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EP1316768A1 - Process and device for the production of an ultra high purity liquid from a cryogenic liquid feed with lower purity - Google Patents

Process and device for the production of an ultra high purity liquid from a cryogenic liquid feed with lower purity Download PDF

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Publication number
EP1316768A1
EP1316768A1 EP02024690A EP02024690A EP1316768A1 EP 1316768 A1 EP1316768 A1 EP 1316768A1 EP 02024690 A EP02024690 A EP 02024690A EP 02024690 A EP02024690 A EP 02024690A EP 1316768 A1 EP1316768 A1 EP 1316768A1
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EP
European Patent Office
Prior art keywords
liquid
separation column
storage tank
evaporator
fraction
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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EP02024690A
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German (de)
French (fr)
Inventor
Gunther Hauck
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Linde GmbH
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Linde GmbH
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Filing date
Publication date
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Publication of EP1316768A1 publication Critical patent/EP1316768A1/en
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • 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
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/44—Separating high boiling, i.e. less volatile components from nitrogen, e.g. CO, Ar, O2, hydrocarbons
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/42—One fluid being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/62—Details of storing a fluid in a tank

Definitions

  • the invention relates to a method for producing a high-purity cryogenic Liquid product from a less pure cryogenic feed liquid, in which a first stream of less pure cryogenic feed liquid from a storage tank into a first separation column is introduced, a second stream less pure cryogenic
  • the feed liquid evaporates from the storage tank in a pressure build-up evaporator and returned to the storage tank, a gaseous fraction from the top Area of the first separation column liquefied in a condenser-evaporator and at from which a highly pure liquid product is obtained.
  • Such a system can be used, for example, to produce high-purity nitrogen be used. It can be obtained more cheaply at the location of the consumer less pure nitrogen can be transported in liquid form; from this less pure cryogenic liquid becomes the required with a relatively uncomplicated apparatus highly pure product made.
  • the procedure is also based on other substances applicable and can for example for the production of high purity oxygen or high pure argon can be used.
  • the invention has for its object such a method and / or specify appropriate device that are particularly simple in terms of equipment.
  • This object is achieved in that a gaseous fraction from the Storage tank is removed and fed to the first separation column.
  • compressed gas e.g. from a pipeline system
  • this can be introduced into the storage tank.
  • a liquid fraction from the bottom of the first Separation column removed and used to cool the condenser-evaporator. This eliminates the need for external cooling to cool the first separation column. If the process is designed as a one-column process, the liquid fraction be introduced directly into the evaporation chamber of the condenser-evaporator. Alternatively, intermediate steps are possible, even those that have the composition change the liquid fraction.
  • the method can also be designed as a two-pillar process by the liquid fraction is introduced into a second separation column and the condenser-evaporator is designed as a reboiler of the second separation column, for example as Bottom reboiler. Since the concentration difference between the head of the first and Sump of the second separation column is relatively low, the operating pressure of the first one Separation column to be only slightly higher than that of the second separation column. As a result, a higher yield is high with the same amount of energy being used pure product possible. This can, for example, also be gaseous from the second Separation column are withdrawn.
  • the combination of the two separation columns and the condenser-evaporator is preferably a classic double column educated.
  • no compressors or pumps are used in the process.
  • no fluid is compressed by a machine to heat or cold for the operation of the separation column (s).
  • a refrigeration cycle intended.
  • the invention also relates to a device according to claim 7.
  • a storage tank 1 stored, the less pure cryogenic feed liquid in the embodiment forms.
  • the tank 1 can, for example, by means of tank vehicles or a pipeline be filled (not shown).
  • Liquid 2 ("second stream of less pure cryogenic Feed liquid ") from the tank is evaporated in a pressure build-up evaporator 3, which is heated with water or air, for example.
  • the resulting one Gaseous nitrogen 4 is introduced into the gas space of the storage tank 1. He flows through heat exchanger tubes 5 and thereby enters indirect heat exchange with the liquid stored in the tank. In this way the pressure level in the Storage tank 1 kept at 5 to 12 bar without the need for external energy would be necessary.
  • the medium for heating the pressure build-up evaporator is in generally available free of charge or at negligible costs.
  • the first Separation column 7 is in the example part of a double column system, which is also a second separation column 8 and a condenser-evaporator 9. Besides, will Steam 10 from the storage tank 1 as a gaseous feed fraction in the first Separation column 7 fed.
  • Top gas 11 of the first separation column 7 is liquefied in the condenser-evaporator 9.
  • Condensate 12 obtained in this way becomes a first part 13 as a return to the first separation column 7 abandoned.
  • a second part 14 is called a high purity liquid product removed and fed to a pure nitrogen tank 15.
  • the rest 16 serves as a return for the second separation column 8.
  • Impure liquid 17 from the bottom of the first separation column 7 is a liquid fraction of the second separation column 8 at an intermediate point fed.
  • a residual liquid 18 is drawn off from the bottom of the second separation column 8.
  • Liquid 20 from the pure nitrogen tank 15 can be vaporized (21) and via line 22 can also be sent to a consumer.
  • Figure 2 differs from Figure 1 in that a compressed gas stream from a external source, for example from a pipeline network for nitrogen technical Purity that is introduced into the system.
  • a compressed gas stream from a external source for example from a pipeline network for nitrogen technical Purity that is introduced into the system.
  • the compressed gas flow 24 in one Heat exchanger 25 cooled and introduced via line 26 into the storage tank 1, in the example together with the steam 4 from the pressure build-up evaporator 3.

