EP1001236A2 - Process for producing ultra pure nitrogen - Google Patents
Process for producing ultra pure nitrogen Download PDFInfo
- Publication number
- EP1001236A2 EP1001236A2 EP99122146A EP99122146A EP1001236A2 EP 1001236 A2 EP1001236 A2 EP 1001236A2 EP 99122146 A EP99122146 A EP 99122146A EP 99122146 A EP99122146 A EP 99122146A EP 1001236 A2 EP1001236 A2 EP 1001236A2
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- EP
- European Patent Office
- Prior art keywords
- column
- free
- nitrogen
- pressure column
- carbon monoxide
- 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.)
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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
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- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
- F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
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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
- F25J3/04084—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 nitrogen
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- F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S62/00—Refrigeration
- Y10S62/92—Carbon monoxide
Definitions
- the invention relates to a process for the production of ultra-pure nitrogen by Cryogenic air separation in a rectification system with at least one Rectification column, whereby compressed and cleaned feed air into a pressure column led, an oxygen-free pressure nitrogen fraction obtained from the pressure column, in a low pressure column and in the low pressure column carbon monoxide free Low pressure nitrogen is obtained as a top gas.
- the object of the invention is therefore to avoid this disadvantage and Reduce energy consumption.
- Another object of the invention is to demonstrate a method which either with a liquid pressure nitrogen fraction directly from the pressure column or is operated from a tank with liquid pressure column nitrogen.
- the oxygen-free pressurized nitrogen fraction is either withdrawn in liquid form from an upper region of the pressure column or is provided from a liquid tank with stored oxygen-free nitrogen and that the oxygen-free pressurized nitrogen fraction is expanded into the low-pressure column heated in its sump, steam rising in the low-pressure column formed and freed of carbon monoxide with the aid of a reflux at the top of the low-pressure column with ultra-pure nitrogen, drawn off at the top of the low-pressure column as carbon monoxide-free head gas and partially liquefied after a pressure increase and the liquefied part in a He-Ne-H 2 - heated in its sump
- the column is relaxed, from which the ultra-pure nitrogen is removed in liquid form.
- the ultra pure nitrogen is obtained in liquid form and is easier to transport in this form and therefore easier to distribute to customers become.
- the process can also be used universally. Because it can with Connection to an air separation plant (with or without liquid nitrogen tank) or only on a liquid nitrogen tank (with spatial separation from the air separation plant) be used. On an air separation plant with a liquid nitrogen tank also the ultra pure liquid nitrogen can be obtained without the Air separation plant is in operation.
- the carbon monoxide-free head gas and a head gas of the He-Ne-H 2 column can be combined to form a cold gas stream free of carbon monoxide.
- the carbon monoxide-free overhead gas can be partially liquefied in a condenser / evaporator against a liquid refrigerant, which is evaporated in the process, and a gas stream resulting from the evaporation of the liquid refrigerant and a top gas from the He-Ne-H 2 column can cold to a carbon monoxide-free Gas flow can be summarized.
- the carbon monoxide-free cold gas stream is advantageously warmed in a heat exchanger, compressed and cooled in countercurrent in the same heat exchanger and then partly in the low-pressure column and partly in the He-Ne-H 2 column for heating the Used sump and liquefied except gaseous residual streams and fed as the liquid refrigerant to the condenser / evaporator.
- the flows liquefied during the heating of the He-Ne-H 2 column and the low-pressure column can be fed to the He-Ne-H 2 column as a return.
- the flows liquefied during the heating of the He-Ne-H 2 column and the low pressure column in the evaporator / condenser of the low pressure column can liquefy the carbon monoxide-free overhead gas of the low pressure column to a residual flow and are at least partially fed as reflux to the He-Ne-H 2 column.
- the disadvantage of an additional investment for the condenser / evaporator is then offset by the advantage, which should not be underestimated, that in the event of air leakage during the compression of the carbon monoxide-free gas stream, the ultrapure liquid nitrogen cannot be contaminated.
- Ultrapure nitrogen can be drawn off liquid from the He-Ne-H 2 column and can be obtained partly as the return of the low-pressure column and partly as a liquid ultra-pure nitrogen product.
- the ultra pure liquid nitrogen product can be fed to a product tank.
