EP0834711A2 - Process and apparatus for the production of high purity nitrogen - Google Patents
Process and apparatus for the production of high purity nitrogen Download PDFInfo
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- EP0834711A2 EP0834711A2 EP97117183A EP97117183A EP0834711A2 EP 0834711 A2 EP0834711 A2 EP 0834711A2 EP 97117183 A EP97117183 A EP 97117183A EP 97117183 A EP97117183 A EP 97117183A EP 0834711 A2 EP0834711 A2 EP 0834711A2
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- Prior art keywords
- column
- nitrogen
- pure nitrogen
- pressure column
- fraction
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04709—Producing crude argon in a crude argon column as an auxiliary column system in at least a dual pressure main column system
- F25J3/04715—The auxiliary column system simultaneously produces oxygen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
- F25J2200/06—Processes or apparatus using separation by rectification in a dual pressure main column system in a classical double column flow-sheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/34—Processes or apparatus using separation by rectification using a side column fed by a stream from the low pressure column
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
Definitions
- the invention relates to a method for obtaining high-purity nitrogen by Cryogenic air separation, in which cleaned and compressed air through Rectification in a column consisting of a pressure column and a low pressure column Double column is disassembled, with pressure column and low pressure column in Heat exchange relationship.
- the process uses a nitrogen rich Fraction from the pressure column introduced into a pure nitrogen column, part of the Head fraction of the pure nitrogen column condensed by indirect heat exchange and at the head of the pure nitrogen column containing a more volatile components Fraction deducted.
- EP-299364-B1 therefore proposed an additional pure nitrogen column to connect to the pressure column, which is used to discharge the more volatile Components.
- the pure nitrogen column is designed as a reinforcement column, whose bottom liquid is returned to the pressure column.
- the highly pure Nitrogen product is withdrawn from the pressure column. This method is suitable the enrichment of helium and neon in the nitrogen product compared to one to significantly reduce ordinary double-column processes.
- the lowest possible content of volatile components in high-purity nitrogen also limited in this process by their concentration in the feed air.
- This object is achieved in that at least one theoretical or practical bottom below the point where the nitrogen-rich fraction from the Pressure column is introduced into the pure nitrogen column, high purity nitrogen as a product is withdrawn from the pure nitrogen column.
- the pure nitrogen column therefore has a stripping section, which is used for further depletion especially of helium, neon and optionally hydrogen.
- This can basically have any number of theoretical floors; it can in principle, any low concentration of volatile components can be achieved, especially one that is below that of the feed air.
- high purity nitrogen with a residual content of less than 1 ppb of more volatile impurities can be obtained.
- the more volatile Shares, especially helium, neon and possibly hydrogen, are on the head deducted from the pure nitrogen column. The deduction can be made directly via the Mass transfer elements of the pure nitrogen column or at the liquefaction room of the Head capacitor of the pure nitrogen column can be arranged.
- the pure nitrogen column has, for example, 3 to 10, preferably 5 to 8 theoretical plates.
- the Pure nitrogen column for example 2 to 8, preferably 2 to 3 theoretical plates be provided.
- the nitrogen-rich fraction is preferably gaseous in the pure nitrogen column introduced.
- At least part of the bottom liquid of the pure nitrogen column evaporated by indirect heat exchange.
- the swamp heater of the Pure nitrogen column can be felt or preferably latent by transfer Heat can be operated from any suitable heating medium.
- air under pressure or the top fraction of a column are suitable for Separation of argon and nitrogen.
- the method has at least one theoretical or practical bottom below where the nitrogen-rich fraction is removed, a nitrogen-rich liquid is taken and as a liquid product withdrawn and / or is given as a return to the low pressure column.
- a nitrogen-rich liquid is taken and as a liquid product withdrawn and / or is given as a return to the low pressure column.
- the Section in the pressure column between these two points is in itself from EP-299364-B1 known and has a higher reflux ratio than the one below Part of the pressure column. This will cause the rising gas to turn on in this section Depleted of carbon monoxide, so that the feed fraction for the pure nitrogen column and thus the product of the pressure column also has a particularly low content Have carbon monoxide.