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  • 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

In a process to extract an ultra-pure fluid at low temperature from a less pure fluid at cryogenic temperature, a gaseous fraction (10) is drawn from a reservoir (1) and surrendered to a separation column (7). <??>Also claimed is a commensurate assembly in which a first flow (6) of the impure fluid is drawn from a reservoir (1) and fed to a separation column (7). A second flow (2) of impure very cold fluid is also drawn from the tank (1), evaporated (3) under pressure and returned to the tank (1). A gaseous fraction (11) from the upper separation column is liquefied by a condenser-evaporator (9) producing an ultra-pure product (14). A flow of pressurized gas (23, 26) is supplied from an external source to the reservoir (1). Before its introduction to the tank (1) vapor (4) derived from very cold liquid and/or pressurized gas (26) is brought into indirect contact with fluid in the tank (1) in a heat exchanger (5). A liquid fraction (17) is drawn from the lower section of the first separator column (7) and used to cool the condenser-evaporator (9).

Description

Die Erfindung betrifft ein Verfahren zur Herstellung eines hoch reinen tiefkalten Flüssigprodukts aus einer weniger reinen tiefkalten Einsatzflüssigkeit, bei dem ein erster Strom weniger reiner tiefkalter Einsatzflüssigkeit aus einem Speichertank in eine erste Trennsäule eingeleitet wird, ein zweiter Strom weniger reiner tiefkalter Einsatzflüssigkeit aus dem Speichertank in einem Druckaufbauverdampfer verdampft und in den Speichertank zurückgeleitet wird, eine gasförmige Fraktion aus dem oberen Bereich der ersten Trennsäule in einem Kondensator-Verdampfer verflüssigt und bei dem ein hoch reines Flüssigprodukt gewonnen wird.The invention relates to a method for producing a high-purity cryogenic Liquid product from a less pure cryogenic feed liquid, in which a first stream of less pure cryogenic feed liquid from a storage tank into a first separation column is introduced, a second stream less pure cryogenic The feed liquid evaporates from the storage tank in a pressure build-up evaporator and returned to the storage tank, a gaseous fraction from the top Area of the first separation column liquefied in a condenser-evaporator and at from which a highly pure liquid product is obtained.