- the ultra pure liquid nitrogen product can be pressurized with a pump, under Use of the cold content in the production of oxygen-free Compressed nitrogen fraction evaporates, warmed up and as a gaseous pressure product Use can be supplied.
- the process for producing ultra pure Liquid nitrogen product also made and ultra-pure nitrogen gas product the cold of the original liquid product is used sensibly become.
- FIG. 1 shows schematically an embodiment of the method according to the invention for the production of ultra-pure nitrogen. Except for a residual content in the range of a few mol ppm of oxygen-free liquid pressure nitrogen fraction 1 is expanded into a heated low pressure column 2, which is operated at a pressure between 4.5 and 5.5 bar. In the low-pressure column 2, rising steam is released from the He-Ne-H 2 column 4 of carbon monoxide and thus also of impurities boiling heavier than carbon monoxide, such as argon and the residual oxygen content, depending on the purity requirement, by means of ultrapure nitrogen 3 which is applied at the top as a return line exempted a few mol-ppb.
- the carbon monoxide-free head gas 5 and a head gas 6 of the He-Ne-H 2 column are combined to form a carbon monoxide-free cold gas stream 7, heated in a heat exchanger 8 and cooled again after compression 9 in the same heat exchanger 8.
- the cooled gas stream 10 is used to a part 11 in the low pressure column 2 and to another part 12 in the He-Ne-H 2 column 4 for heating 13, 14 of the sump and liquefied except for gaseous residual streams 15, 16.
- the liquefied streams 17, 18 are fed to the He-Ne-H 2 column 4 as a return.
- FIG. 2 shows schematically the production of the ultra-pure liquid nitrogen product 20 as in FIG. 1.
- the liquid nitrogen fraction 1 used as the insert is different from in the embodiment according to FIG. 1 of a pressure column 25 of a rectification system removed and fed into the low pressure column 2 via a heat exchanger 24.
- the ultra pure liquid nitrogen product 20 is pressurized by a pump 26 in counterflow to the liquid nitrogen fraction 1 via the heat exchanger 24 passed and using the cold content in a condenser 27 and in one Heat exchanger 28 in the extraction of the oxygen-free pressure nitrogen fraction used, evaporated, warmed and as a gaseous ultra-pure printed product 29 fed for further use.
- FIG. 3 schematically shows an embodiment of the method according to the invention using a condenser / evaporator 30.
- the carbon monoxide-free top gas 5 of the low-pressure column 2 (against one by combining the liquefied streams 17, 18 formed liquid coolant 31, which evaporates here) liquefied in the condenser / evaporator 30 except for a gaseous residual stream 32 and used in the He-Ne-H 2 column 4 as the return 33.
- a gas stream 5 ′ formed during the evaporation of the liquid refrigerant and the top gas 6 of the He-Ne-H 2 column 4 are combined to form the cold carbon monoxide-free gas stream 7.
- Figure 4 schematically shows an embodiment of the method according to the invention in FIG. 2, but carried out with the condenser / evaporator 30 as in FIG. 3.
- FIG. 5 shows schematically that the inventive method on a existing rectification system can be used.
- Condenser 27 is added and the heat exchanger 8 receives two additional ones Passages for the use of the cold of the ultra pure nitrogen 20 'to be heated the cooling and liquefaction of a partial flow 34 of the air 35 for the Rectification system.
- the ultrapure heated in this case in the heat exchanger 8 Nitrogen is used as a gaseous ultrapure printed product 29 for further use fed.
- a common feature of the design of the method according to the invention according to Figures 1 to 5 is that all residual gas flows (15, 16, 36 in Figure 1, 2, 5 and 15, 16, 32, 36 in Figure 3, 4) to a cold residual gas stream 37 summarized heated in the heat exchanger 8 and as an impure gas 38 to the Atmosphere.
- m 3 means: m 3 in the normal state at 0 ° C and 1.0133 bar; ie 1m 3 corresponds to 1.25 kg.