- the high-purity nitrogen can be liquid and / or gaseous from the pure nitrogen column deducted, a particularly low residual volatile However, components can be reached in liquid form when removed.
- the head cooling of the pure nitrogen column can also be carried out by any suitable medium be made.
- An oxygen-enriched fraction is preferably produced taken from the pressure column and in the indirect heat exchange, in which a part the top fraction of the pure nitrogen column condenses, at least partially evaporates.
- one is connected to the low pressure column Pure oxygen column produces a highly pure oxygen product, the Bottom fraction of the pure oxygen column in the indirect heat exchange, in which a part of the top fraction of the pure nitrogen column condenses, at least partially is evaporated.
- Both types of head cooling of the pure nitrogen column are in the EP-299364-B1 shown in detail.
- the fraction from the pure nitrogen column containing the more volatile components can be introduced into a further separation device, which is used to extract helium and / or neon is used.
- the pure nitrogen column of the invention particularly high proportion of the helium and / or neon contained in the air in the Head fraction smuggled, especially when others if necessary existing drains for volatile components (e.g. on Top condenser of the pressure column) also in the separator for the extraction of Helium and / or neon are led.
- the particularly high purity of the Nitrogen product results in a high yield of helium and / or neon.
- a conventional double column 1 for Air separation indicated consisting of a pressure column 2, a low pressure column 3 and a main capacitor (first KDV) 4. Air rising in the pressure column is enriched with nitrogen and volatile components.
- Bottom liquid of the low pressure column 3 partially or completely condensed. This liquefaction is preferably carried out essentially completely, a small non-condensed portion removed via a drain line 8 and discarded or mixed with another residual stream (e.g. stream 12).
- Another part 9 of the top gas 5 is introduced into a pure nitrogen column 10.
- a pure nitrogen column 10 In the exemplary embodiment, there are 3 theoretical ones above the feed point Floors.
- a second KDV 11 is arranged above it, in which the top fraction of the Pure nitrogen column 10 is condensed by indirect heat exchange. Of the fraction 12 remaining in gaseous form contains helium, neon and optionally hydrogen, which are kept away from the nitrogen product.
- the insert fraction 9 for the pure nitrogen column contains a further 8 theoretical ones Floors.
- the content of volatile components in the nitrogen-rich fraction 9 is still about 53 ppm, to about less than 0.1 ppm reduced.
- Liquid high-purity nitrogen is the product 13 from the sump Pure nitrogen column 10 deducted.
- the sump heater (third condenser evaporator) 14 of the pure nitrogen column is, for example, with a partial flow 15 of Operating air operated, which thus condenses at least partially.
- the condensed Air 16 can then be fed into the pressure column 2.
- Part of the liquid flowing down in the pure nitrogen column is at the level of Feeding the nitrogen-rich fraction 9 withdrawn via a line 17 and to Head of the pressure column 2 returned.
- the one taken directly from the pressure column In the example nitrogen becomes 15 theoretical soils below the head removed (18) and fed to the low pressure column 3 as a return.
- a part of Pressure column nitrogen 18 can also be obtained as a liquid product.
- the The main component of the invention is high-purity oxygen.
- an oxygen-rich fraction 20 removed, which is low in volatile components in an additional column 21 introduced, which is designed as a side column to the low pressure column 3 and at Demand can be designed as a raw argon column.
- the additional column 21 becomes one more fraction 22 depleted in less volatile components and one Pure oxygen column 19 abandoned as a return.
- the head cooling 11 of the pure nitrogen column 10, for example by evaporating relaxed sump liquid can be carried out from the pressure column (see Figure 3 from EP-299364-B1). With simultaneous pure oxygen production in one Pure oxygen column 19, however, it is favorable to the oxygen and Integrate nitrogen purification by the second condenser-evaporator 11 serves at the same time as a sump heater for the pure oxygen column 19. Details of the Purest oxygen production and its integration with the purest nitrogen production can be found in EP-299364-B1 (see in particular FIG. 4).
