DE1226616B - Process and device for the production of gaseous pressurized oxygen with simultaneous production of liquid decomposition products by low-temperature air separation - Google Patents

Process and device for the production of gaseous pressurized oxygen with simultaneous production of liquid decomposition products by low-temperature air separation

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Publication number
DE1226616B
DE1226616B DEG33698A DEG0033698A DE1226616B DE 1226616 B DE1226616 B DE 1226616B DE G33698 A DEG33698 A DE G33698A DE G0033698 A DEG0033698 A DE G0033698A DE 1226616 B DE1226616 B DE 1226616B
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DE
Germany
Prior art keywords
nitrogen
pressure column
pressure
column
oxygen
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
DEG33698A
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German (de)
Inventor
Dipl-Ing Godehardt Kessler
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Linde GmbH
Original Assignee
Linde GmbH
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Filing date
Publication date
Application filed by Linde GmbH filed Critical Linde GmbH
Priority to DEG33698A priority Critical patent/DE1226616B/en
Priority to US240667A priority patent/US3216206A/en
Publication of DE1226616B publication Critical patent/DE1226616B/en
Pending 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
    • F25J3/04406—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
    • F25J3/04006—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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
    • F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
    • F25J3/04224—Cores associated with a liquefaction or refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04309—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04357—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
    • F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
    • 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
    • F25J2200/32—Processes or apparatus using separation by rectification using a side column fed by a stream from the 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • 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
    • F25J2220/44—Separating high boiling, i.e. less volatile components from nitrogen, e.g. CO, Ar, O2, hydrocarbons
    • 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

BUNDESREPUBLIK DEUTSCHLANDFEDERAL REPUBLIC OF GERMANY

DEUTSCHESGERMAN

PATENTAMTPATENT OFFICE

AUSLEGESCHRIFTEDITORIAL

Int. CL: Int. CL:

F25jF25j

Deutsche KL: 17 g-2/01German KL: 17 g-2/01

Nummer: 1226 616Number: 1226 616

Aktenzeichen: G 336981 a/17 gFile number: G 336981 a / 17 g

Anmeldetag: 29. November 1961Filing date: November 29, 1961

Auslegetag: 13. Oktober 1966Opening day: October 13, 1966

Die Erfindung betrifft ein Verfahren und eine Einrichtung zur Gewinnung von gasförmigem Drucksauerstoff mit gleichzeitiger Erzeugung flüssiger Zerlegungsprodukte durch Tieftemperatur-Luftzerlegung in einer Doppel-Rektifikationssäule unter Anwendung eines Stickstoffkreislaufs aus der Drucksäule über einen Hochdruckkompressor, ein Entspannungsventil und zurück zur Kälteerzeugung, wobei der Sauerstoff flüssig dem Sumpf der Niederdrucksäule entnommen, auf den gewünschten Enddruck ge- ίο bracht und unter Wärmeaustausch mit Kreislaufgas verdampft wird und wobei eine Stickstoffteilmenge aus dem Oberteil derDrucksäule nach Wärmeaustausch mit einem Teilstrom des komprimierten Kreislaufstickstoffs arbeitsleistend entspannt und mit Kopf-Stickstoff aus der Niederdrucksäule zusammen als Regeneratorspülgas verwendet wird.The invention relates to a method and a device for obtaining gaseous pressurized oxygen with simultaneous generation of liquid decomposition products through low-temperature air separation in a double rectification column using a nitrogen cycle from the pressure column a high pressure compressor, an expansion valve and back to refrigeration, with the Liquid oxygen taken from the bottom of the low-pressure column to the desired final pressure brought and is evaporated with heat exchange with circulating gas and with a partial amount of nitrogen from the top of the pressure column after heat exchange with a partial flow of the compressed circulating nitrogen working relaxed and with head nitrogen from the low pressure column together as Regenerator purge gas is used.