Ein derartiges System kann beispielsweise zur Erzeugung hoch reinen Stickstoffs eingesetzt werden. Am Ort des Verbrauchers kann dabei kostengünstig erhältlicher weniger reiner Stickstoff flüssig antransportiert werden; aus dieser weniger reinen tiefkalten Flüssigkeit wird mit einer relativ unkomplizierten Apparatur das benötigte hoch reine Produkt hergestellt. Das Verfahren ist aber auch auf andere Substanzen anwendbar und kann beispielsweise zur Herstellung hoch reinen Sauerstoffs oder hoch reinen Argons eingesetzt werden.Such a system can be used, for example, to produce high-purity nitrogen be used. It can be obtained more cheaply at the location of the consumer less pure nitrogen can be transported in liquid form; from this less pure cryogenic liquid becomes the required with a relatively uncomplicated apparatus highly pure product made. The procedure is also based on other substances applicable and can for example for the production of high purity oxygen or high pure argon can be used.

Ein Verfahren der eingangs genannten Art ist aus US 5421164 bekannt. Dieses System kann aus technisch reinem Stickstoff, der aus einem Speichertank kommt, hoch reinen Stickstoff herstellen, ohne dass dazu bewegliche Maschinen wie zum Beispiel Verdichter oder Pumpen notwendig wären.A method of the type mentioned is known from US 5421164. This System can be made from technically pure nitrogen that comes from a storage tank Produce high purity nitrogen without the need for moving machines such as Example compressors or pumps would be necessary.

Der Erfindung liegt die Aufgabe zugrunde, ein derartiges Verfahren und/oder eine entsprechende Vorrichtung anzugeben, die apparativ besonders einfach sind.The invention has for its object such a method and / or specify appropriate device that are particularly simple in terms of equipment.

Diese Aufgabe wird dadurch gelöst, dass eine gasförmige Einsatzfraktion aus dem Speichertank entnommen und der ersten Trennsäule zugeleitet wird. This object is achieved in that a gaseous fraction from the Storage tank is removed and fed to the first separation column.

Dadurch kann auf einen separaten Wärmetauscher zur Erzeugung von aufsteigendem Dampf für die ersten Trennsäule verzichtet werden. Der für den Betrieb der Trennsäule erforderliche Dampf wird direkt dem Speichertank entnommen.This allows a separate heat exchanger to be used to generate ascending Steam for the first separation column can be dispensed with. The one for the operation of the separation column required steam is taken directly from the storage tank.

Wenn vor Ort Druckgas (zum Beispiel aus einem Leitungssystem) vorhanden ist, dessen Zusammensetzung ähnlich derjenigen der tiefkalten Einsatzflüssigkeit ist, kann dieses in den Speichertank eingeleitet werden.If compressed gas (e.g. from a pipeline system) is available on site, whose composition is similar to that of the cryogenic feed liquid this can be introduced into the storage tank.

Dabei ist es günstig, wenn in dem Druckaufbauverdampfer aus tiefkalter Flüssigkeit erzeugter Dampf und/oder der Druckgasstrom vor seiner Einleitung in den Speichertank in indirekten Wärmeaustausch mit der im Speichertank befindlichen tiefkalten Einsatzflüssigkeit gebracht wird. Dadurch wird zusätzlicher Dampf erzeugt, der als gasförmige Einsatzfraktion zur Verfügung steht.It is advantageous if in the pressure build-up evaporator from cryogenic liquid generated steam and / or the pressurized gas stream before its introduction into the Storage tank in indirect heat exchange with that in the storage tank cryogenic feed liquid is brought. This creates additional steam which is available as a gaseous feed fraction.