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- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
Abstract
Description
Die Erfindung betrifft ein Verfahren zur Gewinnung von hochreinem Stickstoff durch Tieftemperaturzerlegung von Luft, bei dem gereinigte und verdichtete Luft durch Rektifikation in einer aus einer Drucksäule und einer Niederdrucksäule bestehenden Doppelsäule zerlegt wird, wobei Drucksäule und Niederdrucksäule in Wärmeaustauschbeziehung stehen. Bei dem Verfahren wird eine stickstoffreiche Fraktion aus der Drucksäule in eine Reinstickstoffsäule eingeführt, ein Teil der Kopffraktion der Reinstickstoffsäule durch indirekten Wärmeaustausch kondensiert und am Kopf der Reinstickstoffsäule eine leichterflüchtige Komponenten enthaltende Fraktion abgezogen.The invention relates to a method for obtaining high-purity nitrogen by Cryogenic air separation, in which cleaned and compressed air through Rectification in a column consisting of a pressure column and a low pressure column Double column is disassembled, with pressure column and low pressure column in Heat exchange relationship. The process uses a nitrogen rich Fraction from the pressure column introduced into a pure nitrogen column, part of the Head fraction of the pure nitrogen column condensed by indirect heat exchange and at the head of the pure nitrogen column containing a more volatile components Fraction deducted.
Bei einem üblichen Doppelsäulenverfahren zur Gewinnung von Stickstoff und Sauerstoff aus Luft wird das Stickstoffprodukt vom Kopf der Niederdrucksäule und/oder der Drucksäule abgezogen. In diesem Stickstoffprodukt sind damit sämtliche Luftkomponenten enthalten, die leichterflüchtig als Stickstoff sind, insbesondere Helium, Neon und gegebenenfalls Wasserstoff.In a conventional double column process for the production of nitrogen and Oxygen from air becomes the nitrogen product from the top of the low pressure column and / or the pressure column deducted. So there are all in this nitrogen product Contain air components that are more volatile than nitrogen, in particular Helium, neon and possibly hydrogen.
In der EP-299364-B1 wurde daher vorgeschlagen, eine zusätzliche Reinstickstoffsäule mit der Drucksäule zu verbinden, die zur Ausschleusung der leichterflüchtigen Komponenten dient. Die Reinstickstoffsäule ist als Verstärkungssäule ausgebildet, deren Sumpfflüssigkeit wieder in die Drucksäule zurückgeleitet wird. Das hochreine Stickstoffprodukt wird aus der Drucksäule abgezogen. Dieses Verfahren ist geeignet, die Anreicherung von Helium und Neon im Stickstoffprodukt gegenüber einem gewöhnlichen Doppelsäulenverfahren wesentlich zu verringern. Allerdings ist der geringstmögliche Gehalt an leichterflüchtigen Komponenten im hochreinen Stickstoff auch bei diesem Verfahren durch deren Konzentration in der Einsatzluft beschränkt.EP-299364-B1 therefore proposed an additional pure nitrogen column to connect to the pressure column, which is used to discharge the more volatile Components. The pure nitrogen column is designed as a reinforcement column, whose bottom liquid is returned to the pressure column. The highly pure Nitrogen product is withdrawn from the pressure column. This method is suitable the enrichment of helium and neon in the nitrogen product compared to one to significantly reduce ordinary double-column processes. However, the lowest possible content of volatile components in high-purity nitrogen also limited in this process by their concentration in the feed air.
Der Erfindung liegt daher die Aufgabe zugrunde, ein Verfahren der eingangs genannten Art und eine entsprechende Vorrichtung zu entwickeln, die eine besonders hohe Reinheit im hochreinen Stickstoffprodukt, insbesondere einen besonders niedrigen Gehalt an leichterflüchtigen Komponenten ermöglichen.The invention is therefore based on the object of a method of the beginning mentioned type and to develop a corresponding device that a particularly high purity in the high-purity nitrogen product, especially one particularly allow low content of volatile components.
