DE10332863A1 - Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream - Google Patents
Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream Download PDFInfo
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- DE10332863A1 DE10332863A1 DE10332863A DE10332863A DE10332863A1 DE 10332863 A1 DE10332863 A1 DE 10332863A1 DE 10332863 A DE10332863 A DE 10332863A DE 10332863 A DE10332863 A DE 10332863A DE 10332863 A1 DE10332863 A1 DE 10332863A1
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- krypton
- xenon
- argon
- nitrogen
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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- 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
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- 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
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- 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
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- F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
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Abstract
Description
Die Erfindung betrifft ein Verfahren gemäß dem Oberbegriff des Patentanspruchs 1, das zur Gewinnung von Krypton und/oder Xenon durch Tieftemperaturzerlegung von Luft dient.The invention relates to a method according to the generic term of claim 1, for the extraction of krypton and / or xenon by low-temperature decomposition of air.
Die Grundlagen der Tieftemperaturzerlegung von Luft im Allgemeinen sowie der Aufbau von Rektifiziersystemen zur Stickstoff-Sauerstoff-Trennung im Speziellen sind in der Monografie "Tieftemperaturtechnik" von Hausen/Linde (2. Auflage, 1985) und in einem Aufsatz von Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, Seite 35) beschrieben. Die Hochdrucksäule wird unter einem höheren Druck als die Niederdrucksäule betrieben; die beiden Säulen stehen vorzugsweise in Wärmeaustauschbeziehung zueinander, beispielsweise über einen Hauptkondensator, in dem Kopfgas der Hochdrucksäule gegen verdampfende Sumpfflüssigkeit der Niederdrucksäule verflüssigt wird. Das Rektifiziersystem der Erfindung kann als klassisches Doppelsäulensystem ausgebildet sein, aber auch als Drei- oder Mehrsäulensystem. Zusätzlich zu den Kolonnen zur Stickstoff-Sauerstoff-Trennung können weitere Vorrichtungen zur Gewinnung anderer Luftkomponenten, insbesondere von Edelgasen aufweisen, beispielsweise eine Argongewinnung.The basics of low temperature decomposition of Air in general and the construction of rectification systems for Nitrogen-oxygen separation in particular are in the monograph "Low temperature technology" by Hausen / Linde (2nd edition, 1985) and in an article by Latimer in Chemical Engineering Progress (Vol. 63, No.2, 1967, page 35). The high pressure column will under a higher one Pressure than the low pressure column operated; the two pillars are preferably in heat exchange relationship to each other, for example about a main condenser, in the top gas against the high pressure column evaporating swamp liquid the low pressure column liquefied becomes. The rectification system of the invention can be used as a classic double column system be designed, but also as a three or multi-column system. In addition to the columns for nitrogen-oxygen separation can be further Devices for extracting other air components, in particular of noble gases, for example argon production.
Das erzeugte Krypton-Xenon-Konzentrat kann an Ort und Stelle in weiteren Verfahrensschritten zu reinem Krypton und/oder Xenon getrennt werden. Alternativ wird es gespeichert, zum Beispiel in einem Flüssigtank, und an einem anderen Ort weiterverarbeitet.The krypton-xenon concentrate produced can on the spot in further process steps to pure krypton and / or xenon are separated. Alternatively, it is saved for example in a liquid tank, and processed at another location.
Bei dem bekannten und bei dem älteren Verfahren wird die Spülflüssigkeit aus dem ersten Kondensator-Verdampfer ohne konzentrationsverändernde Maßnahmen in die Krypton-Xenon-Anreicherungssäule geführt.In the known and in the older method becomes the rinsing liquid from the first condenser-evaporator without concentration-changing activities into the krypton-xenon enrichment column.
Der Erfindung liegt die Aufgabe zugrunde, das Verfahren weiter zu verbessern und insbesondere auf besonders wirtschaftliche Weise durchzuführen.The invention has for its object that Processes to be further improved and in particular to particularly economical ones Way to perform.
Diese Aufgabe wird dadurch gelöst; dass mindestens ein Teil der Spülflüssigkeit stromaufwärts der Krypton-Xenon-Anreicherungssäule einer Reinigung unterworfen wird, indem sie in eine Zusatzsäule eingeleitet wird und in der Zusatzsäule im Gegenstrom zu einem stickstoffarmen Gas geführt wird, wobei gereinigte Spülflüssigkeit aus der Zusatzsäule abgezogen und in die Krypton-Xenon-Anreicherungssäule eingeleitet wird.This solves this problem; that at least part of the rinsing liquid upstream of the Krypton-xenon enrichment column is subjected to cleaning by introducing it into an additional column will and in the additional column is led in countercurrent to a low-nitrogen gas, with purified rinse subtracted from the additional column and introduced into the krypton-xenon enrichment column becomes.