Die bekanntgewordenen Luftzerlegungsverfahren haben den Nachteil, daß man bei gleichzeitiger Entnahme besonders reiner Zerlegungsprodukte neben der Gewinnung von gasförmigem Drucksauerstoff nicht ohne Zuhilfenahme einer Hilfskältequelle oder entsprechenden Energieaufwand auskommt. Der verdichtete und durch Kühlung unter Zuhilfenahme einer Hilfskältequelle verflüssigte Kreislaufstickstoff wird dabei auf einen Zwischendruck entspannt, unter dem ein gasförmig anfallender Anteil in der Lage ist, eine Zusatzkolonne für die Gewinnung einer Teilmenge besonders reinen Sauerstoffs zu beheizen, und anschließend in die Drucksäule unter weiterer Drosselentspannung eingeblasen. Bei Entnahme flüssiger Zerlegungsprodukte muß ihre Kondensationswärme noch zusätzlich abgeführt werden, wozu ein besonderer, die Wirtschaftlichkeit des Verfahrens belastender Energieaufwand notwendig ist.The air separation processes that have become known have the disadvantage that they are removed at the same time particularly pure decomposition products in addition to the extraction of gaseous pressurized oxygen cannot do without the aid of an auxiliary cooling source or the corresponding expenditure of energy. The condensed one and circulating nitrogen is liquefied by cooling with the aid of an auxiliary cold source relaxed to an intermediate pressure under which a gaseous portion is able to produce a To heat additional column for the recovery of a portion of particularly pure oxygen, and then blown into the pressure column with further throttle relaxation. When removing liquid decomposition products their heat of condensation must also be dissipated, including a special, The cost-effectiveness of the process is a burdening energy expenditure.

Der Erfindung liegt die Aufgabe zugrunde, gleichzeitig flüssige Luftzerlegungsprodukte neben Drucksauerstoff ohne Sauerstoffkompressoren in einfacher und wirtschaftlicher Weise ohne Verwendung einer Hilfskältequelle zu erzeugen.The invention is based on the object of simultaneously providing liquid air separation products in addition to pressurized oxygen without oxygen compressors in a simple and economical manner without using a Generate auxiliary cold source.

Diese Aufgabe wird dadurch gelöst, daß eine weitere Stickstoffteilmenge aus dem Oberteil der Drucksäule durch Wärmeaustausch teils mit Zerlegungsluft in einem bereits mit Stickstoff gespülten Regenerator in seiner letzten Schaltphase und teils mit einem Teilstrom des komprimierten Kreislaufstickstoffs in Wärmeaustauschern angewärmt, vereinigt, nach der Verdichtung auf Hochdruck durch Wärmeaustausch mit dem Teilstrom des zu komprimierenden Kreislaufstickstoffs und mit Drucksauerstoff vorgekühlt und ein Teilstrom dieses vorgekühlten Hochdruckstickstoffs arbeitsleistend entspannt und gasförmig in den oberen Verfahren und Einrichtung zur Gewinnung von
gasförmigem Drucksauerstoff mit gleichzeitiger
Erzeugung flüssiger Zerlegungsprodukte durch
Tieftemperatur-LuftzerlegungThis object is achieved in that a further partial amount of nitrogen from the upper part of the pressure column is heated, combined by heat exchange partly with decomposition air in a regenerator already flushed with nitrogen in its last switching phase and partly with a partial flow of the compressed circulating nitrogen in heat exchangers, after compression to high pressure precooled by heat exchange with the partial flow of the circulating nitrogen to be compressed and with pressurized oxygen and a partial flow of this precooled high-pressure nitrogen expands and gaseous in the above process and device for the production of work
gaseous pressure oxygen with simultaneous
Generation of liquid decomposition products by
Low temperature air separation

Anmelder:Applicant:

Linde Aktiengesellschaft,
Wiesbaden, Hildastr. 2-10Linde Aktiengesellschaft,
Wiesbaden, Hildastr. 2-10

Als Erfinder benannt:
Dipl.-Ing. Godehardt Keßler,
Straßlach bei MünchenNamed as inventor:
Dipl.-Ing. Godehardt Keßler,
Straßlach near Munich

Teil der Drucksäule geblasen wird, während der restliche Teilstrom des Hochdruckstickstoffs durch weiteren Wärmeaustausch mit dem Teilstrom des zu komprimierenden Kreislaufstickstoffs und den Zerlegungsprodukten mindestens teilweise verflüssigt und in den oberen Teil der Drucksäule drosselentspannt wird.Part of the pressure column is blown, while the remaining partial flow of the high pressure nitrogen is blown through further Heat exchange with the partial flow of the circulating nitrogen to be compressed and the decomposition products at least partially liquefied and throttle-relieved in the upper part of the pressure column will.