Diese Aufgabe wird dadurch gelöst, daß mindestens einen theoretischen oder praktischen Boden unterhalb der Stelle, an der die stickstoffreiche Fraktion aus der Drucksäule in die Reinstickstoffsäule eingeführt wird, hochreiner Stickstoff als Produkt aus der Reinstickstoffsäule abgezogen wird.This object is achieved in that at least one theoretical or practical bottom below the point where the nitrogen-rich fraction from the Pressure column is introduced into the pure nitrogen column, high purity nitrogen as a product is withdrawn from the pure nitrogen column.
Die Reinstickstoffsäule weist also einen Abtriebsteil auf, der zur weiteren Abreicherung insbesondere von Helium, Neon und gegebenenfalls Wasserstoff dient. Dieser kann grundsätzlich eine beliebig hohe Zahl von theoretischen Böden aufweisen; es kann also prinzipiell eine beliebig niedrige Konzentration an leichterflüchtigen Komponenten erreicht werden, insbesondere eine, die unterhalb als derjenigen der Einsatzluft liegt. Beispielsweise ist kann hochreiner Stickstoff mit einem Restgehalt von weniger als 1 ppb an leichterflüchtigen Verunreinigungen gewonnen werden. Die leichterflüchtigen Anteile, insbesondere Helium, Neon und gegebenenfalls Wasserstoff, werden am Kopf der Reinstickstoffsäule abgezogen. Der Abzug kann unmittelbar über den Stoffaustauschelementen der Reinstickstoffsäule oder am Verflüssigungsraum des Kopfkondensators der Reinstickstoffsäule angeordnet sein.The pure nitrogen column therefore has a stripping section, which is used for further depletion especially of helium, neon and optionally hydrogen. This can basically have any number of theoretical floors; it can in principle, any low concentration of volatile components can be achieved, especially one that is below that of the feed air. For example, high purity nitrogen with a residual content of less than 1 ppb of more volatile impurities can be obtained. The more volatile Shares, especially helium, neon and possibly hydrogen, are on the head deducted from the pure nitrogen column. The deduction can be made directly via the Mass transfer elements of the pure nitrogen column or at the liquefaction room of the Head capacitor of the pure nitrogen column can be arranged.
Zwischen Einleitung der stickstoffreiche Fraktion aus der Drucksäule und Abzug des hochreinen Stickstoffprodukts weist die Reinstickstoffsäule beispielsweise 3 bis 10, vorzugsweise 5 bis 8 theoretische Böden auf. Oberhalb der Zuspeisestelle kann die Reinstickstoffsäule beispielsweise 2 bis 8, vorzugsweise 2 bis 3 theoretische Böden vorgesehen sein.Between the introduction of the nitrogen-rich fraction from the pressure column and the withdrawal of the high purity nitrogen product, the pure nitrogen column has, for example, 3 to 10, preferably 5 to 8 theoretical plates. Above the feed point, the Pure nitrogen column, for example 2 to 8, preferably 2 to 3 theoretical plates be provided.
Bei der Erfindung können in der Reinstickstoffsäule und den übrigen Kolonnen beispielsweise Böden, Füllkörper, geordnete Packung oder eine beliebige Kombination verschiedener Typen als Stoffaustauschelemente eingesetzt werden.In the invention can in the pure nitrogen column and the other columns for example bottoms, packing, orderly packing or any combination different types can be used as mass transfer elements.
Die stickstoffreiche Fraktion wird vorzugsweise gasförmig in die Reinstickstoffsäule eingeführt.The nitrogen-rich fraction is preferably gaseous in the pure nitrogen column introduced.
Vorzugsweise wird mindestens ein Teil der Sumpfflüssigkeit der Reinstickstoffsäule durch indirekten Wärmeaustausch verdampft. Die Sumpfheizung der Reinstickstoffsäule kann durch Übertragung von fühlbarer oder vorzugsweise latenter Wärme von jedem geeigneten Heizmedium betrieben werden. Vorzugsweise das Heizmittel durch eine Luftkomponente oder durch ein Gemisch aus Luftgasen gebildet und kondensiert bei dem indirekten Wärmeaustausch. Als Heizmittel besonders geeignet sind unter Druck stehende Luft oder die Kopffraktion einer Kolonne zur Trennung von Argon und Stickstoff. Preferably at least part of the bottom liquid of the pure nitrogen column evaporated by indirect heat exchange. The swamp heater of the Pure nitrogen column can be felt or preferably latent by transfer Heat can be operated from any suitable heating medium. Preferably that Heating means formed by an air component or by a mixture of air gases and condenses in indirect heat exchange. Especially as a heating medium air under pressure or the top fraction of a column are suitable for Separation of argon and nitrogen.