Vorzugsweise wird eine flüssige Fraktion aus dem unteren Bereich der ersten Trennsäule abgezogen und zur Kühlung des Kondensator-Verdampfers eingesetzt. Dadurch kann auf externe Kälte zur Kühlung der ersten Trennsäule verzichtet werden. Falls das Verfahren als Einsäulen-Prozess ausgebildet ist, kann die flüssige Fraktion direkt in den Verdampfungsraum des Kondensator-Verdampfers eingeleitet werden. Alternativ sind Zwischenschritte möglich, auch solche, welche die Zusammensetzung der flüssigen Fraktion verändern.Preferably, a liquid fraction from the bottom of the first Separation column removed and used to cool the condenser-evaporator. This eliminates the need for external cooling to cool the first separation column. If the process is designed as a one-column process, the liquid fraction be introduced directly into the evaporation chamber of the condenser-evaporator. Alternatively, intermediate steps are possible, even those that have the composition change the liquid fraction.

Das Verfahren kann auch als Zwei-Säulen-Prozess ausgebildet sein, indem die flüssige Fraktion in eine zweite Trennsäule eingeleitet wird und der Kondensator-Verdampfer als Aufkocher der zweiten Trennsäule ausgebildet ist, beispielsweise als Sumpfaufkocher. Da der Konzentrationsunterschied zwischen Kopf der ersten und Sumpf der zweiten Trennsäule relativ gering ist, braucht der Betriebsdruck der ersten Trennsäule nur geringfügig höher als derjenige der zweiten Trennsäule zu sein. Hierdurch ist bei gleich bleibendem Energieeinsatz eine höhere Ausbeute an hoch reinem Produkt möglich. Dieses kann beispielsweise auch gasförmig aus der zweiten Trennsäule abgezogen werden. Die Kombination aus den beiden Trennsäulen und dem Kondensator-Verdampfer ist vorzugsweise als klassische Doppelsäule ausgebildet. The method can also be designed as a two-pillar process by the liquid fraction is introduced into a second separation column and the condenser-evaporator is designed as a reboiler of the second separation column, for example as Bottom reboiler. Since the concentration difference between the head of the first and Sump of the second separation column is relatively low, the operating pressure of the first one Separation column to be only slightly higher than that of the second separation column. As a result, a higher yield is high with the same amount of energy being used pure product possible. This can, for example, also be gaseous from the second Separation column are withdrawn. The combination of the two separation columns and the condenser-evaporator is preferably a classic double column educated.

Vorzugsweise werden in dem Verfahren keine Verdichter oder Pumpen eingesetzt. Insbesondere wird kein Fluid mittels einer Maschine verdichtet, um Wärme oder Kälte für den Betrieb der Trennsäule(n) zu liefern. Erst recht ist kein Kältekreislauf vorgesehen.Preferably no compressors or pumps are used in the process. In particular, no fluid is compressed by a machine to heat or cold for the operation of the separation column (s). Especially not a refrigeration cycle intended.

Die Erfindung betrifft außerdem eine Vorrichtung gemäß den Patentanspruch 7.The invention also relates to a device according to claim 7.

Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand von in den Zeichnungen dargestellten Ausführungsbeispielen näher erläutert, welche die Erzeugung hoch reinen Stickstoffs aus technisch reinem Stickstoff betreffen. Hierbei zeigen:

Figur 1
ein erstes Ausführungsbeispiel der Erfindung, das ohne die Zufuhr eines Gases von außen auskommt, und
Figur 2
ein zweites Ausführungsbeispiel mit Zufuhr eines Druckgasstroms von außen.
The invention and further details of the invention are explained in more detail below with reference to exemplary embodiments illustrated in the drawings, which relate to the production of high-purity nitrogen from technically pure nitrogen. Here show:
Figure 1
a first embodiment of the invention, which does not require the supply of a gas from the outside, and
Figure 2
a second embodiment with supply of a pressurized gas stream from the outside.