Der Energie- und Kältegewinn bei der nun wirtschaftlich durchführbaren arbeitsleistenden Entspannung einer Teilmenge des hochverdichteten Kreislaufstickstoffs ist so bedeutend, daß man ohne Zuhilfenahme einer zusätzlichen Kältequelle beträchtliche Anteile der Zerlegungsprodukte, wie Stickstoff und Sauerstoff, flüssig gewinnen kann.The energy and cold gain in the now economically feasible work-performing relaxation a portion of the highly compressed circulatory nitrogen is so important that you can do without help an additional source of cold, considerable proportions of the decomposition products, such as nitrogen and Oxygen can be obtained in liquid form.

Mit Vorteil kann demnach ein Teil des im Sumpf der Niederdrucksäule anfallenden Sauerstoffs flüssig als Produkt entnommen werden, ohne ihn unter Wärmeaufnahme aus der zu zerlegenden Luft zu verdampfen. Accordingly, some of the oxygen occurring in the bottom of the low-pressure column can advantageously be liquid can be removed as a product without evaporating it from the air to be broken down while absorbing heat.

Außerdem ist auch die zusätzliche Gewinnung einer Teilmenge besonders reinen Sauerstoffs in bekannter Weise in einer entsprechenden Zusatzsäule, die mit Kreislaufstickstoff einer entsprechenden Druckstufe beheizt ist, möglich und besonders vorteilhaft.In addition, the additional production of a partial amount of particularly pure oxygen is also known Way in a corresponding additional column, which with circulating nitrogen of a corresponding pressure level is heated, possible and particularly advantageous.

Desgleichen kann nach der Erfindung ein Teil des aus der Luft anfallenden Stickstoffs mit Vorteil in flüssiger Form aus dem oberen Teil der Drucksäule gewonnen werden.Likewise, according to the invention, some of the nitrogen obtained from the air can advantageously be used in liquid form can be obtained from the upper part of the pressure column.

Für besondere Reinheitsansprüche wird dabei in der Weise vorgegangen, daß ein Teil des aus dem Oberteil der Drucksäule entnommenen Stickstoffs einer zusätzlichen Rektifiziersäule zugeleitet wird, der reiner flüssiger Stickstoff am Kopf als Produkt entnommen wird, während das Sumpfprodukt dieser Säule auf den Kopf der Drucksäule zurückgeführt wird.For special purity requirements, the procedure is that part of the from the Upper part of the pressure column removed nitrogen is fed to an additional rectification column, the pure liquid nitrogen is removed at the top as product, while the bottom product of this Column is returned to the top of the pressure column.

609 670/74609 670/74

Der Kopfkondensator der zusätzlichen Säule wird dabei vorteilhaft mit einer Teilmenge des entspannten Sauerstoffs aus dem Sumpf der Drucksäule gekühlt, die anschließend einem Boden im mittleren Teil der Niederdrucksäule zugeführt wird.The top condenser of the additional column is advantageous with a subset of the relaxed Oxygen from the sump of the pressure column is cooled, which is then a bottom in the middle Part of the low pressure column is fed.

Ein weiterer Kältegewinn läßt sich mit Vorteil bei zweckmäßiger Gestaltung des Stickstoffwärmeaustausches in an sich bekannter Weise durch Entspannung einer Teilmenge des gasförmig aus der Drucksäule abgezogenen Stickstoffs in einer Entspannungsturbine erzielen. A further gain in cold can advantageously be achieved with an expedient design of the nitrogen heat exchange in a manner known per se by releasing a portion of the gas from the pressure column Achieve withdrawn nitrogen in an expansion turbine.

Die Gestaltung des Wärmeaustausches zwischen der eintretenden Luft und aus der Drucksäule anfallendem Stickstoff läßt sich schließlich dadurch noch verbessern, daß aus dem mit zu komprimierendem Kreislaufstickstoff aus der Drucksäule beschickten Regenerator eine Teilmenge nach Vorwärmung abgezweigt und im Wärmeaustausch mit komprimiertem Kreislauf stickstoff angewärmt wird.The design of the heat exchange between the incoming air and the air coming from the pressure column Nitrogen can finally be improved by removing the with to be compressed Cycle nitrogen from the pressure column fed regenerator diverted a portion after preheating and nitrogen is heated in the heat exchange with compressed circuit.

