DE3016317A1 - Liquid nitrogen prodn. process - feeds liquid oxygen into base of low pressure column for air decomposition - Google Patents

Liquid nitrogen prodn. process - feeds liquid oxygen into base of low pressure column for air decomposition

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Publication number
DE3016317A1
DE3016317A1 DE19803016317 DE3016317A DE3016317A1 DE 3016317 A1 DE3016317 A1 DE 3016317A1 DE 19803016317 DE19803016317 DE 19803016317 DE 3016317 A DE3016317 A DE 3016317A DE 3016317 A1 DE3016317 A1 DE 3016317A1
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Germany
Prior art keywords
pressure column
nitrogen
liquid
liquid oxygen
low pressure
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.)
Withdrawn
Application number
DE19803016317
Other languages
German (de)
Inventor
Klaus Dipl.-Ing. 4000 Düsseldorf Baumgärtner
Werner Dipl.-Ing. 4100 Duisburg Klug
Gottfried Ing.(grad.) 4224 Hünxe Panhaus
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Messer Griesheim GmbH
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Messer Griesheim GmbH
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Application filed by Messer Griesheim GmbH filed Critical Messer Griesheim GmbH
Priority to DE19803016317 priority Critical patent/DE3016317A1/en
Publication of DE3016317A1 publication Critical patent/DE3016317A1/en
Withdrawn legal-status Critical Current

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Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04763Start-up or control of the process; Details of the apparatus used
    • F25J3/04866Construction and layout of air fractionation equipments, e.g. valves, machines
    • F25J3/04951Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
    • F25J3/04963Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation 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
    • F25J3/04309Generation 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04406Processes 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
    • F25J3/04412Processes 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04642Recovering noble gases from air
    • F25J3/04745Krypton and/or Xenon
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/34Processes or apparatus using separation by rectification using a side column fed by a stream from the low pressure column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/90Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94Details relating to the withdrawal point
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00Processes characterised by the type or other details of the feed stream
    • F25J2210/50Oxygen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3

Landscapes

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

Abstract

The process produces liquid nitrogen using the refrigerating action resulting from evaporation of liquid oxygen. The liquid oxygen is fed externally into the base of a low pressure column of a two-column unit, for air decomposition, where it evaporates in a main condenser under the action of the condensing nitrogen in a medium-pressure column. The nitrogen is collected below the main condenser, and drawn off as the product. The gaseous nitrogen can be drawn off from the head of the medium-pressure column, expanded to produce output, and brought into heat-exchange contact with the air to be decomposed.

Description

MESSER GRIESHEIM GMBH MG 1227MESSER GRIESHEIM GMBH MG 1227

Kennwort: O2/N3-Konvertierung EM 922Password: O 2 / N 3 conversion EM 922

Erfinder: K.Baumgärtner Ordner: aInventor: K. Baumgärtner File: a

W.Klug
G.Panhaus
W. Clever
G. Panhaus

Verfahren zur Gewinnung von flüssigem StickstoffProcess for the production of liquid nitrogen

Die Erfindung betrifft ein Verfahren zur Gewinnung von flüssigem Stickstoff unter Verwendung der durch die Verdampfung von flüssigem Sauerstoff gewonnenen Kälte. The invention relates to a method for obtaining liquid nitrogen using the cold obtained by the evaporation of liquid oxygen.

Die Kapazität der nach dem Zweisäulenprinzip arbeitenden Luftzerlegungsanlagen ist in den letzten Jahren sehr vergrößert worden. Neben gasförmigem Sauerstoff und Stickstoff erzeugen derartige Anlagen auch diese Gase im flüssigen Zustand. Die Flexibilität der Luftzerlegungsanlagen ist allerdings begrenzt, d.h. das Verhältnis der erzeugten flüssigen und gasförmigen Produkte zueinander kann nur in gewissem Umfang variiert werden. Die Anpassung an die stark schwankende Marktlage ist mit den grossen Anlagen daher schwierig. Häufig tritt z.B. eine verstärkte Nachfrage nach flüssigem Stickstoff auf, die ausThe capacity of those working on the two-pillar principle Air separation plants have been greatly enlarged in recent years. In addition to gaseous oxygen and nitrogen Such systems also generate these gases in their liquid state. The flexibility of air separation plants is limited, however, i.e. the ratio of the liquid and gaseous products produced to one another can only be varied to a certain extent. The adjustment to the strongly fluctuating market situation is with the big Investments are therefore difficult. Often, for example, there is an increased demand for liquid nitrogen that is released

130044/0506130044/0506

.3·.3 ·

den genannten Gründen nur befriedigt werden kann, indem flüssiger Stickstoff von Wettbewerbern zugekauft wird. Dies ist mit erheblichen Kosten verbunden.the reasons mentioned can only be satisfied by purchasing liquid nitrogen from competitors. This is associated with considerable costs.

Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art zu schaffen, welches es gestattet, eine vorhandene Luftzerlegungsanlage hinsichtlich der Ausbringung an flüssigem Stickstoff flexibler zu betreiben.The invention is therefore based on the object of creating a method of the type mentioned at the outset which it allows an existing air separation plant to be more flexible with regard to the discharge of liquid nitrogen to operate.

Es wurde nun ein Verfahren zur Gewinnung von flüssigem Stickstoff unter Verwendung der durch die Verdampfung von flüssigem Sauerstoff gewonnenen Kälte gefunden,bei dem gemäß der Erfindung der flüssige Sauerstoff extern in den Boden der Niederdrucksäule eines Zweisäulenapparates zur Luftzerlegung eingespeist wird, wo er im Haupt kondensator gegen kondensierenden Stickstoff in der Mitteldrucksäule verdampft, welcher unterhalb des Hauptkondensators aufgefangen und als Produkt der Anlage entnommen wird.There has now been a method of recovering liquid nitrogen using that by evaporation found cold obtained by liquid oxygen, in which, according to the invention, the liquid oxygen is external is fed into the bottom of the low-pressure column of a two-column apparatus for air separation, where it is in the main condenser evaporates against condensing nitrogen in the medium pressure column, which is below the main condenser is collected and taken as a product of the system.

In dem erfindungsgemäßen Verfahren wird daher extern vorhandener flüssiger Sauerstoff dazu benutzt, die Ausbringung von flüssigem Stickstoff einer vorhandenen Luftzerlegungsanlage zu vergrößern, indem der Sauerstoff verdampft wird und eine entsprechend größere Menge Stick stoff verflüssigt wird. Durch die Einspeisung des flüssigen Sauerstoffs in die Niederdrucksäule wird dort das Flüssig-Dampf-Verhältnis so geändert, daß aus der Mit-0 teldrucksäule eine erhöhte Menge an flüssigem Stickstoff abgezogen werden kann.In the method according to the invention, therefore, is external existing liquid oxygen is used for the application of liquid nitrogen to an existing one To enlarge air separation plant by the oxygen is evaporated and a correspondingly larger amount of stick substance is liquefied. By feeding the liquid oxygen into the low-pressure column, the Liquid-vapor ratio changed so that from the Mit-0 teldrucksäule an increased amount of liquid nitrogen can be withdrawn.

Der für das erfindungsgemäße Verfahren erforderliche externe flüssige Sauerstoff kann von anderem Luftzerlegungsanlagen bezogen werden oder in der vorhandenenThe one required for the method according to the invention external liquid oxygen can be obtained from other air separation units be related or in the existing

130044/0506130044/0506

Anlage zuvor selbst erzeugt und gespeichert worden sein.System must have been generated and saved beforehand.

Besonders vorteilhaft ist das erfindungsgemäße Verfahren, wenn es mit einer arbeitsleitenden Entspannung von gasförmig aus dem Kopf der Mitteldrucksäule abgezogenem Stickstoff durchgeführt wird. Die hierdurch erzeugte Kälte dient normalerweise dazu, die zu zerlegende Luft durch Wärmeaustausch zusätzlich abzukühlen und ermöglicht hierdurch die Produktion von flüssigem Stickstoff. Bei Einspeisung von externem flüssigen Sauerstoff gemäß der Erfindung kann auf diese arbeitsleistende Entspannung des gasförmigen Stickstoffs ganz oder teilweise verzichtet werden und eine entsprechende Stickstoffmenge zusätzlich als flüssiges Produkt gewonnen werden. Hierdurch wird das erfindungsgemäße Verfahren, was die Ausbringung von flüssigem Stickstoff anbetrifft, äußerst flexibel.The method according to the invention is particularly advantageous, if it is with a working relaxation of gaseous nitrogen withdrawn from the top of the medium pressure column is carried out. The resulting Cold is normally used to additionally cool the air to be separated by exchanging heat thereby the production of liquid nitrogen. When feeding in external liquid oxygen according to the Invention can relate to this work-performing relaxation of the gaseous nitrogen can be completely or partially dispensed with and a corresponding amount of nitrogen in addition can be obtained as a liquid product. As a result, the method according to the invention, what the application of As for liquid nitrogen, extremely flexible.