In dem System der Figur 1 wird technisch reiner Stickstoff in einem Speichertank 1 gelagert, der in dem Ausführungsbeispiel die weniger reine tiefkalte Einsatzflüssigkeit bildet. Der Tank 1 kann beispielsweise mittels Tankfahrzeugen oder einer Rohrleitung befüllt werden (nicht dargestellt). Flüssigkeit 2 ("zweiter Strom weniger reiner tiefkalter Einsatzflüssigkeit") aus dem Tank wird in einem Druckaufbauverdampfer 3 verdampft, der beispielsweise mit Wasser oder Luft beheizt wird. Der dabei entstandene gasförmige Stickstoff 4 wird in den Gasraum des Speichertanks 1 eingeleitet. Er durchströmt dabei Wärmetauscherrohre 5 und tritt dabei in indirekten Wärmeaustausch mit der im Tank lagernden Flüssigkeit. Auf diese Weise wird das Druckniveau im Speichertank 1 auf 5 bis 12 bar gehalten, ohne dass dazu die Zufuhr externer Energie notwendig wäre. (Das Medium zur Beheizung des Druckaufbauverdampfers steht in der Regel kostenlos oder zu vemachlässigbaren Kosten zur Verfügung.)In the system of FIG. 1, technically pure nitrogen is stored in a storage tank 1 stored, the less pure cryogenic feed liquid in the embodiment forms. The tank 1 can, for example, by means of tank vehicles or a pipeline be filled (not shown). Liquid 2 ("second stream of less pure cryogenic Feed liquid ") from the tank is evaporated in a pressure build-up evaporator 3, which is heated with water or air, for example. The resulting one Gaseous nitrogen 4 is introduced into the gas space of the storage tank 1. He flows through heat exchanger tubes 5 and thereby enters indirect heat exchange with the liquid stored in the tank. In this way the pressure level in the Storage tank 1 kept at 5 to 12 bar without the need for external energy would be necessary. (The medium for heating the pressure build-up evaporator is in generally available free of charge or at negligible costs.)

Ein anderer Strom 6 flüssigen Stickstoffs aus dem Tank wird als "erster Strom weniger reiner tiefkalter Einsatzflüssigkeit" in eine erste Trennsäule 7 eingeleitet. Die erste Trennsäule 7 ist in dem Beispiel Teil eines Doppelsäulen-Systems, das außerdem eine zweite Trennsäule 8 und einen Kondensator-Verdampfer 9 aufweist. Außerdem wird Dampf 10 aus dem Speichertank 1 als gasförmige Einsatzfraktion in die erste Trennsäule 7 eingespeist.Another stream 6 of liquid nitrogen from the tank is called the "first stream less pure cryogenic feed liquid "is introduced into a first separation column 7. The first Separation column 7 is in the example part of a double column system, which is also a second separation column 8 and a condenser-evaporator 9. Besides, will Steam 10 from the storage tank 1 as a gaseous feed fraction in the first Separation column 7 fed.

Kopfgas 11 der ersten Trennsäule 7 wird im Kondensator-Verdampfer 9 verflüssigt. Dabei gewonnenes Kondensat 12 wird zu einem ersten Teil 13 als Rücklauf auf die erste Trennsäule 7 aufgegeben. Ein zweiter Teil 14 wird als hoch reines Flüssigprodukt entnommen und einem Reinstickstofftank 15 zugeleitet. Der Rest 16 dient als Rücklauf für die zweite Trennsäule 8. Unreine Flüssigkeit 17 vom Sumpf der ersten Trennsäule 7 wird als flüssige Fraktion der zweiten Trennsäule 8 an einer Zwischenstelle zugeleitet.Top gas 11 of the first separation column 7 is liquefied in the condenser-evaporator 9. Condensate 12 obtained in this way becomes a first part 13 as a return to the first separation column 7 abandoned. A second part 14 is called a high purity liquid product removed and fed to a pure nitrogen tank 15. The rest 16 serves as a return for the second separation column 8. Impure liquid 17 from the bottom of the first separation column 7 is a liquid fraction of the second separation column 8 at an intermediate point fed.