Das erfindungsgemäße Verfahren soll nunmehr an Hand eines Schemas für Luftzerlegung beispielsweise näher erläutert werden.The method according to the invention should now be based on a scheme for air separation, for example are explained in more detail.

Komprimierte Luft wird durch Leitung 1 einem der zyklisch vertauschbaren Regeneratoren la bis Id zugeführt und gelangt durch Leitung 2 in die Drucksäule 3 einer Rektifizierkolonne. Aus dem Unterteil dieser Drucksäule wird durch Leitung 4 unreiner Sauerstoff und durch 'die Leitungen 5 und 6 am Oberteil der Drucksäule 3 weitgehend angereicherter Stickstoff abgezogen. Am Kopf der Drucksäule 3 befindet sich der Hauptkondensator 7, der gleichzeitig den Heizkörper für den Sumpf 9 der Niederdracksäule 8 bildet.Compressed air is fed through line 1 to one of the cyclically interchangeable regenerators la to Id and passes through line 2 into the pressure column 3 of a rectification column. From the lower part of this pressure column, impure oxygen is withdrawn through line 4 and largely enriched nitrogen is withdrawn through lines 5 and 6 at the upper part of the pressure column 3. At the top of the pressure column 3 is the main condenser 7, which at the same time forms the heating element for the sump 9 of the low-pressure column 8.

In dem Sumpf 9 um die Kühlrohre des Hauptkondensators 7 sammelt sich flüssiger Sauerstoff an. Der unreine Sauerstoff aus Leitung 4 wird über zwei wechselweise betriebene Adsorber 10 und Leitung 11 sowie Wärmeaustauscher 12 und Leitung 13 zum Teil über das Entspannungsventil 14 in den mittleren Teil der Niederdrucksäule 8 eingeführt, während ein anderer Teil über das Entspannungsventil 15 und Leitung 16 dem Kondensator 17 einer zusätzlichen Stickstoff-Rektifiziersäule 18 zugeführt wird, aus dem der verdampfende unreine Sauerstoff durch Leitung 19 ebenfalls in den mittleren Teil der Säule 8 etwas tiefer eintritt. Der Zusatzsäule 18 wird Stickstoff durch die Leitung 5 zugeführt. Aus dem Sumpf der zusätzlichen Säule 18 wird durch Leitung 20 flüssiger sauerstoffhaltiger Stickstoff in die Drucksäule 3 zurückgeführt. Der sich auf dem Boden 21 ansammelnde flüssige Stickstoff wird über Leitung 22 und das Entspannungsventil 23 mit Fortsetzungsleitung 24 auf den Kopf der' Säule 8 mit der Speicher- und Verteilertasse 25 als Waschflüssigkeit, gegebenenfalls unter Zwischenkühlung, entspannt. Die Leitung 26 führt gasförmigen Stickstoff über den Wärmeaustauscher 12 und die Leitung 27 sowie die Sammelleitung 28 mit den Zweigleitungen 29 und 30 zu zwei der Regeneratoren la bis Id, aus denen er durch die Leitungen 31 und 32 zu beliebiger Verwendung austritt.In the sump 9 around the cooling tubes of the main condenser 7, liquid oxygen collects. The impure oxygen from line 4 is introduced via two alternately operated adsorbers 10 and line 11 as well as heat exchangers 12 and line 13 in part via the expansion valve 14 into the middle part of the low-pressure column 8, while another part is introduced into the condenser via the expansion valve 15 and line 16 17 is fed to an additional nitrogen rectification column 18, from which the evaporating impure oxygen also enters the middle part of the column 8 somewhat deeper through line 19. The additional column 18 is supplied with nitrogen through line 5. From the bottom of the additional column 18, liquid oxygen-containing nitrogen is returned to the pressure column 3 through line 20. The liquid nitrogen accumulating on the bottom 21 is expanded via line 22 and the expansion valve 23 with continuation line 24 to the top of the column 8 with the storage and distribution cup 25 as washing liquid, optionally with intermediate cooling. The line 26 leads gaseous nitrogen via the heat exchanger 12 and the line 27 and the collecting line 28 with the branch lines 29 and 30 to two of the regenerators la to Id, from which it exits through the lines 31 and 32 for any use.