Darüber hinaus ist es von Vorteil, wenn bei dem erfindungs gemäßen Verfahren eine Anreicherung von Krypton und Xenon durchgeführt wird. Hierzu wird vom Boden der Niederdrucksäule flüssiger Sauerstoff abgezogen und nach Abtrennung eines an Kryton und Xenon angereicherten Teilstromes in einer Krypten-Xenon-Anreicherungsanlage in gasförmigem Zustand als Produkt abgeführt. Abgesehen davon, daß auf diese Weise auch eine Kohlenwasserstoffanreicherung vermieden wird, läßt sich hierdurch auch das im extern zugeführten flüssigen Sauerstoff ggf. vorhandene Krypton und Xenon gewinnen.In addition, it is advantageous if, in the method according to the invention, an enrichment of krypton and Xenon is carried out. This is done from the bottom of the low-pressure column liquid oxygen withdrawn and after separation of a substream enriched in Kryton and Xenon discharged as a product in a crypt xenon enrichment system in a gaseous state. Apart from that from the fact that in this way also a hydrocarbon enrichment is avoided, this also allows any existing liquid oxygen that is supplied externally to be eliminated Win krypton and xenon.

Ein Ausführungsbeispiel der Erfindung wird anhand der beigefügten Zeichnung dargestellt. Es handelt sich hierbei um ein Luftzerlegungsverfahren mit arbeitsleistender Stickstoffentspannung und Anreicherung von Krypton undAn embodiment of the invention is illustrated with reference to the accompanying drawing. It is an air separation process with work-performing Nitrogen relaxation and enrichment of krypton and

Xenon.
35
Xenon.
35

1300-44/05061300-44 / 0506

Die verdichtete zu zerlegende Luft gelangt durch die Leitung 1 über die Wärmeaustauscher 2 in die Mitteldrucksäule 3. Hier wird sie zerlegt in reinen Stickstoff (O2-Gehalt unter 2 vpm) im Kopf der Mitteldrucksäule 3 und in eine Sumpfflüssigkeit mit etwa 39% Sauerstoffgehalt. Oberhalb des obersten Bodens der Mitteldrucksäule wird durch Leitung 4 gasförmiger Stickstoff entnommen und nach teilweiser Anwärmung in den Wärmeaustauschern in der Entspannungsturbine 5 arbeitsleistend entspannt.The compressed air to be separated passes through the line 1 via the heat exchanger 2 into the medium-pressure column 3. Here it is broken down into pure nitrogen (O 2 content below 2 vpm) in the top of the medium-pressure column 3 and into a sump liquid with about 39% oxygen content. Above the uppermost base of the medium-pressure column, gaseous nitrogen is withdrawn through line 4 and, after partial heating in the heat exchangers in the expansion turbine 5, is expanded to perform work.

Der entspannte Stickstoff verläßt die Entspannungsturbine 5 durch die Leitung 6, durchströmt die Wärmeaustauscher und steht für die Weiterverdichtung zur Verfügung. Die durch die Entspannungsturbine 5 erzeugte Überschußkälte wird im normalen Betrieb durch die Entnahme von flussigern Stickstoff abgebaut. Dieser flüssige Stickstoff wird in der Mitteldrucksäule 3 unterhalb des Hauptkondensators 7 aufgefangen und durch Leitung 8 als Produkt aus der Anlage abgeführt. Die Sumpfflüssigkeit wird aus der Mitteldrucksäule 3 durch Leitung 10 über den Wärmeaustauscher geführt und durch das Entspannungsventil 12 in den mittleren Teil der Niederdrucksäule 9 entspannt. Außerdem wird durch Leitung 13 aus dem mittleren Teil der Mitteldrucksäule 3 eine flüssige Zwischenfraktion abgezogen, durch den Wärmeaustauscher 11 geführt und über das Entspannungsventil 14 in den Kopf der Niederdrucksäule 9 entspannt.The expanded nitrogen leaves the expansion turbine 5 through line 6 and flows through the heat exchanger and is available for further compression. The excess cold generated by the expansion turbine 5 is due to the removal of liquids during normal operation Nitrogen degraded. This liquid nitrogen is in the medium pressure column 3 below the main condenser 7 collected and discharged through line 8 as a product from the system. The sump liquid comes from the medium pressure column 3 passed through line 10 over the heat exchanger and through the expansion valve 12 in the middle Part of the low pressure column 9 relaxed. In addition, through line 13 from the middle part of the medium-pressure column 3 withdrawn a liquid intermediate fraction, passed through the heat exchanger 11 and via the expansion valve 14 relaxed in the head of the low pressure column 9.