Vom Sumpf der zweiten Trennsäule 8 wird eine Restflüssigkeit 18 abgezogen. Am Kopf wird hoch reines Stickstoffgas 19 entnommen und einem Verbraucher zugeführt. Flüssigkeit 20 aus dem Reinstickstofftank 15 kann verdampft (21) und über Leitung 22 ebenfalls einem Verbraucher zugeleitet werden.A residual liquid 18 is drawn off from the bottom of the second separation column 8. At the Highly pure nitrogen gas 19 is removed from the head and fed to a consumer. Liquid 20 from the pure nitrogen tank 15 can be vaporized (21) and via line 22 can also be sent to a consumer.

Figur 2 unterscheidet sich dadurch von Figur 1, dass ein Druckgasstrom aus einer äußeren Quelle, beispielsweise aus einem Rohrleitungsnetz für Stickstoff technischer Reinheit, in das System eingebracht wird. Dazu wird der Druckgasstrom 24 in einem Wärmetauscher 25 abgekühlt und über Leitung 26 in den Speichertank 1 eingeführt, in dem Beispiel gemeinsam mit dem Dampf 4 aus dem Druckaufbauverdampfer 3.Figure 2 differs from Figure 1 in that a compressed gas stream from a external source, for example from a pipeline network for nitrogen technical Purity that is introduced into the system. For this purpose, the compressed gas flow 24 in one Heat exchanger 25 cooled and introduced via line 26 into the storage tank 1, in the example together with the steam 4 from the pressure build-up evaporator 3.

In dem Wärmetauscher 25 wird im Gegenstrom zu dem Druckgas 23 hoch reines Stickstoffgas 19 vom Kopf der zweiten Trennsäule 8 erwärmt und schließlich über Leitung 27 mit dem verdampften hoch reinen Stickstoff 22 aus dem Reinstickstofftank 15 vermischt.In the heat exchanger 25 is highly pure in counterflow to the compressed gas 23 Nitrogen gas 19 heated from the top of the second separation column 8 and finally over Line 27 with the vaporized high-purity nitrogen 22 from the pure nitrogen tank 15 mixed.

Claims (7)