Im Rahmen der Erfindung hat sich herausgestellt, dass die Spülflüssigkeit aus dem ersten Kondensator-Verdampfer noch relativ viel Stickstoff enthält (beispielsweise etwa 20 bis 40 mol-%). Dieser Stickstoff gelangt bei den bekannten Verfahren in vollem Umfang in die Krypton-Xenon-Anreicherungssäule und in deren Kopfprodukt. Dies stellt Ballast für die Krypton-Xenon-Anreicherungssäule dar und verteuert damit die Krypton-Xenon-Gewinnung.Within the scope of the invention found that the rinsing liquid relatively much nitrogen from the first condenser-evaporator contains (for example about 20 to 40 mol%). This nitrogen arrives in the known methods in full in the krypton-xenon enrichment column and in their top product. This represents ballast for the krypton-xenon enrichment column and thus makes krypton-xenon production more expensive.
Mit Hilfe des erfindungsgemäßen Reinigungsschrittes wird der Stickstoffgehalt in der Spülflüssigkeit auf beispielsweise höchstens 1 mol-%; vorzugsweise höchstens 10 ppm verringert. Entsprechend vermindert sich die Menge der in der Krypton-Xenon-Anreicherungssäule eingeführten und dort zu verdampfenden Flüssigkeit. Außerdem vermindert sich der Stickstoffgehalt des Kopfgases der Krypton-Xenon-Anreicherungssäule erheblich. Falls diese wieder in das Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung eingeführt wird, verbessert dies die dortige Trennwirkung. Der Effekt ist insbesondere dann deutlich zu spüren, wenn dem Rektifiziersystem zur Stickstoff-Sauerstoff-Trennung eine Argongewinnung angeschlossen ist, und äußert sich in diesem Fall in einer besonders hohen Argonausbeute.With the help of the cleaning step according to the invention the nitrogen content in the rinsing liquid is, for example at the most 1 mol%; preferably at most 10 ppm reduced. The amount of in of the krypton-xenon enrichment column and introduced there liquid to be evaporated. Moreover the nitrogen content of the top gas of the krypton-xenon enrichment column decreases considerably. If this goes back into the rectification system for nitrogen-oxygen separation introduced this improves the separation effect there. The effect is special then clearly felt if the rectification system for nitrogen-oxygen separation produces argon is connected, and is expressed in in this case in a particularly high argon yield.
Die Zusatzsäule gemäß der Erfindung ist im Vergleich zu den übrigen Säulen des Systems sehr klein und damit kostengünstig. Sie braucht lediglich beispielsweise 4 bis 10, vorzugsweise 5 bis 7 theoretische oder praktische Böden aufzuweisen, vorzugsweise in Form klassischer Rektifizierböden, zum Beispiel in Form von Siebböden.The additional column according to the invention is compared to the rest columns of the system is very small and therefore inexpensive. It only needs, for example 4 to 10, preferably 5 to 7 theoretical or practical floors, preferably in the form of classic rectification trays, for example in the form of Sieve trays.
Unter einem "stickstoffarmen" Gas wird hier beispielsweise eine Fraktion verstanden, die maximal 10 mol-%, insbesondere maximal 1 mol-%, vorzugsweise maximal 1 ppm Stickstoff enthält.Under a "low nitrogen" gas a fraction is understood here, for example, which has a maximum of 10 mol%, in particular a maximum of 1 mol%, preferably a maximum of 1 ppm Contains nitrogen.
Das stickstoffarme Gas, das in der Zusatzsäule in Gegenstromkontakt mit der Spülflüssigkeit gebracht wird, kann aus jeder geeigneten Quelle innerhalb des Verfahrens stammen, zum Beispiel aus dem unteren Bereich der Niederdrucksäule. Vorzugsweise wird es jedoch aus dem oberen Bereich der Krypton-Xenon-Anreicherungssäule entnommen.The low nitrogen gas that is in the additional column brought into countercurrent contact with the rinsing liquid can be from any suitable source within the process originate, for example, from the lower area of the low pressure column. Preferably however, it is removed from the top of the krypton-xenon enrichment column.
Aus dem oberen Bereich der Krypton-Xenon-Anreicherungssäule wird vorzugsweise ein Kopfgas entnommen und mindestens zum Teil als Rückführgas in die Niederdrucksäule eingeleitet, um den darin enthaltenen Sauerstoff als Produkt zu gewinnen. Alternativ kann das Kopfgas der Krypton-Xenon-Anreicherungssäule direkt als Produkt abgeführt werden.A top gas is preferably withdrawn from the upper region of the krypton-xenon enrichment column and at least partially introduced as return gas into the low-pressure column in order to obtain the oxygen contained therein as a product. Alternatively, the top gas of the Krypton-Xe non-enrichment column can be discharged directly as a product.
Wie bereits erwähnt, kommen die Vorteile der Erfindung besonders stark zu Tragen, wenn das Verfahren eine Argongewinnung aufweist. Hierbei wird eine argonhaltige Fraktion aus der Niederdrucksäule in eine Rohargonrektifikation eingeleitet.As mentioned earlier, the benefits of Invention to be particularly strong when the process is an argon production having. Here, an argon-containing fraction from the low pressure column into a Raw argon rectification initiated.