Vom Kopf der Niederdrucksäule 9 wird über Leitung 15 unreiner Stickstoff abgezogen, in den Wärmeaustauschern 11 und 2 angewärmt und aus der Anlage abgeführt. In der Anlage wird außerdem Krypton und Xenon angereichert. Zu diesem Zweck wird am Boden der Niederdrucksäule 9 im Hauptkondensator 7 der sich dort sammelnde flüssige Sauerstoff auf ca. 150 vpm Krypton angereichert. Ein Teil dieses flüssigen Sauerstoffs wird durch die Leitung 16 in die Krypton-Xenon-Anreicherungsanlage 17 geführt.From the top of the low-pressure column 9, line 15 becomes more impure Nitrogen is drawn off, heated in the heat exchangers 11 and 2 and discharged from the system. In the plant it is also enriched with krypton and xenon. For this purpose, the bottom of the low pressure column 9 is im Main capacitor 7, the liquid oxygen that collects there is enriched to approx. 150 vpm krypton. A Part of this liquid oxygen is fed through line 16 into the krypton-xenon enrichment system 17.

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Hier wird ein kleiner,hoch mit Krypton und Xenon angereicherter Teilstrom abgetrennt und durch Leitung 18 einer nicht dargestellten Anlage zur Gewinnung von Krypton und Xenon zugeführt. Die Hauptmenge wird gasförmig durch Leitungen 19 und 23 der Sperrkolonne 20 zugeführt. In dieser wird mit kryptonfreiem flüssigen Sauerstoff der aus der Niederdrucksäule9 durch Leitung 21 und Ventil 22 abgezogen wird, über einige Böden das in dem Sauerstoffgas, welches über Leitung 19. zugeführt wird, noch enthaltene Krypton ausgewaschen. Die gleiche Behandlung wird dem durch Leitung 23 aus der Niederdrucksäule 9 abgezogenen gasförmigen Sauerstoff zuteil. Der sich am Boden der Sperrkolonne 20 anreichernde flüssige Sauerstoff wird durch Leitung 24 zurück in den Boden der Niederdrucksäule 9 geleitet. Durch diesen Kondensatorkreislauf wird außerdem eine gefährliche Anreicherung von Kohlenwasserstoffen am Boden der Niederdrucksäule 9 vermieden, da auch die Kohlenwasserstoffe durch Leitung 16 ständig abgeführt und in der Krypton-Xenon-Anreicherungsanlage 17 entfernt werden. Aus der Sperrkolonne 20 wird durch Leitung 25 gasförmiger Sauerstoff abgezogen, in den Wärmeaustauschern 2 erwärmt und als Produkt der Anlage entnommen. Falls nun eine erhöhte Nachfrage nach flüssigem Stickstoff vorhanden ist und überschüssiger flüssiger Sauerstoff vorrätig ist, wird erfindungsgemäß,wie folgt verfahren:Here is a small, highly enriched one with krypton and xenon Partial stream separated and through line 18 of a plant, not shown, for the extraction of Krypton and Xenon supplied. The main amount becomes gaseous through lines 19 and 23 of the barrier column 20 fed. In this, the krypton-free liquid oxygen from the low-pressure column 9 is fed through line 21 and valve 22 is withdrawn, via some trays that in the oxygen gas which is supplied via line 19 is washed out, still contained krypton. The same treatment is given to that through line 23 from the low pressure column 9 withdrawn gaseous oxygen allocated. The liquid accumulating at the bottom of the barrier column 20 Oxygen is passed back into the bottom of the low pressure column 9 through line 24. Through this condenser circuit there is also a dangerous accumulation of hydrocarbons at the bottom of the low pressure column 9 avoided, since the hydrocarbons are also continuously removed through line 16 and in the krypton-xenon enrichment system 17 can be removed. From the barrier column 20, gaseous oxygen is generated through line 25 withdrawn, heated in the heat exchangers 2 and removed as a product of the system. If now an increased There is demand for liquid nitrogen and excess liquid oxygen is available according to the invention, proceed as follows:

Der externe flüssige Sauerstoff wird mit der Pumpe 26 über die Leitung 27 in den Kondensatorkreislauf gepumpt.The external liquid oxygen is supplied with the pump 26 pumped via line 27 into the condenser circuit.