Verfahren zur Herstellung eines hoch reinen tiefkalten Flüssigprodukts aus einer weniger reinen tiefkalten Einsatzflüssigkeit, bei dem ein erster Strom (6) weniger reiner tiefkalter Einsatzflüssigkeit aus einem Speichertank (1) in eine erste Trennsäule (7) eingeleitet wird, ein zweiter Strom (2) weniger reiner tiefkalter Einsatzflüssigkeit aus dem Speichertank (1) in einem Druckaufbauverdampfer (3) verdampft und in den Speichertank (1) zurückgeleitet (4) wird, eine gasförmige Fraktion (11) aus dem oberen Bereich der ersten Trennsäule (7) in einem Kondensator-Verdampfer (9) verflüssigt und bei dem ein hoch reines Flüssigprodukt (14) gewonnen wird, dadurch gekennzeichnet, dass eine gasförmige Einsatzfraktion (10) aus dem Speichertank (1) entnommen und der ersten Trennsäule (7) zugeleitet wird.Method for producing a highly pure cryogenic liquid product from a less pure cryogenic feed liquid, in which a first stream (6) of less pure cryogenic feed liquid is introduced from a storage tank (1) into a first separation column (7), a second stream (2) less Pure cryogenic feed liquid from the storage tank (1) is evaporated in a pressure build-up evaporator (3) and returned to the storage tank (1) (4), a gaseous fraction (11) from the upper area of the first separation column (7) in a condenser-evaporator (9) liquefied and in which a highly pure liquid product (14) is obtained, characterized in that a gaseous feed fraction (10) is removed from the storage tank (1) and fed to the first separation column (7). Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass ein Druckgasstrom (23, 26) aus einer äußeren Quelle in den Speichertank (1) eingeleitet wird.A method according to claim 1, characterized in that a compressed gas stream (23, 26) from an external source is introduced into the storage tank (1). Verfahren nach Anspruch 1 oder 5, dadurch gekennzeichnet, dass in dem Druckaufbauverdampfer aus tiefkalter Flüssigkeit erzeugter Dampf (4) und/oder der Druckgasstrom (26) vor seiner Einleitung in den Speichertank (1) in indirekten Wärmeaustausch (5) mit der im Speichertank (1) befindlichen tiefkalten Einsatzflüssigkeit gebracht wird.Method according to Claim 1 or 5, characterized in that steam (4) and / or the compressed gas stream (26) generated in the pressure build-up evaporator from cryogenic liquid before it is introduced into the storage tank (1) in indirect heat exchange (5) with that in the storage tank ( 1) located cryogenic feed liquid is brought. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass eine flüssige Fraktion (17) aus dem unteren Bereich der ersten Trennsäule (7) abgezogen und zur Kühlung des Kondensator-Verdampfers (9) eingesetzt wird.Method according to one of claims 1 to 3, characterized in that a liquid fraction (17) is drawn off from the lower region of the first separation column (7) and used to cool the condenser-evaporator (9). Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass die flüssige Fraktion (17) in eine zweite Trennsäule (8) eingeleitet wird und der Kondensator-Verdampfer (9) als Aufkocher der zweiten Trennsäule ausgebildet ist.A method according to claim 4, characterized in that the liquid fraction (17) is introduced into a second separation column (8) and the condenser-evaporator (9) is designed as a reboiler of the second separation column. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, dass keine Verdichter oder Pumpen eingesetzt werden. Method according to one of claims 1 to 5, characterized in that no compressors or pumps are used. Vorrichtung zur Herstellung eines hoch reinen tiefkalten Flüssigprodukts aus einer weniger reinen tiefkalten Einsatzflüssigkeit mit einem Speichertank (1) für weniger reine tiefkalte Einsatzflüssigkeit, mit einer Flüssigkeitsleitung (6) zur Einleitung eines ersten Stroms weniger reiner tiefkalter Einsatzflüssigkeit aus einem Speichertank (1) in eine erste Trennsäule (7), mit einem Druckaufbausystem (2, 3, 4, 5), das einen Druckaufbauverdampfer (3) zur Verdampfung eines zweiten Stroms weniger reiner tiefkalter Einsatzflüssigkeit aus dem Speichertank (1) aufweist, mit einem Kondensator-Verdampfer (9) zur Verflüssigung einer gasförmigen Fraktion (11) aus dem oberen Bereich der ersten Trennsäule (7) und mit einer Produktleitung (14) für hoch reines Flüssigprodukt, gekennzeichnet durch eine Gasleitung (10) zur Überleitung einer gasförmigen Einsatzfraktion aus dem Speichertank (1) in die erste Trennsäule (7).Device for producing a highly pure cryogenic liquid product from a less pure cryogenic feed liquid with a storage tank (1) for less pure cryogenic feed liquid, with a liquid line (6) for introducing a first stream of less pure cryogenic feed liquid from a storage tank (1) into a first Separating column (7), with a pressure build-up system (2, 3, 4, 5), which has a pressure build-up evaporator (3) for evaporating a second stream of less pure cryogenic feed liquid from the storage tank (1), with a condenser-evaporator (9) Liquefaction of a gaseous fraction (11) from the upper area of the first separation column (7) and with a product line (14) for highly pure liquid product, characterized by a gas line (10) for transferring a gaseous feed fraction from the storage tank (1) into the first Separation column (7).
EP02024690A 2001-11-28 2002-11-05 Process and device for the production of an ultra high purity liquid from a cryogenic liquid feed with lower purity Withdrawn EP1316768A1 (en)

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