Wie aus
Weil im Rahmen der Erfindung eine niedrige Stickstoffkonzentration in der Krypton-Xenon-Anreicherungssäule herrscht, muss das Rückführgas aus deren oberem Bereich nicht wie bei dem bekannten Verfahren relativ weit oben in die Niederdrucksäule eingeleitet werden, sondern es wird unterhalb des Argonübergangs eingeleitet, das heißt unterhalb der Stelle, an welcher der argonangereicherte Dampf für die Rohargonrektifikation entnommen wird. Hierdurch wird das Rücklaufverhältnis in dem unteren Teil der Niederdrucksäule verbessert und damit eine besonders hohe Argonausbeute erzielt. Die Einleitung des Rückführgases kann zum Beispiel unmittelbar oberhalb des Sumpfs der Niederdrucksäule vorgenommen werden.Because within the scope of the invention If the krypton-xenon enrichment column has a low nitrogen concentration, the recycle gas must be removed from it Upper area is not relatively wide as in the known method introduced into the low pressure column at the top be, but it is introduced below the argon transition, that is, below the place where the argon-enriched steam for crude argon rectification is removed. As a result, the reflux ratio in the lower part of the Low-pressure column improved and thus achieved a particularly high argon yield. The introduction of the return gas can for example be made directly above the bottom of the low pressure column become.
Um die Kopffraktion der Zusatzsäule für die weitere Trennung zu nutzen, ist es günstig, wenn ein stickstoffhaltiges Gas aus dem oberen Bereich der Zusatzsäule abgezogen und in die Niederdrucksäule eingeleitet wird, insbesondere an einer Zwischenstelle oberhalb des Argonübergangs.To the top fraction of the additional column for the further It's good to use separation, when a nitrogenous gas is withdrawn from the top of the additional column and introduced into the low pressure column is, especially at an intermediate point above the argon transition.
Wegen des niedrigen N2O-Gehalts im Sumpf der Niederdrucksäule kann die Erfindung besonders vorteilhaft in Verfahren und Vorrichtung angewendet werden, die einen Fallfilmverdampfer als Hauptkondensator aufweisen, das heißt wenn sauerstoffreiche Flüssigkeit aus dem unteren Abschnitt der Niederdrucksäule in dem Verdampfungsraum eines zweiten Kondensator-Verdampfers (Hauptkondensators) teilweise verdampft wird, wobei der zweite Kondensator-Verdampfer (Hauptkondensators) als Fallfilmverdampfer ausgebildet ist.Because of the low N 2 O content in the bottom of the low-pressure column, the invention can be used particularly advantageously in processes and apparatus which have a falling film evaporator as the main condenser, that is to say when oxygen-rich liquid from the lower section of the low-pressure column in the evaporation space of a second condenser-evaporator (Main condenser) is partially evaporated, the second condenser-evaporator (main condenser) being designed as a falling film evaporator.
Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von Krypton und/oder Xenon durch Tieftemperaturzerlegung von Luft gemäß den Patentansprüchen 9 beziehungsweise 10.The invention also relates to a Device for extracting krypton and / or xenon by cryogenic decomposition of air according to claims 9 and 10th
Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispiels näher erläutert.The invention and further details The invention are described below with reference to one in the drawing schematically illustrated embodiment explained in more detail.
Über
Leitung
Die sauerstoffangereicherte Sumpfflüssigkeit
Der erste Kondensator-Verdampfer
Verbleibende Flüssigkeit wird als "Spülflüssigkeit"
Die Krypton-Xenon-Anreicherungssäule
Vom Sumpf der Krypton-Xenon-Anreicherungssäule
Von der Niederdrucksäule
Der flüssige Sauerstoff
Mindestens ein Teil
Verdampfung und Anwärmung können beispielsweise
in indirektem Wärmeaustausch
mit einem Hochdruckluftstrom durchgeführt werden. Im Ausführungsbeispiel
wird dazu jedoch ein Stickstoff-Kreislauf eingesetzt, der gleichzeitig
zur Erzeugung von Verfahrenskälte
zum Ausgleich von Austausch- und Isolationsverlusten sowie zur Produktverflüssigung
dient. Hierbei ist das Linde-VARIPOX©-Verfahren
realisiert, das die Erzeugung variabler Mengen an Drucksauerstoff
bei stationärem
Betrieb des Rektifiziersystems erlaubt. Dieser Prozess ist in
Der Kreislauf wird durch einen Teil
Ein zweiter Teil
Über
eine Argonübergangs-Leitung
Am Kopf der zweiten Rohargonsäule
Gasförmig verbliebenen Rohargon
Zwischen den Blöcken
Claims (10)
Priority Applications (1)
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DE10332863A DE10332863A1 (en) | 2003-07-18 | 2003-07-18 | Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream |
Applications Claiming Priority (1)
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DE10332863A DE10332863A1 (en) | 2003-07-18 | 2003-07-18 | Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream |
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DE10332863A1 true DE10332863A1 (en) | 2004-02-26 |
Family
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DE10332863A Withdrawn DE10332863A1 (en) | 2003-07-18 | 2003-07-18 | Krypton and xenon recovery by low-temperature fractionation of air yields higher purity products and higher argon productivity, using low nitrogen content scrubbing liquid stream |
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2003
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