Es ist günstig, wenn bei dem Verfahren mindestens einen theoretischen oder praktischen Boden unterhalb der Stelle, an der die stickstoffreiche Fraktion entnommen wird, eine stickstoffreiche Flüssigkeit entnommen und als Flüssigprodukt abgezogen und/oder als Rücklauf auf die Niederdrucksäule aufgegeben wird. Der Abschnitt in der Drucksäule zwischen diesen beiden Stellen ist an sich aus der EP-299364-B1 bekannt und weist ein höheres Rücklaufverhältnis als der darunterliegende Teil der Drucksäule auf. Dadurch wird das aufsteigende Gas in diesem Abschnitt an Kohlenmonoxid abgereichert, so daß die Einsatzfraktion für die Reinstickstoffsäule und damit auch das Produkt der Drucksäule einen besonders geringen Gehalt an Kohlenmonoxid aufweisen.It is advantageous if the method has at least one theoretical or practical bottom below where the nitrogen-rich fraction is removed, a nitrogen-rich liquid is taken and as a liquid product withdrawn and / or is given as a return to the low pressure column. Of the Section in the pressure column between these two points is in itself from EP-299364-B1 known and has a higher reflux ratio than the one below Part of the pressure column. This will cause the rising gas to turn on in this section Depleted of carbon monoxide, so that the feed fraction for the pure nitrogen column and thus the product of the pressure column also has a particularly low content Have carbon monoxide.
Der hochreine Stickstoff kann flüssig und/oder gasförmig aus der Reinstickstoffsäule abgezogen werden, ein besonders niedriger Restgehalt an leichterflüchtigen Komponenten kann jedoch beim Abzug in flüssiger Form erreicht werden.The high-purity nitrogen can be liquid and / or gaseous from the pure nitrogen column deducted, a particularly low residual volatile However, components can be reached in liquid form when removed.
Die Kopfkühlung der Reinstickstoffsäule kann ebenfalls durch jedes geeignete Medium vorgenommen werden. Vorzugsweise wird eine sauerstoffangereicherte Fraktion aus der Drucksäule entnommen und bei dem indirekten Wärmeaustausch, bei dem ein Teil der Kopffraktion der Reinstickstoffsäule kondensiert, mindestens teilweise verdampft. Alternativ oder ergänzend dazu wird in einer mit der Niederdrucksäule verbundenen Reinsauerstoffsäule ein hochreines Sauerstoffprodukt erzeugt, wobei die Sumpffraktion der Reinsauerstoffsäule bei dem indirekten Wärmeaustausch, bei dem ein Teil der Kopffraktion der Reinstickstoffsäule kondensiert, mindestens teilweise verdampft wird. Beide Varianten der Kopfkühlung der Reinstickstoffsäule sind in der EP-299364-B1 im Detail dargestellt.The head cooling of the pure nitrogen column can also be carried out by any suitable medium be made. An oxygen-enriched fraction is preferably produced taken from the pressure column and in the indirect heat exchange, in which a part the top fraction of the pure nitrogen column condenses, at least partially evaporates. Alternatively or in addition, one is connected to the low pressure column Pure oxygen column produces a highly pure oxygen product, the Bottom fraction of the pure oxygen column in the indirect heat exchange, in which a part of the top fraction of the pure nitrogen column condenses, at least partially is evaporated. Both types of head cooling of the pure nitrogen column are in the EP-299364-B1 shown in detail.