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Abstract
Description
Die Erfindung betrifft ein Verfahren zur Gewinnung von ultrareinem Stickstoff durch Tieftemperaturzerlegung von Luft in einem Rektifiziersystem mit wenigstens einer Rektifiziersäule, wobei verdichtete und gereinigte Einsatzluft in eine Drucksäule geführt, aus der Drucksäule eine sauerstofffreie Druckstickstofffraktion gewonnen, in eine Niederdrucksäule geführt und in der Niederdrucksäule kohlenmonoxidfreier Niederdruckstickstoff als Kopfgas gewonnen wird.The invention relates to a process for the production of ultra-pure nitrogen by Cryogenic air separation in a rectification system with at least one Rectification column, whereby compressed and cleaned feed air into a pressure column led, an oxygen-free pressure nitrogen fraction obtained from the pressure column, in a low pressure column and in the low pressure column carbon monoxide free Low pressure nitrogen is obtained as a top gas.
In der zur Veröffentlichung vorgesehenen deutschen Patentanmeldung mit dem
Aktenzeichen 198 06 576 ist ein Verfahren nach dem Oberbegriff des Anspruchs 1
bekannt. Einer Drucksäule wird eine sauerstofffreie Druckstickstofffraktion entnommen,
wobei die Drucksäule mindestens 160 theoretische Böden aufweist, um den
Druckstickstoff aus dieser Drucksäule darüber hinaus kohlenmonoxidfrei zu
entnehmen. Der Energieaufwand hierfür ist allerdings trotz der 160 theoretischen
Böden immer noch sehr hoch. Nachteilig ist außerdem, daß ein Großteil des
ultrareinen Stickstoffs gasförmig gewonnen wird.In the German patent application intended for publication with the
Case number 198 06 576 is a method according to the preamble of
Aufgabe der Erfindung ist es deshalb, diesen Nachteil zu vermeiden und den Energiebedarf zu senken.The object of the invention is therefore to avoid this disadvantage and Reduce energy consumption.
Eine weitere Aufgabe der Erfindung besteht darin, ein Verfahren aufzuzeigen, das wahlweise mit einer flüssigen Druckstickstofffraktion direkt aus der Drucksäule oder aus einem Tank mit flüssigem Drucksäulenstickstoff betrieben wird.Another object of the invention is to demonstrate a method which either with a liquid pressure nitrogen fraction directly from the pressure column or is operated from a tank with liquid pressure column nitrogen.
Diese Aufgaben werden erfindungsgemäß gelöst von einem Verfahren mit den
Merkmalen des Anspruchs 1. Ausführungen der Erfindung sind Gegenstand von
Unteransprüchen.According to the invention, these objects are achieved by a method with the
Features of
Kennzeichnend an der Erfindung ist, daß die sauerstofffreie Druckstickstofffraktion entweder aus einem oberen Bereich der Drucksäule flüssig entnommen oder aus einem Flüssigkeitstank mit gespeichertem sauerstofffreiem Stickstoff bereitgestellt wird und daß die sauerstofffreie Druckstickstofffraktion in die in ihrem Sumpf beheizte Niederdrucksäule entspannt wird, wobei in der Niederdrucksäule aufsteigender Dampf gebildet und mit Hilfe eines am Kopf der Niederdrucksäule aufgegebenen Rücklaufes mit ultrareinem Stickstoff von Kohlenmonoxid befreit, am Kopf der Niederdrucksäule als kohlenmonoxidfreies Kopfgas abgezogen und nach einer Druckerhöhung teilweise verflüssigt wird und der verflüssigte Teil in eine in ihrem Sumpf beheizte He-Ne-H2-Säule entspannt wird, aus der der ultrareine Stickstoff flüssig entnommen wird.It is characteristic of the invention that the oxygen-free pressurized nitrogen fraction is either withdrawn in liquid form from an upper region of the pressure column or is provided from a liquid tank with stored oxygen-free nitrogen and that the oxygen-free pressurized nitrogen fraction is expanded into the low-pressure column heated in its sump, steam rising in the low-pressure column formed and freed of carbon monoxide with the aid of a reflux at the top of the low-pressure column with ultra-pure nitrogen, drawn off at the top of the low-pressure column as carbon monoxide-free head gas and partially liquefied after a pressure increase and the liquefied part in a He-Ne-H 2 - heated in its sump The column is relaxed, from which the ultra-pure nitrogen is removed in liquid form.