Flüssiger hochreiner Stickstoff wird aus der Tasse 33 der zusätzlichen Säule 18 über Leitung 34 in einen Tank 35 abgezogen, aus dem er durch Leitung 36 als Produkt gewonnen werden kann. Flüssiger Sauerstoff wird aus dem Hauptkondensator 7 durch Leitung 37 abgezogen und gelangt in den Tank 38, woraus er durch Leitung 39 als Produkt abgezogen werden kann.Liquid high purity nitrogen is from the cup 33 of the additional column 18 via line 34 into a Tank 35 withdrawn, from which it can be obtained through line 36 as a product. Liquid oxygen is withdrawn from the main condenser 7 through line 37 and enters the tank 38, from which it can be withdrawn as product through line 39.

Ein anderer Teil des flüssigen Sauerstoffs wird durch die Leitung 41 abgezogen und gelangt zu der Hochdruckpumpe 42. Von hieraus gelangt der Sauerstoff unter Druck über die Leitung 43 zum Wärmeaustauscher 43 α, über die Leitung 44 zum Wärmeaustauscher 44 λ, über die Leitung 45 zum Wärmeaustauscher 45 α und wird über die Leitung 46 gasförmig als Drucksauerstoff abgegeben.
Die Leitung 6 liefert weitgehend angereichertenAnother part of the liquid oxygen is withdrawn through line 41 and reaches the high pressure pump 42. From here, the oxygen under pressure reaches the heat exchanger 43 α via line 43, via line 44 to heat exchanger 44 λ, via line 45 to the heat exchanger 45 α and is released in gaseous form as pressurized oxygen via line 46.
The line 6 delivers largely enriched

ίο Stickstoff zu einem der Regeneratoren la bis Id und über die Zweigleitung 48 zum Wärmeautauscher 43 b. Vom Wärmeaustauscher 43 & gelangt der Stickstoff über die Leitung 49 zum Wärmeaustauscher 45 b, über die Leitung 50 zum Wärmeaustauscher 45 c und durch die Leitung 51 zu der aus dem Regenerator Id kommenden Stickstoffleitung 52, die ihrerseits zum Hochdruckkompressor 53 führt, der mit Vorteil als Trockenlaufkompressor ausgebildet ist, um Verölen der Wärmeaustauscheinrichtungen und immerhin bestehende Explosionsgefahren durch vom Kreislaufstickstoff in die Drucksäule 3 mitgerissene Schmiermittel zu vermeiden.ίο nitrogen to one of the regenerators la to Id and via the branch line 48 to the heat exchanger 43 b. From the heat exchanger 43 & the nitrogen arrives via the line 49 to the heat exchanger 45 b, via the line 50 to the heat exchanger 45 c and through the line 51 to the nitrogen line 52 coming from the regenerator Id , which in turn leads to the high pressure compressor 53, which is advantageously used as The dry-running compressor is designed to prevent the heat exchange devices from becoming oily and, after all, the risk of explosion caused by the lubricant entrained into the pressure column 3 by the circulating nitrogen.