Die leichterflüchtige Komponenten enthaltende Fraktion aus der Reinstickstoffsäule kann in eine weitere Trenneinrichtung eingeleitet wird, die zur Gewinnung von Helium und/oder Neon dient. In diesem Fall wird in der Reinstickstoffsäule der Erfindung besonders hoher Anteil des in der Luft enthaltenen Heliums und/oder Neons in die Kopffraktion geschleust, insbesondere dann, wenn auch andere gegebenenfalls vorhandene Ablässe für leichterflüchtige Komponenten (beispielsweise am Kopfkondensator der Drucksäule) ebenfalls in die Trenneinrichtung zur Gewinnung von Helium und/oder Neon geführt werden. Die besonders hohe Reinheit des Stickstoffprodukts resultiert in einer hohen Ausbeute an Helium und/oder Neon. The fraction from the pure nitrogen column containing the more volatile components can be introduced into a further separation device, which is used to extract helium and / or neon is used. In this case, the pure nitrogen column of the invention particularly high proportion of the helium and / or neon contained in the air in the Head fraction smuggled, especially when others if necessary existing drains for volatile components (e.g. on Top condenser of the pressure column) also in the separator for the extraction of Helium and / or neon are led. The particularly high purity of the Nitrogen product results in a high yield of helium and / or neon.
Vorzugsweise wird ein Teil der in der Reinstickstoffsäule herabfließenden Flüssigkeit an einer Zwischenstelle der Reinstickstoffsäule abgezogen und in die Drucksäule eingeleitet. Dadurch kann auch bei relativ geringer Menge an hochreinem Stickstoffprodukt eine wirksame Ausschleusung der leichterflüchtigen Komponenten bewirkt werden, ohne daß dazu ein besonders hoher Umsatz am Sumpfverdampfer der Reinstickstoffsäule notwendig wäre. Der Flüssigkeitsabzug liegt vorzugsweise etwa auf gleicher Höhe wie die Einspeisung der stickstoffreichen Fraktion.Part of the liquid flowing down in the pure nitrogen column is preferably withdrawn at an intermediate point of the pure nitrogen column and into the pressure column initiated. This means that even with a relatively small amount of high-purity Nitrogen product an effective discharge of the more volatile components be effected without a particularly high conversion on the bottom evaporator the pure nitrogen column would be necessary. The liquid drain is preferably approximately at the same level as the feed of the nitrogen-rich fraction.
Die Erfindung bezieht sich außerdem auf eine Vorrichtung gemäß Patentanspruch 9.The invention also relates to a device according to claim 9.
Die Erfindung sowie weitere Einzelheiten der Erfindung werden im folgenden anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispiels näher erläutert. Die in der Zeichnung nicht ausdrücklich gezeigten Verfahrensschritte und Vorrichtungsteile können in jeder dem Fachmann geläufigen Form ausgeführt werden, insbesondere so wie sie in den Figuren 3 und 4 und der Beschreibung der EP-299364-B1 erläutert werden.The invention and further details of the invention are described below an embodiment shown schematically in the drawing explained. The process steps and not explicitly shown in the drawing Device parts can be made in any form familiar to the person skilled in the art, in particular as shown in Figures 3 and 4 and the description of EP-299364-B1 are explained.
Auf der rechten Seite der Zeichnung ist eine konventionelle Doppelsäule 1 zur
Luftzerlegung angedeutet, die aus einer Drucksäule 2, einer Niederdrucksäule 3 und
einem Hauptkondensator (ersten KDV) 4 besteht. In der Drucksäule aufsteigende Luft
wird an Stickstoff und leichterflüchtigen Komponenten angereichert. Kopfgas 5 der
Drucksäule wird zu einem Teil 6 im Hauptkondensator 4 gegen verdampfende
Sumpfflüssigkeit der Niederdrucksäule 3 teilweise oder vollständig kondensiert.