Mit dem erfindungsgemäßen Verfahren wird der ultrareine Stickstoff flüssig gewonnen und kann in dieser Form leichter transportiert und deshalb einfacher an Kunden verteilt werden. Das Verfahren ist darüber hinaus universell einsetzbar. Es kann nämlich mit Anschluß an eine Luftzerlegungsanlage (mit oder ohne Flüssigstickstofftank) oder nur an einem Flüssigstickstofftank (mit räumlicher Trennung von der Luftzerlegungsanlage) verwendet werden. An einer Luftzerlegungsanlage mit Flüssigstickstofftank kann außerdem der ultrareine Flüssigstickstoff gewonnen werden, ohne daß die Luftzerlegungsanlage in Betrieb ist.With the method according to the invention, the ultra pure nitrogen is obtained in liquid form and is easier to transport in this form and therefore easier to distribute to customers become. The process can also be used universally. Because it can with Connection to an air separation plant (with or without liquid nitrogen tank) or only on a liquid nitrogen tank (with spatial separation from the air separation plant) be used. On an air separation plant with a liquid nitrogen tank also the ultra pure liquid nitrogen can be obtained without the Air separation plant is in operation.
Bei der Ausgestaltung des erfindungsgemäßen Verfahrens können das kohlenmonoxidfreie Kopfgas und ein Kopfgas der He-Ne-H2-Säule zu einem kohlenmonoxidfreien kalten Gasstrom zusammengefaßt werden.In the embodiment of the method according to the invention, the carbon monoxide-free head gas and a head gas of the He-Ne-H 2 column can be combined to form a cold gas stream free of carbon monoxide.
Alternativ kann das kohlenmonoxidfreie Kopfgas gegen einen flüssigen Kälteträger, der hierbei verdampft wird, in einem Kondensator/Verdampfer teilweise verflüssigt werden und ein bei der Verdampfung des flüssigen Kälteträgers entstehender Gasstrom und ein Kopfgas der He-Ne-H2-Säule können zu einem kohlenmonoxidfreien kalten Gasstrom zusammengefaßt werden.Alternatively, the carbon monoxide-free overhead gas can be partially liquefied in a condenser / evaporator against a liquid refrigerant, which is evaporated in the process, and a gas stream resulting from the evaporation of the liquid refrigerant and a top gas from the He-Ne-H 2 column can cold to a carbon monoxide-free Gas flow can be summarized.
Mit Vorteil wird in beiden Fällen der kohlenmonoxidfreie kalte Gasstrom in einem Wärmeaustauscher angewärmt, verdichtet und im Gegenstrom im gleichen Wärmetauscher wieder abgekühlt und anschließend zu einem Teil in der Niederdrucksäule und zu einem anderen Teil in der He-Ne-H2-Säule zur Beheizung des Sumpfes verwendet und dabei bis auf gasförmig verbleibende Restströme verflüssigt und als der flüssige Kälteträger dem Kondensator/Verdampfer zugeführt.In both cases, the carbon monoxide-free cold gas stream is advantageously warmed in a heat exchanger, compressed and cooled in countercurrent in the same heat exchanger and then partly in the low-pressure column and partly in the He-Ne-H 2 column for heating the Used sump and liquefied except gaseous residual streams and fed as the liquid refrigerant to the condenser / evaporator.
Die bei der Beheizung der He-Ne-H2-Säule und der Niederdrucksäule verflüssigten Ströme können der He-Ne-H2-Säule als Rücklauf zugeführt werden. The flows liquefied during the heating of the He-Ne-H 2 column and the low-pressure column can be fed to the He-Ne-H 2 column as a return.
Bei der oben als alternativ bezeichneten Verwendung eines Kondensator/Verdampfer kann mit Hilfe der bei der Beheizung der He-Ne-H2-Säule und der Niederdrucksäule verflüssigten Ströme in dem Verdampfer/Kondensator der Niederdrucksäule das kohlenmonoxidfreie Kopfgas der Niederdrucksäule bis auf einen Reststrom verflüssigt und mindestens teilweise als Rücklauf der He-Ne-H2-Säule zugeführt werden. Dem Nachteil einer zusätzlichen Investition für den Kondensator/Verdampfer steht dann der nicht zu unterschätzende Vorteil gegenüber, daß bei Luftleckagen bei der Verdichtung des kohlenmonoxidfreien Gasstromes keine Verunreinigung des ultrareinen Flüssigstickstoffs erfolgen kann.In the use of a condenser / evaporator referred to above as alternative, the flows liquefied during the heating of the He-Ne-H 2 column and the low pressure column in the evaporator / condenser of the low pressure column can liquefy the carbon monoxide-free overhead gas of the low pressure column to a residual flow and are at least partially fed as reflux to the He-Ne-H 2 column. The disadvantage of an additional investment for the condenser / evaporator is then offset by the advantage, which should not be underestimated, that in the event of air leakage during the compression of the carbon monoxide-free gas stream, the ultrapure liquid nitrogen cannot be contaminated.