Der hier je nach Bedarf an flüssigen Luftzerlegungsprodukten auf 50 bis 200 ata komprimierte Stickstoff gelangt durch die Leitung 54 und die Zweigleitungen 55 und 56 zu den Wärmeaustauschern 45 c bzw. 45 a. Die Leitung 57 liefert den Stickstoff vom Wärmeaustauscher 45 c zum Wärmeaustauscher 45 b. Vom Wärmeaustauscher 45 & zum Wärmeaustauscher 44 a und vom Wärmeaustauscher 45 a zum Wärmeaustauscher 44 a führen die Leitungen 58 bzw. 59. Die Leitungen 60 und 61 führen die beiden Ströme vom Wärmeaustauscher 44 a zum Wärmeaustauscher 43 b bzw. 43 a. Die Leitungen 62 und 63 führen den tiefgekühlten Stickstoff aus den Wärmeaustauschern 43 b bzw. 43 a über Entspannungsventile 65 bzw. 64 sowie die Leitungen 67 bzw. 66 auf den Kopf der Drucksäule 3.
Die Stickstoffleitung 49 besitzt noch eine Abzweigleitung 69, die einen Teil des Stickstoffs über die Entspannungsturbine 70 und Leitung 71 der Sammelleitung 28 zu zwei der Regeneratoren la bis Id zuführt. Der Leitung 49 wird dann sinngemäß aus dem Kreislauf regenerator (gezeichnet la") durch Leitung 72 wieder Stickstoff zugeführt.The nitrogen compressed here to 50 to 200 ata depending on the need for liquid air separation products passes through line 54 and branch lines 55 and 56 to heat exchangers 45 c and 45 a. The line 57 supplies the nitrogen from the heat exchanger 45 c to the heat exchanger 45 b. Lines 58 and 59 lead from heat exchanger 45 & to heat exchanger 44 a and from heat exchanger 45 a to heat exchanger 44 a. Lines 60 and 61 lead the two flows from heat exchanger 44 a to heat exchanger 43 b and 43 a, respectively. The lines 62 and 63 lead the deep-frozen nitrogen from the heat exchangers 43 b and 43 a via expansion valves 65 and 64 and the lines 67 and 66 to the top of the pressure column 3.
The nitrogen line 49 also has a branch line 69 which feeds part of the nitrogen via the expansion turbine 70 and line 71 of the collecting line 28 to two of the regenerators 1a to Id . The line 49 is then fed from the regenerator circuit (drawn la ") through line 72 again nitrogen.

Aus den Hochdruckleitungen 57 und 59 für vorgekühlten Stickstoff wird durch Leitung 73 eine Teilmenge entnommen, in der Entspannungsturbine 74 entspannt und durch Leitung 75 in die Drucksäule 3 eingeblasen.The high-pressure lines 57 and 59 for precooled nitrogen are converted into a partial amount through line 73 taken, expanded in the expansion turbine 74 and through line 75 into the pressure column 3 blown in.

Der dabei erzielte Energie- und Kältegewinn ist beträchtlich und gestattet den Ausgleich des Kältehaushalts auch bei Entnahme relativ großer Anteile der Zerlegungsprodukte in flüssigem oder besonders reinem Zustand.The energy and cold gain achieved in this way is considerable and allows the cold balance to be balanced even with the removal of relatively large proportions of the decomposition products in liquid or special pure state.

Mit besonderem Vorteil wird dabei eine Entspannungsturbine angewandt, da ihre kontinuierliche Arbeitsweise störende Schwingungen vermeidet. Außerdem wird die Gefahr von Verstopfungen und von Explosionen in der mit angereichertem Sauerstoff beaufschlagten Drucksäule durch Schmiermittel, die z. B. aus einer Kolben-Entspannungsmaschine mitgerissen werden können, vermieden, da die Turbine ohne Schmierung der gasbeaufschlagten Teile auskommt. Hinzu kommt Materialersparnis und Wartungsfreiheit gegenüber einer Kolbenmaschine, was mit Rücksicht auf die notwendige Kälteisolation von besonderem Vorteil ist.An expansion turbine is used with particular advantage because of its continuous mode of operation avoids disturbing vibrations. It also increases the risk of clogging and of Explosions in the pressure column charged with enriched oxygen by lubricants that z. B. can be carried away from a piston expansion machine, avoided because the turbine does not require lubrication of the gas-exposed parts. In addition, there is material savings and no maintenance compared to a piston engine, which takes into account the necessary cold insulation of particular advantage is.

1010

Das erfindungsgemäße Verfahren kann sinngemäß abgewandelt auch für die Zerlegung beliebiger anderer Gasgemische als Luft, beispielsweise Kohlenwasserstoff-Gasgemische, wie Erdgas, angewandt werden. Dabei kann z. B. als Kreislaufgas anstatt Stickstoff ein dem Hauptbestandteil des zu zerlegenden Gasgemisches entsprechendes Gas, z. B. Methan, angewandt werden.The method according to the invention can also be modified accordingly for the decomposition of any other Gas mixtures as air, for example hydrocarbon gas mixtures, such as natural gas, are used. It can, for. B. as a cycle gas instead of nitrogen, the main component of the to be dismantled Gas mixture corresponding gas, e.g. B. methane, can be used.