Vorzugsweise wird diese Verflüssigung im wesentlichen vollständig durchgeführt,
wobei ein kleiner nicht kondensierter Anteil über eine Ablaßleitung 8 entnommen und
verworfen oder einem anderen Reststrom (beispielsweise Strom 12) zugemischt wird.On the right side of the drawing is a conventional double column 1 for
Air separation indicated, consisting of a pressure column 2, a low pressure column 3 and
a main capacitor (first KDV) 4. Air rising in the pressure column
is enriched with nitrogen and volatile components. Top gas 5 the
Pressure column becomes
Ein anderer Teil 9 des Kopfgases 5 wird in eine Reinstickstoffsäule 10 eingeführt.
Oberhalb der Einspeisestelle befinden sich in dem Ausführungsbeispiel 3 theoretische
Böden. Darüber ist ein zweiter KDV 11 angeordnet, in dem die Kopffraktion der
Reinstickstoffsäule 10 durch indirekten Wärmeaustausch kondensiert wird. Der
gasförmig verbliebene Anteil 12 enthält Helium, Neon und gegebenenfalls Wasserstoff,
die damit aus dem Stickstoffprodukt ferngehalten werden. Unterhalb der Einspeisung
der Einsatzfraktion 9 für die Reinstickstoffsäule befinden sich weitere 8 theoretische
Böden. Dadurch wird der Gehalt an leichterflüchtigen Komponenten, der in der
stickstoffreichen Fraktion 9 noch etwa 53 ppm beträgt, auf etwa weniger als 0,1 ppm
vermindert. Flüssiger hochreiner Stickstoff wird als Produkt 13 vom Sumpf der
Reinstickstoffsäule 10 abgezogen. Die Sumpfheizung (dritter Kondensator-Verdampfer)
14 der Reinstickstoffsäule wird beispielsweise mit einem Teilstrom 15 der
Einsatzluft betrieben, die damit mindestens teilweise kondensiert. Die kondensierte
Luft 16 kann anschließend in die Drucksäule 2 eingespeist werden.Another part 9 of the top gas 5 is introduced into a pure nitrogen column 10.
In the exemplary embodiment, there are 3 theoretical ones above the feed point
Floors. A second KDV 11 is arranged above it, in which the top fraction of the
Pure nitrogen column 10 is condensed by indirect heat exchange. Of the
Ein Teil der in der Reinstickstoffsäule herabfließenden Flüssigkeit wird auf Höhe der
Zuspeisung der stickstoffreichen Fraktion 9 über eine Leitung 17 abgezogen und zum
Kopf der Drucksäule 2 zurückgeführt. Der direkt der Drucksäule entnommene
Stickstoff wird in dem Beispiel 15 theoretische Böden unterhalb des Kopfes
entnommen (18) und der Niederdrucksäule 3 als Rücklauf zugeführt. Ein Teil der
Drucksäulenstickstoffs 18 kann auch als Flüssigprodukt gewonnen werden.Part of the liquid flowing down in the pure nitrogen column is at the level of
Feeding the nitrogen-rich fraction 9 withdrawn via a
Bei dem Ausführungsbeispiel wird zusätzlich zur Reinststickstoffgewinnung, die
Hauptbestandteil der Erfindung ist, hochreiner Sauerstoff gewonnen. Dazu wird der
Niederdrucksäule 3 oberhalb ihres Sumpfes eine sauerstoffreiche Fraktion 20
entnommen, die arm an schwererflüchtigen Komponenten ist, in eine Zusatzsäule 21
eingeschleust, die als Seitenkolonne zur Niederdrucksäule 3 ausgebildet ist und bei
Bedarf als Rohargonsäule ausgebildet sein kann. Der Zusatzsäule 21 wird eine weiter
an schwererflüchtigen Anteilen abgereicherte Fraktion 22 entnommen und einer
Reinsauerstoffsäule 19 als Rücklauf aufgegeben.In the embodiment, in addition to the purest nitrogen production, the
The main component of the invention is high-purity oxygen. For this the
Low pressure column 3 above its sump an oxygen-
Die Kopfkühlung 11 der Reinstickstoffsäule 10 beispielsweise durch Verdampfen von entspannter Sumpfflüssigkeit aus der Drucksäule durchgeführt werden (siehe Figur 3 von EP-299364-B1). Bei gleichzeitiger Reinstsauerstoffgewinnung in einer Reinsauerstoffsäule 19 ist es jedoch günstig, die Sauerstoff- und die Stickstoffreinigung zu integrieren, indem der zweite Kondensator-Verdampfer 11 gleichzeitig als Sumpfheizung der Reinsauerstoffsäule 19 dient. Einzelheiten zu der Reinstsauerstoffgewinnung und ihrer Integration mit der Reinststickstoffgewinnung sind der EP-299364-B1 zu entnehmen (siehe insbesondere Figur 4).The head cooling 11 of the pure nitrogen column 10, for example by evaporating relaxed sump liquid can be carried out from the pressure column (see Figure 3 from EP-299364-B1). With simultaneous pure oxygen production in one Pure oxygen column 19, however, it is favorable to the oxygen and Integrate nitrogen purification by the second condenser-evaporator 11 serves at the same time as a sump heater for the pure oxygen column 19. Details of the Purest oxygen production and its integration with the purest nitrogen production can be found in EP-299364-B1 (see in particular FIG. 4).