Aus der He-Ne-H2-Säule kann ultrareiner Stickstoff flüssig abgezogen und teils als der Rücklauf der Niederdrucksäule und teils als flüssiges ultrareines Stickstoffprodukt gewonnen werden.Ultrapure nitrogen can be drawn off liquid from the He-Ne-H 2 column and can be obtained partly as the return of the low-pressure column and partly as a liquid ultra-pure nitrogen product.
Das ultrareine Flüssigstickstoffprodukt kann einem Produkttank zugeführt werden.The ultra pure liquid nitrogen product can be fed to a product tank.
Das ultrareine Flüssigstickstoffprodukt kann mit einer Pumpe auf Druck gebracht, unter Nutzung des Kälteinhaltes bei der Gewinnung der sauerstofffreien Druckstickstofffraktion verdampft, angewärmt und als gasförmiges Druckprodukt einer Verwendung zugeführt werden.The ultra pure liquid nitrogen product can be pressurized with a pump, under Use of the cold content in the production of oxygen-free Compressed nitrogen fraction evaporates, warmed up and as a gaseous pressure product Use can be supplied.
In diesem Fall kann mit dem Verfahren zur Herstellung von ultrareinem Flüssigstickstoffprodukt auch gasförmiges ultrareines Stickstoffprodukt hergestellt und dabei die Kälte des ursprünglich vorliegenden Flüssigproduktes sinnvoll genutzt werden.In this case, the process for producing ultra pure Liquid nitrogen product also made and ultra-pure nitrogen gas product the cold of the original liquid product is used sensibly become.
Die Erfindung wird anhand von fünf Ausgestaltungen mit fünf Figuren näher erläutert.
Äquivalente Verfahrensströme und -schritte sind in den Figuren 1 bis 5 mit identischen Bezugsziffern versehen.Equivalent process streams and steps are identical in FIGS. 1 to 5 Provide reference numbers.
Figur 1 zeigt schematisch eine Ausführung des erfindungsgemäßen Verfahrens zur
Gewinnung von ultrareinem Stickstoff. Eine bis auf einen Restgehalt im Bereich
weniger mol-ppm sauerstofffreie flüssige Druckstickstofffraktion 1 wird in eine beheizte
Niederdrucksäule 2 entspannt, die bei einem Druck zwischen 4,5 und 5,5 bar betrieben
wird. In der Niederdrucksäule 2 aufsteigender Dampf wird durch als Rücklauf am Kopf
aufgegebenen ultrareinen Stickstoff 3 aus einer He-Ne-H2-Säule 4 von Kohlenmonoxid
und damit auch von schwerer als Kohlenmonoxid siedenden Verunreinigungen wie
Argon und dem Restgehalt an Sauerstoff je nach Reinheitsanforderung bis auf wenige
mol-ppb befreit. Das kohlenmonoxidfreie Kopfgas 5 und ein Kopfgas 6 der He-Ne-H2-Säule
werden zu einem kohlenmonoxidfreien kalten Gasstrom 7 zusammengefaßt, in
einem Wärmeaustauscher 8 angewärmt und nach einer Verdichtung 9 im gleichen
Wärmetauscher 8 wieder abgekühlt. Der abgekühlte Gasstrom 10 wird zu einem Teil
11 in der Niederdrucksäule 2 und zu einem anderen Teil 12 in der He-Ne-H2-Säule 4
zur Beheizung 13, 14 des Sumpfes verwendet und dabei bis auf gasförmig
verbleibende Restströme 15, 16 verflüssigt. Die verflüssigten Ströme 17, 18 werden
der He-Ne-H2-Säule 4 als Rücklauf zugeführt. Aus der He-Ne-H2-Säule 4 wird
kohlenmonoxidfreier ultrareiner Stickstoff 19 flüssig abgezogen, der nun auch das