Gleichzeitig wird die Entspannungsturbine 5 um etwa den gleichen Betrag zurückgefahren. Die hierdurch eingesparte Stickstoffmenge kondensiert zusätzlich im Hauptkondensator 7 und wird durch Leitung 8 und Ventil 28 flüssig der Anlage entnommen. Die zu entnehmende Stickstoffmenge ist äquivalent der eingespeisten Sauerstoffmenge,At the same time, the expansion turbine 5 is reduced by approximately the same amount. The saved Amount of nitrogen also condenses in the main condenser 7 and becomes liquid through line 8 and valve 28 taken from the system. The amount of nitrogen to be withdrawn is equivalent to the amount of oxygen fed in,

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verringert um einen Betrag, der durch das Reduzieren der Entspannungsturbine 5 ausfällt. Von wesentlicher Bedeutung für die Sicherheit des Verfahrens ist der gleichzeitige Betrieb der Krypten-Xenon-Anreicherungsanlage 17, da mit dem durch Leitung 26 zugeführten externen flüssigen Sauerstoff zusätzlich Kohlenwasserstoffe und Krypton/Xenon in die Anlage gelangen. Diese werden, wie beschrieben, in der Krypton-Xenon-Anreicherungsanlage 17 entfernt.
10
reduced by an amount that fails due to the reduction of the expansion turbine 5. The simultaneous operation of the crypt xenon enrichment system 17 is essential for the safety of the process, since hydrocarbons and krypton / xenon also get into the system with the external liquid oxygen supplied through line 26. As described, these are removed in the krypton-xenon enrichment system 17.
10

Ergänzend seien einige Zahlenangaben gemacht:In addition, some figures are given:

Druck in der Mitteldrucksäule 3: 6 bar. Druck in der Niederdrucksäule 9: 1,5 bar. Zugeführte Luftmenge: 155 000 Nm3/h.Pressure in the medium pressure column 3: 6 bar. Pressure in the low pressure column 9: 1.5 bar. Amount of air supplied: 155,000 Nm 3 / h.

Die Mengenbilanz für Krypton (stimmt annähernd auch für Methan) sieht folgendermaßen aus:The mass balance for krypton (also roughly correct for methane) looks like this:

Mit der Luft eingebracht: 155 000 Nm3/h χ 1,1 vpm =0,17 Nm3/h Kr. Das sind bei einer Ausbeute von 80% ca. 0,135 Nm3/h Kr.Introduced with the air: 155,000 Nm 3 / h χ 1.1 vpm = 0.17 Nm 3 / h Kr. With a yield of 80%, this is approx. 0.135 Nm 3 / h Kr.

Mit dem externen flüssigen Sauerstoff werden eingebracht: Ca. 0,01 Nm3/h Kr. Es stehen somit insgesamt 0,145 Nm3/h Kr zur Verfügung.With the external liquid oxygen, the following are introduced: Approximately 0.01 Nm 3 / h Kr. A total of 0.145 Nm 3 / h Kr is thus available.

Bei einer Entnahme von 1000 Nm3/h flüssigem Sauerstoff mit einem Gehalt von ca. 150 vpm Kr über Leitung 16 bleibt die Kryptonkonzentration am Boden der Niederdrucksäule 9 erhalten.With a withdrawal of 1000 Nm 3 / h of liquid oxygen with a content of approx. 150 vpm Kr via line 16, the krypton concentration at the bottom of the low-pressure column 9 is retained.

über Leitung 19 werden 900 Nm3/h gasförmiger Sauerstoff zurückgeführt. 900 Nm 3 / h of gaseous oxygen are returned via line 19.

Ba/HiBa / Hi

Ffm., 27.03.1980
35
Ffm., March 27, 1980
35

130044/0506130044/0506

Zusammenfassungsummary Verfahren zur Gewinnung von flüssigem StickstoffProcess for the production of liquid nitrogen

Bei einer nach dem Zweisäulenprinzip arbeitenden Luftzerlegungsanlage wird flüssiger Stickstoff durch arbeitsleistende Entspannung von gasförmigem Stickstoff erzeugt.In an air separation plant that works according to the two-column principle liquid nitrogen is generated by the work-performing expansion of gaseous nitrogen.