Claims (8)

Patentansprüche:Patent claims: 1. Verfahren zur Gewinnung von gasförmigem Drucksauerstoff mit gleichzeitiger Erzeugung flüssiger Zerlegungsprodukte durch Tieftemperatur-Luftzerlegung in einer Doppel-Rektifikationssäule unter Anwendung eines Stickstoffkreislaufs aus der Drucksäule über einen Hochdruckkompressor, ein Entspannungsventil und zurück zur Kälteerzeugung, wobei der Sauerstoff flüssig dem Sumpf der Niederdrucksäule entnommen, auf den gewünschten Enddruck gebracht und unter ao Wärmeaustausch mit Kreislaufgas verdampft wird und wobei eine Stickstoffteilmenge aus dem Oberteil der Drucksäule nach Wärmeaustausch mit einem Teilstrom des komprimierten Kreislaufstickstoffs arbeitsleistend entspannt und mit Kopfstickstoff aus der Niederdrucksäule zusammen als Regeneratorspülgas verwendet wird, dadurch gekennzeichnet, daß eine weitere Stickstoffteilmenge aus dem Oberteil der Drucksäule durch Wärmeaustausch teils mit Zerlegungsluft in einem bereits mit Stickstoff gespülten Regenerator in seiner letzten Schaltphase und teils mit einem Teilstrom des komprimierten Kreislaufstickstoffs in Wärmeaustauschern angewärmt, vereinigt, nach der Verdichtung auf Hochdruck durch Wärmeaustausch mit dem Teilstrom des zu komprimierenden Kreislaufstickstoffs und mit Drucksauerstoff vorgekühlt und ein Teilstrom dieses vorgekühlten Hochdruckstickstoffs arbeitsleistend entspannt und gasförmig in den oberen Teil der Drucksäule geblasen wird, während der restliche Teilstrom des Hochdruckstickstoffs durch weiteren Wärmeaustausch mit dem Teilstrom des zu komprimierenden Kreislaufstickstoffs und den Zerlegungsprodukten mindestens teilweise verflüssigt und in den oberen Teil der Drucksäule drosselentspannt wird.1. Process for the production of gaseous pressurized oxygen with simultaneous generation liquid separation products by cryogenic air separation in a double rectification column using a nitrogen cycle from the pressure column via a high pressure compressor, a relief valve and back to the refrigeration, whereby the oxygen is liquid dem Taken from the bottom of the low pressure column, brought to the desired final pressure and under ao Heat exchange with circulating gas is evaporated and with a partial amount of nitrogen from the upper part the pressure column after heat exchange with a partial flow of the compressed circulating nitrogen working relaxed and with head nitrogen from the low-pressure column together is used as Regeneratorspülgas, characterized in that a further Partial amount of nitrogen from the upper part of the pressure column through heat exchange partly with decomposition air in a regenerator already flushed with nitrogen in its last switching phase and partly heated with a partial flow of the compressed cycle nitrogen in heat exchangers, united, after compression to high pressure by heat exchange with the partial flow of the to be compressed circulating nitrogen and precooled with pressurized oxygen and a partial flow this pre-cooled high-pressure nitrogen is relaxed and gaseous in the upper one, performing work Part of the pressure column is blown, while the remaining partial flow of high pressure nitrogen by further heat exchange with the partial flow of the circulating nitrogen to be compressed and the decomposition products are at least partially liquefied and in the upper part of the Pressure column is relaxed throttle. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß ein Teil des flüssigen Sauerstoffs aus dem Sumpf der Niederdrucksäule unter Druck verdampft und der Rest flüssig als Produkt entnommen wird.2. The method according to claim 1, characterized in that part of the liquid oxygen evaporated under pressure from the bottom of the low-pressure column and the remainder is a liquid product is removed. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß dem oberen Teil der Drucksäule ein Teil des flüssigen Stickstoffs als Produkt entnommen wird.3. The method according to claim 1, characterized in that the upper part of the pressure column part of the liquid nitrogen is removed as a product. 