leichter siedende Neon und erst recht die noch leichter siedenden Bestandteile
Wasserstoff und Helium je nach Anforderung in der Größenordnung von wenigen mol-ppb
enthält. Der flüssige ultrareine Stickstoff 19 wird zu einem Teil 3 als der Rücklauf
der Niederdrucksäule 2 verwendet und zu einem anderen Teil als flüssiges ultrareines
Flüssigstickstoffprodukt 20 gewonnen und einem Produkttank 21 zugeführt. Figure 1 shows schematically an embodiment of the method according to the invention for the production of ultra-pure nitrogen. Except for a residual content in the range of a few mol ppm of oxygen-free liquid
In der Ausgestaltung des erfindungsgemäßen Verfahrens wie in Figur 1 wird die als
Einsatz verwendete flüssige Druckstickstofffraktion 1 einem Flüssigkeitstank 22 über
eine Druckerhöhungspumpe 23 entnommen und über einen Wärmeaustauscher 24 in
die Niederdrucksäule 2 geführt. Im Wärmeaustauscher 24 wird das ultrareine
Flüssigstickstoffprodukt 20 unterkühlt und anschließend ohne gasförmige
Entspannungsverluste in den Produkttank 21 entspannt. Wegen der Unterkühlung des
Flüssigstickstoffproduktes 20 kann der Produkttank 21 als drucklos betriebener
Flüssigkeitstank ausgeführt werden.In the embodiment of the method according to the invention as in FIG. 1, the as
Insert used liquid
Figur 2 zeigt schematisch die Gewinnung des ultrareinen Flüssigstickstoffproduktes 20
wie in Figur 1. Die als Einsatz verwendete flüssige Stickstofffraktion 1 wird anders als
in der Ausgestaltung nach Figur 1 einer Drucksäule 25 eines Rektifiziersystems
entnommen und über einen Wärmeaustauscher 24 in die Niederdrucksäule 2 geführt.
Das ultrareine Flüssigstickstoffprodukt 20 wird mit einer Pumpe 26 auf Druck gebracht
im Gegenstrom zur flüssigen Stickstofffraktion 1 über den Wärmeaustauscher 24
geleitet und unter Nutzung des Kälteinhalts in einem Kondensator 27 und in einem
Wärmeaustauscher 28 bei der Gewinnung der sauerstofffreien Druckstickstofffraktion
verwendet, dabei verdampft, angewärmt und als gasförmiges ultrareines Druckprodukt
29 einer weiteren Verwendung zugeführt.FIG. 2 shows schematically the production of the ultra-pure
Figur 3 zeigt schematisch eine Ausführung des erfindungsgemäßen Verfahrens unter
Verwendung eines Kondensator/Verdampfers 30. Anders als in der Ausgestaltung
nach Figur 1 wird in der Ausgestaltung nach Figur 3 das kohlenmonoxidfreie Kopfgas 5
der Niederdrucksäule 2 (gegen einen durch Zusammenführung der verflüssigten
Ströme 17, 18 gebildeten flüssigen Kälteträger 31, der hierbei verdampft,) in dem
Kondensator/Verdampfer 30 bis auf einen gasförmig verbleibenden Reststrom 32
verflüssigt und in der He-Ne-H2-Säule 4 als Rücklauf 33 verwendet. Ein bei der
Verdampfung des flüssigen Kälteträgers entstehender Gasstrom 5' und das Kopfgas 6
der He-Ne-H2-Säule 4 werden zu dem kalten kohlenmonoxidfreien Gasstrom 7
zusammengefaßt.FIG. 3 schematically shows an embodiment of the method according to the invention using a condenser /
Mit dem Kondensator/Verdampfer 30 ist zwar eine zusätzliche Investition verbunden,