Claims (9)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19640711 | 1996-10-02 | ||
DE1996140711 DE19640711A1 (en) | 1996-10-02 | 1996-10-02 | Method and device for obtaining high-purity nitrogen |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0834711A2 true EP0834711A2 (en) | 1998-04-08 |
EP0834711A3 EP0834711A3 (en) | 1998-07-15 |
Family
ID=7807713
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97117183A Withdrawn EP0834711A3 (en) | 1996-10-02 | 1997-10-02 | Process and apparatus for the production of high purity nitrogen |
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EP (1) | EP0834711A3 (en) |
DE (1) | DE19640711A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1001236A2 (en) * | 1998-11-11 | 2000-05-17 | Linde Aktiengesellschaft | Process for producing ultra pure nitrogen |
US8661847B2 (en) | 2008-08-11 | 2014-03-04 | Robert Brockmann | Production of a clean gas, in particular for testing a pressurized construction component for leaks |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19819263C2 (en) * | 1998-04-30 | 2003-08-21 | Linde Ag | Process and device for the production of pressurized nitrogen |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3079759A (en) * | 1961-03-22 | 1963-03-05 | Air Prod & Chem | Separation of gaseous mixtures |
EP0299364A2 (en) * | 1987-07-09 | 1989-01-18 | Linde Aktiengesellschaft | Process and apparatus for air separation by rectification |
US5123947A (en) * | 1991-01-03 | 1992-06-23 | Air Products And Chemicals, Inc. | Cryogenic process for the separation of air to produce ultra high purity nitrogen |
-
1996
- 1996-10-02 DE DE1996140711 patent/DE19640711A1/en not_active Withdrawn
-
1997
- 1997-10-02 EP EP97117183A patent/EP0834711A3/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3079759A (en) * | 1961-03-22 | 1963-03-05 | Air Prod & Chem | Separation of gaseous mixtures |
EP0299364A2 (en) * | 1987-07-09 | 1989-01-18 | Linde Aktiengesellschaft | Process and apparatus for air separation by rectification |
US5123947A (en) * | 1991-01-03 | 1992-06-23 | Air Products And Chemicals, Inc. | Cryogenic process for the separation of air to produce ultra high purity nitrogen |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP1001236A2 (en) * | 1998-11-11 | 2000-05-17 | Linde Aktiengesellschaft | Process for producing ultra pure nitrogen |
EP1001236A3 (en) * | 1998-11-11 | 2000-11-08 | Linde Aktiengesellschaft | Process for producing ultra pure nitrogen |
US6276172B1 (en) | 1998-11-11 | 2001-08-21 | Linde Aktiengesellschaft | Process for producing ultrapure nitrogen |
US8661847B2 (en) | 2008-08-11 | 2014-03-04 | Robert Brockmann | Production of a clean gas, in particular for testing a pressurized construction component for leaks |
Also Published As
Publication number | Publication date |
---|---|
DE19640711A1 (en) | 1998-04-09 |
EP0834711A3 (en) | 1998-07-15 |
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