4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß ein Teil des aus dem oberen Teil der Drucksäule entnommenen Stickstoffs einer zusätzlichen Rektifiziersäule zugeleitet wird, der reiner flüssiger Stickstoff am Kopf als Produkt entnommen wird, während das Sumpfprodukt dieser Säule auf den Kopf der Drucksäule zurückgeführt wird.4. The method according to claim 1, characterized in that part of the from the upper Part of the nitrogen removed from the pressure column is fed to an additional rectification column, the pure liquid nitrogen is removed as product at the top, while the bottom product this column is returned to the top of the pressure column. 5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß der Kopfkondensator der zusätzlichen Stickstoff-Rektifiziersäule mit einer Teilmenge des aus dem Sumpf der Drucksäule entnommenen und entspannten Sauerstoffs gekühlt wird, die anschließend einem Boden im mittleren Teil der Niederdrucksäule zugeführt wird.5. The method according to claim 4, characterized in that the top capacitor of the additional Nitrogen rectification column with a portion of that from the bottom of the pressure column extracted and relaxed oxygen is cooled, which is then a floor in the central part of the low pressure column is supplied. 6. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß eine Teilmenge besonders reinen Sauerstoffs in an sich bekannter Weise in einer mit Sauerstoff aus dem Sumpf der Niederdrucksäule beschickten Zusatzsäule, deren Sumpf mit Kreislaufstickstoff einer entsprechenden Druckstufe beheizt ist, gewonnen wird.6. The method according to claim 1, characterized in that a subset is particularly pure Oxygen in a manner known per se in one with oxygen from the bottom of the low-pressure column charged additional column, the bottom of which with circulating nitrogen of a corresponding Pressure stage is heated, is obtained. 7. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß aus dem zu komprimierendem Kreislaufstickstoff aus der Drucksäule beschickten Regenerator eine Teilmenge nach Vorwärmung abgezweigt und im Wärmeaustausch mit komprimiertem Kreislaufstickstoff angewärmt wird.7. The method according to claim 1, characterized in that from the to be compressed Cycle nitrogen from the pressure column fed regenerator a partial amount after preheating branched off and warmed up in the heat exchange with compressed circulating nitrogen will. 8. Einrichtung zur Durchführung des Verfahrens nach einem oder mehreren der Ansprüche 1 bis 7, dadurch gekennzeichnet, daß zur Entspannung einer Teilmenge des Kreislaufstickstoffs eine Entspannungsturbine (74) dient, deren Eintrittsstutzen mit den Leitungen (57, 59) aus dem Hochdruckkompressor (53) nachgeschalteten, im Gegenstrom mit Stickstoff aus dem Oberteil der Drucksäule (3) bzw. Sauerstoff aus dem Sumpf der Niederdrucksäule (8) gekühlten Wärmeaustauschern (45 c, 45 ä) verbunden ist, während die Austrittsleitung der Entspannungsturbine (74) zur Drucksäule (3) führt.8. Device for carrying out the method according to one or more of claims 1 to 7, characterized in that an expansion turbine (74) is used to expand a portion of the circulating nitrogen, the inlet nozzle of which with the lines (57, 59) from the high-pressure compressor (53) downstream, in countercurrent with nitrogen from the upper part of the pressure column (3) or oxygen from the bottom of the low pressure column (8) cooled heat exchangers (45 c, 45 e) is connected, while the outlet line of the expansion turbine (74) to the pressure column (3) leads. In Betracht gezogene Druckschriften:
Deutsche Patentschrift Nr. 921 809;
Hausen, »Handbuch der Kältetechnik«, 8. Band (1957), S. 30.Considered publications:
German Patent No. 921 809;
Hausen, "Handbuch der Kältetechnik", Volume 8 (1957), p. 30. Hierzu 1 Blatt Zeichnungen1 sheet of drawings 609 670/74 10.66 © Bundesdruckerei Berlin609 670/74 10.66 © Bundesdruckerei Berlin
DEG33698A 1961-11-29 1961-11-29 Process and device for the production of gaseous pressurized oxygen with simultaneous production of liquid decomposition products by low-temperature air separation Pending DE1226616B (en)

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