxygen at the foot of the low-pressure column. 33 l> e indicates the outlet valve for the withdrawal of small amounts of liquid for the purpose of Reduction of the amount of hydrocarbons in the system. For desorption of the adsorber 34 the valves 36, 37, 39, 40 and 41 are provided in a manner known per se.

Es liegt im Rahmen der Erfindung, von allen bekannten Maßnahmen zur Verringerung der Kohlenwasserstoffgefahr Gebrauch zu machen, z. B. selbstreinigende Regeneratoren als Wärmetauscher für die Kühlung der Luft und/oder SiMcagel-Adsorber für die Reinigung der sauerstoff reichen Flüssigkeit zwischen Drucksäule und oberer Säule vorzusehen.It is within the scope of the invention, of all known measures to reduce the risk of hydrocarbons To make use, e.g. B. self-cleaning regenerators as heat exchangers for the Cooling the air and / or SiMcagel adsorber for to provide cleaning of the oxygen-rich liquid between the pressure column and the upper column.

Claims (3)

Patentansprüche:Patent claims: 1. Verfahren zum Eindampfen von durch Rektifikation mit kohlenwasserstoffverunTeinigter Luft1. Process for the evaporation of air polluted by rectification with hydrocarbons in einer Rektifikationssäule gewonnenem, ko'hlenwasserstoffhaltigem, flüssigem Sauerstoff in einem aus einem Bündel parallel geschalteter Rohre bestehenden Verdampfer durch Wärmeaustausch mit einem außen an dem Rohrbündel kondensierenden Gas, wobei dem Verdampfer mehr flüssiger Sauerstoff zugeführt als verdampft wird, und der entstehende gasförmige Sauerstoff im Gleichstrom mit der verdampfenden Flüssigkeit von oben nach unten oder umgekehrt fließt, und der nicht verdampfte Teil in das Bad von flüssigem Sauerstoff am Fuß der Rektifikationssäule zurückgeführt wird, nach Patentanmeldung G 21735 Ia/17g, dadurch gekennzeichnet, daß im Gleidhstromverdampfer so viel flüssiger Sauerstoff verdampft wird, daß zusammen mit der zu erzeugenden, zum Wärmeaustauscher abgeführten auch die zur Rektifikation erforderliche Menge von Sauerstoffgas entsteht, die zur Rektifiziersäule zurückgeführt wird. Hydrogen-containing liquid oxygen obtained in a rectification column in an evaporator consisting of a bundle of tubes connected in parallel by heat exchange with a gas condensing on the outside of the tube bundle, whereby more liquid oxygen is fed to the evaporator than is evaporated, and the resulting gaseous oxygen in cocurrent flows with the evaporating liquid from top to bottom or vice versa, and the non-evaporated part is returned to the bath of liquid oxygen at the foot of the rectification column, according to patent application G 21735 Ia / 17g, characterized in that so much liquid oxygen is evaporated in the Gleidhstrom evaporator that, together with the amount of oxygen gas to be generated and discharged to the heat exchanger, the amount of oxygen gas required for rectification also arises, which is returned to the rectification column . 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß Flüssigkeit und/oder Dampf des Verdampfungskreislaufs mittels Adsorptionsmitteln von den Kohlenwasserstoffen befreit werden.2. The method according to claim 1, characterized in that liquid and / or vapor of the Evaporation cycle can be freed from the hydrocarbons by means of adsorbents. 3. Einrichtung zur Durchführung des Verfahrens nach Anspruch 1 oder 2 mittels Zweisäulenrektifikation, dadurch gekennzeichnet, daß das am Fuß der Niederdrucksäule befindliche Bad von flüssigem Sauerstoff räumlich getrennt ist von dem zur Bildung von Waschflüssigkeit für die Vorrektifikationsdrucksäule vorgesehenen Druckstickstoffkondensator, welcher zur Kondensation gasförmigen Druckstickstoffs durch Verdampfen flüssigen, aus der Niederdru-cksäule mit einer Pumpe durch den Verdampfer im Gleichstrom mit den entstehenden Dämpfen geführten Sauerstoffs dient, und daß Adsorber vorgesehen sind, durch welche unverdampfter flüssiger Sauerstoff und erzeugter Sauer stoff dampf zur Niederdrucksäule zurückgeführt werden.3. Device for carrying out the method according to claim 1 or 2 by means of two-column rectification, characterized in that the bath of liquid oxygen located at the foot of the low pressure column is spatially separated from the pressurized nitrogen condenser provided for the formation of washing liquid for the pre-rectification pressure column, which for the condensation of gaseous pressure nitrogen by evaporation of liquid, from the low pressure column with a Pump through the evaporator in cocurrent with the resulting vapors of guided oxygen serves, and that adsorbers are provided, through which non-evaporated liquid oxygen and generated Oxygen vapor can be returned to the low-pressure column. Hierzu 1 Blatt Zeichnungen1 sheet of drawings © 809 635/105 9.5»© 809 635/105 9.5 »
DEG21772A 1957-03-20 1957-03-26 Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process Pending DE1039079B (en)

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DEG21735A DE1033689B (en) 1957-03-20 1957-03-20 Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process
DEG21772A DE1039079B (en) 1957-03-20 1957-03-26 Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process
US721492A US2975606A (en) 1957-03-20 1958-03-14 Procedure for the vaporization of liquid oxygen which contains hydrocarbons
GB8972/58A GB851619A (en) 1957-03-20 1958-03-20 Improvements in or relating to the rectification of air

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DEG21735A DE1033689B (en) 1957-03-20 1957-03-20 Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process
DEG21772A DE1039079B (en) 1957-03-20 1957-03-26 Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process

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