Zwecks Vergrößerung der Erzeugung von flüssigem Stickstoff wird externer flüssiger Sauerstoff in den Boden der Niederdrucksäule (9) eingespeist. Hierdurch kondensiert zusätzlich Stickstoff, der unterhalb des Hauptkondensators (7) aus der Mitteldrucksäule (3) abgezogen, wird. Zum Schutz gegen eine Kohlenwasserstoffanreicherung dient ein Kondensatorkrexslauf über eine Krypton-Xenon- Anreicherungsanlage (17).In order to increase the production of liquid nitrogen, external liquid oxygen is introduced into the soil the low pressure column (9) fed. This also condenses nitrogen below the main condenser (7) is withdrawn from the medium pressure column (3). To protect against hydrocarbon accumulation a condenser drain over a krypton-xenon enrichment system (17) is used.

Ba/Hi
EM 922
Ffm., 27.03.1980
Ba / Hi
EM 922
Ffm., March 27, 1980

130044/0506130044/0506

Claims (2)

AnsprücheExpectations Verfahren zur Gewinnung von flüssigem Stickstoff unter Verwendung der durch die Verdampfung von flüssigem Sauerstoff gewonnenen Kälte,
dadurch gekennzeichnet,
Process for the production of liquid nitrogen using the cold obtained by the evaporation of liquid oxygen,
characterized,
daß der flüssige Sauerstoff extern in den Boden der Niederdrucksäule (9) eines Zweisäulenapparates zur Luftzerlegung eingespeist wird, wo er im Hauptkondensator (7) gegen kondensierenden Stickstoff in der Mitteldrucksäule (3) verdampft, welcher unterhalb des Hauptkondensators aufgefangen und als Produkt der Anlage entnommen wird.that the liquid oxygen is externally in the bottom of the low pressure column (9) of a two-column apparatus Air separation is fed in, where it is in the main condenser (7) against condensing nitrogen in the Medium pressure column (3) evaporates, which is collected below the main condenser and as a product is taken from the system.
2. Verfahren nach Anspruch 1,
dadurch gekennzeichnet,
2. The method according to claim 1,
characterized,
daß aus dem Kopf der Mitteldrucksäule gasförmiger Stickstoff abgezogen, arbeitsleistend entspannt (5) und in Wärmeaustausch (2) mit der zu zerlegenden Luft gebracht wird.that gaseous nitrogen is withdrawn from the head of the medium pressure column, expanded to provide work (5) and is brought into heat exchange (2) with the air to be separated. 3, Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet,3, method according to claim 1 or 2, characterized, daß vom Boden der Niederdrucksäule flüssiger Sauerstoff abgezogen und nach Abtrennung eines an Krypton und Xenon angereicherten TeilStroms (18) in einer Krypton-Xenon-Anreicherungsanlage (17) in gasförmigem Zustand als Produkt abgeführt wird.that withdrawn from the bottom of the low pressure column liquid oxygen and after separation of one of krypton and xenon-enriched partial stream (18) in one Krypton-xenon enrichment system (17) is discharged in a gaseous state as a product. Ba/Hi
EM 922
Ffm., 27.03.1980
Ba / Hi
EM 922
Ffm., March 27, 1980
1300U/05061300U / 0506
DE19803016317 1980-04-28 1980-04-28 Liquid nitrogen prodn. process - feeds liquid oxygen into base of low pressure column for air decomposition Withdrawn DE3016317A1 (en)

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EP0640802A1 (en) * 1993-08-23 1995-03-01 The Boc Group, Inc. Air separation
DE3606967C2 (en) * 1985-03-11 2000-08-10 Air Liquide Process for the production of nitrogen under pressure and plant for carrying out the process
EP0628778B2 (en) 1993-06-07 2001-03-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and high pressure gas supply unit for an air constituent consuming installation

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DE3606967C2 (en) * 1985-03-11 2000-08-10 Air Liquide Process for the production of nitrogen under pressure and plant for carrying out the process
EP0628778B2 (en) 1993-06-07 2001-03-21 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Process and high pressure gas supply unit for an air constituent consuming installation
EP0640802A1 (en) * 1993-08-23 1995-03-01 The Boc Group, Inc. Air separation
AU670387B2 (en) * 1993-08-23 1996-07-11 Boc Group, Inc., The Pumped liquid oxygen method and apparatus

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