aber die Säulen 2, 4 werden so entkoppelt, daß selbst im Falle einer bei der
Verdichtung auftretenden Leckage von Luft in das kohlenmonoxidfreie Gas 7, 10 hinein
die He-Ne-H2-Säule 4 und damit das ultrareine Stickstoffprodukt 20 nicht kontaminiert
werden.An additional investment is connected to the condenser /
Figur 4 zeigt schematisch eine Ausgestaltung des erfindungsgemäßen Verfahrens wie
in Figur 2, aber ausgeführt mit dem Kondensator/Verdampfer 30 wie in Figur 3.Figure 4 schematically shows an embodiment of the method according to the invention
in FIG. 2, but carried out with the condenser /
Figur 5 zeigt schematisch, daß das erfindungsgemäße Verfahren an einem
existierenden Rektifiziersystem verwendet werden kann. Ausgehend von der
Ausgestaltung des Verfahrens wie in Figur 2 wird am Rektifiziersystem der
Kondensator 27 ergänzt und der Wärmeaustauscher 8 erhält zwei zusätzliche
Passagen für die Nutzung der Kälte des anzuwärmenden ultrareinen Stickstoffs 20' bei
der Abkühlung und Verflüssigung eines Teilstromes 34 der Luft 35 für das
Rektifiziersystem. Der hierbei im Wärmeaustauscher 8 angewärmte ultrareine
Stickstoff wird als gasförmiges ultrareines Druckprodukt 29 einer weiteren Verwendung
zugeführt.Figure 5 shows schematically that the inventive method on a
existing rectification system can be used. Starting from the
Design of the method as in FIG. 2 is carried out on the
Ein gemeinsames Merkmal der Ausgestaltung des erfindungsgemäßen Verfahrens
gemäß Figur 1 bis 5 besteht darin, daß alle anfallenden Restgasströme (15, 16, 36 in
Figur 1, 2, 5 und 15, 16, 32, 36 in Figur 3, 4) zu einem kalten Restgasstrom 37
zusammengefaßt im Wärmeaustauscher 8 angewärmt und als unreines Gas 38 an die
Atmosphäre geleitet werden.A common feature of the design of the method according to the invention
according to Figures 1 to 5 is that all residual gas flows (15, 16, 36 in
Figure 1, 2, 5 and 15, 16, 32, 36 in Figure 3, 4) to a cold
m3 bedeutet in diesem Beispiel: m3 im Normzustand bei 0°C und 1,0133 bar; d.h. 1m3 entspricht 1,25 kg.In this example, m 3 means: m 3 in the normal state at 0 ° C and 1.0133 bar; ie 1m 3 corresponds to 1.25 kg.
Mit dem erfindungsgemäßen Verfahren in der Ausgestaltung von Figur 1 werden aus 1750 m3/h flüssigem Stickstoff mit 1 mol-ppm Kohlenmonoxid 1500 m3/h ultrareiner flüssiger Stickstoff mit 20 mol-ppb Kohlenmonoxid erzeugt. Hierbei entstehen 100 m3/h Verluste bei der Verdichtung und 150 m3/h Restgas. 12.500 m3/h Stickstoff werden von 6,5 auf 7 bar verdichtet; die Druckerhöhungspumpe arbeitet zwischen 1 bar am Eintritt und 7 bar am Austritt.With the method according to the invention in the embodiment of FIG. 1, 1500 m 3 / h of ultrapure liquid nitrogen with 20 mol-ppb of carbon monoxide are produced from 1750 m 3 / h of liquid nitrogen with 1 mol-ppm carbon monoxide. This results in losses of 100 m 3 / h during compression and 150 m 3 / h residual gas. 12,500 m 3 / h of nitrogen are compressed from 6.5 to 7 bar; the booster pump works between 1 bar at the inlet and 7 bar at the outlet.
Claims (9)
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
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DE19852019 | 1998-11-11 | ||
DE19852019 | 1998-11-11 | ||
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DE19924375 | 1999-05-27 |
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EP (1) | EP1001236B1 (en) |
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DE10158327A1 (en) * | 2001-11-28 | 2003-06-18 | Linde Ag | Process and apparatus for producing high purity nitrogen from less pure nitrogen |
DE10205094A1 (en) * | 2002-02-07 | 2003-08-21 | Linde Ag | Method and device for producing high-purity nitrogen |
CN102959352B (en) * | 2009-07-24 | 2016-07-06 | 英国备选能源国际有限公司 | Carbon dioxide and the separation of hydrogen |
CN102797974A (en) * | 2012-07-31 | 2012-11-28 | 张立永 | Hydrogen maser |
CN114165989A (en) * | 2021-11-22 | 2022-03-11 | 四川空分设备(集团)有限责任公司 | Device and method for preparing medium-pressure nitrogen |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4464188A (en) * | 1983-09-27 | 1984-08-07 | Air Products And Chemicals, Inc. | Process and apparatus for the separation of air |
US5167125A (en) * | 1991-04-08 | 1992-12-01 | Air Products And Chemicals, Inc. | Recovery of dissolved light gases from a liquid stream |
EP0569310A1 (en) * | 1992-05-08 | 1993-11-10 | Nippon Sanso Corporation | Installation for air liquefaction separation and process therefor |
EP0834711A2 (en) * | 1996-10-02 | 1998-04-08 | Linde Aktiengesellschaft | Process and apparatus for the production of high purity nitrogen |
DE19806576A1 (en) * | 1998-02-17 | 1998-08-06 | Linde Ag | Recovery of highest purity nitrogen@ for semiconductor industry |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
US5170630A (en) * | 1991-06-24 | 1992-12-15 | The Boc Group, Inc. | Process and apparatus for producing nitrogen of ultra-high purity |
US5351492A (en) * | 1992-09-23 | 1994-10-04 | Air Products And Chemicals, Inc. | Distillation strategies for the production of carbon monoxide-free nitrogen |
FR2696821B1 (en) * | 1992-10-09 | 1994-11-10 | Air Liquide | Process and installation for producing ultra-pure nitrogen under pressure. |
JP3447437B2 (en) * | 1995-07-26 | 2003-09-16 | 日本エア・リキード株式会社 | High-purity nitrogen gas production equipment |
US5906113A (en) * | 1998-04-08 | 1999-05-25 | Praxair Technology, Inc. | Serial column cryogenic rectification system for producing high purity nitrogen |
-
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- 1999-10-29 TW TW088118824A patent/TW432191B/en not_active IP Right Cessation
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- 1999-11-05 AT AT99122146T patent/ATE278166T1/en not_active IP Right Cessation
- 1999-11-05 ES ES99122146T patent/ES2229608T3/en not_active Expired - Lifetime
- 1999-11-09 CA CA002289173A patent/CA2289173A1/en not_active Abandoned
- 1999-11-10 SG SG1999005577A patent/SG74755A1/en unknown
- 1999-11-10 US US09/437,263 patent/US6276172B1/en not_active Expired - Fee Related
- 1999-11-10 JP JP11319519A patent/JP2000180051A/en active Pending
- 1999-11-11 KR KR1019990049862A patent/KR20000035406A/en not_active Application Discontinuation
- 1999-11-11 CN CNB991238044A patent/CN1134640C/en not_active Expired - Fee Related
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4464188A (en) * | 1983-09-27 | 1984-08-07 | Air Products And Chemicals, Inc. | Process and apparatus for the separation of air |
US5167125A (en) * | 1991-04-08 | 1992-12-01 | Air Products And Chemicals, Inc. | Recovery of dissolved light gases from a liquid stream |
EP0569310A1 (en) * | 1992-05-08 | 1993-11-10 | Nippon Sanso Corporation | Installation for air liquefaction separation and process therefor |
EP0834711A2 (en) * | 1996-10-02 | 1998-04-08 | Linde Aktiengesellschaft | Process and apparatus for the production of high purity nitrogen |
DE19806576A1 (en) * | 1998-02-17 | 1998-08-06 | Linde Ag | Recovery of highest purity nitrogen@ for semiconductor industry |
Also Published As
Publication number | Publication date |
---|---|
DE59910646D1 (en) | 2004-11-04 |
SG74755A1 (en) | 2000-08-22 |
CN1134640C (en) | 2004-01-14 |
KR20000035406A (en) | 2000-06-26 |
EP1001236A3 (en) | 2000-11-08 |
US6276172B1 (en) | 2001-08-21 |
ATE278166T1 (en) | 2004-10-15 |
CA2289173A1 (en) | 2000-05-11 |
ES2229608T3 (en) | 2005-04-16 |
TW432191B (en) | 2001-05-01 |
JP2000180051A (en) | 2000-06-30 |
EP1001236B1 (en) | 2004-09-29 |
DE19929798A1 (en) | 2000-05-25 |
CN1255619A (en) | 2000-06-07 |
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