EP0628777B1 - Process and apparatus for obtaining argon - Google Patents

Process and apparatus for obtaining argon Download PDF

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Publication number
EP0628777B1
EP0628777B1 EP94107374A EP94107374A EP0628777B1 EP 0628777 B1 EP0628777 B1 EP 0628777B1 EP 94107374 A EP94107374 A EP 94107374A EP 94107374 A EP94107374 A EP 94107374A EP 0628777 B1 EP0628777 B1 EP 0628777B1
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Prior art keywords
column
argon
fraction
crude argon
semipure
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EP94107374A
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German (de)
French (fr)
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EP0628777A1 (en
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Horst Dipl.-Ing. Corduan
Hartwin Dipl.-Ing. Lindner
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Linde GmbH
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Linde GmbH
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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
    • F25J3/04151—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
    • F25J3/0423—Subcooling of liquid process streams
    • 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
    • F25J3/04406—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 using a dual pressure main column system
    • F25J3/04412—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 using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • 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
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
    • 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
    • F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
    • F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
    • F25J3/04703—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser being arranged in more than one vessel
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/58—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/50—Processes or apparatus involving steps for recycling of process streams the recycled stream being oxygen
    • 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
    • Y10S62/923—Inert gas
    • Y10S62/924—Argon

Definitions

  • the invention relates to a method and a device for the production of argon, wherein in the process air in a rectification system with at least one Air separation column and a raw argon column is disassembled, one containing argon Oxygen fraction removed from the air separation column and into a crude argon column a raw argon fraction is initiated in the upper area of the raw argon column removed and a first reflux liquid to be added and in the lower A first residual fraction is taken from the area of the crude argon column.
  • GB-A-2107597 relates to the separation by distillation of components whose Boiling points are very close together, especially a process for Heavy water enrichment. It is suggested to use this process instead to be carried out in up to four columns in only two serially connected separation columns. Liquid from the first of the two columns is applied to the second column. Steam from the second column is passed through a compressor and a heat exchanger returned to the first pillar.
  • the invention has for its object a method and an apparatus to develop the type mentioned above, which is characterized by particularly high efficiency distinguish, in particular by relatively little equipment for raw argon production.
  • This object is achieved in that the crude argon fraction is in the lower range a semi-pure column is introduced, being in the upper region of the semi-pure column one oxygen-depleted argon fraction was taken and a second Return liquid to be added and in the lower area of the semi-pure column a second residual fraction is removed, which the first return liquid for forms the raw argon column.
  • the return liquid is therefore the liquid of another rectification column formed, into which the crude argon product is conversely introduced. This can help a head capacitor for the raw argon column can be dispensed with.
  • the product fraction from the crude argon column is further oxygenated in the semi-pure column depleted.
  • a semi-pure column By using a semi-pure column, one can essentially oxygen-free argon product can be obtained, the overall height of the Crude argon column is not only reduced by dispensing with a top condenser be, but overall very flexible to the circumstances of the whole Air separation plant can be adapted. It is deliberately avoided to achieve the lowest possible oxygen concentration in the raw argon column. In the context of the invention, it has been found that the invention Process economic benefits by reducing the size of the raw argon column offers, in many cases, against the cost of the additional pillar prevail.
  • the oxygen-depleted argon fraction is used as a product or intermediate withdrawn in gaseous or liquid form. It can, for example in a pure argon column, further cleaned, in particular freed of nitrogen.
  • the pressure in the lower region of the semi-pure column is preferably essentially equal to the pressure in the upper area of the raw argon column.
  • the return liquid for the semi-pure column can basically by condensation the corresponding top fraction generated or supplied from another source will.
  • At least part of the argon fraction is from the upper region the semi-pure column condensed by indirect heat exchange, at least part of the condensate forms the second return liquid.
  • a top condenser is arranged above the rectification area of the semi-pure column.
  • the liquid evaporating against the condensing argon fraction Fraction preferably through oxygen-enriched liquid from the pressure column educated.
  • the evaporated liquid fraction is then in the low pressure column fed.
  • This variant of the method according to the invention for example in the case of sump liquid from the pressure column for condensation of the depleted argon fraction is particularly energetically favorable.
  • the evaporation of the liquid In this case, fraction preferably takes place under essentially low-pressure column pressure or under a slightly higher pressure.
  • Packings and / or ordered ones are preferably used in the crude argon and / or semi-pure column Packs used as mass transfer elements. Because of her special Orderly packs are preferred with low pressure loss. Even in the other rectification columns used in the process, for example in the Low-pressure column of a two-stage air separator can fill or packing, in particular ordered packs can be used.
  • any ordered pack can be used will.
  • the use of internals such as those in the not previously published documents WO 93/19335 or WO 93/19336 are.
  • the invention also relates to a device for the production of argon according to the Claims 8 to 13.
  • an argon-containing oxygen stream 4 is removed, the also contaminants in the form of nitrogen and other air components contains, and in a raw argon column 5 in raw argon 6 and a first residual fraction 8 Cut.
  • the latter - if necessary by means of a pump, not shown - for Low pressure column 3 returned and slightly below the point of removal for the oxygen flow containing argon is fed back.
  • crude argon 6 obtained at the top of the crude argon column 5 a semi-pure column 9 a further rectification step for the removal of less volatile Proportions, especially of oxygen, subjected.
  • the raw argon becomes this preferably fed into the lower region of this column 9 in gaseous form.
  • oxygen depleted argon is from the upper area of the semi-pure column 9 withdrawn in gaseous (10) and / or liquid (15).
  • Return liquid 11 for the semi-pure column is obtained by condensation of the top fraction by means of indirect heat exchange 13 against relaxed sump liquid from the Pressure column 2 of the air separator 1 generated.
  • the resulting steam is over Line 16 discharged and introduced into the low-pressure column 3 at a suitable point.
  • the crude argon column 5 does not require a top condenser. Your need for return liquid 7 is covered by sump liquid 12, which is in the semi-pure column 9 arises. As a rule, a pump 17 must be used to compensate for the height difference to overcome in line 7.
  • the rectification areas shown throughout in the drawing consist of Reality from multiple sections.
  • mass transfer elements especially in Crude argon and semi-pure column preferably used ordered packs. It However, parts of the columns with conventional rectification trays can also be used be equipped.
  • the crude argon column has a rectification section on, the semi-pure column three.
  • the number of these sections can, however vary in the crude argon column from one to about three, in the semi-pure column about from two to six.
  • the crude argon column 5 contains, for example, 30 to 120, preferably about 60 to 90 theoretical floors.
  • the number of theoretical plates in the semi-pure column 9 is, for example, 60 to 150, preferably about 90 to 120.
  • the ratio of theoretical plate numbers (crude argon column 5 to semi-pure column 9) is, for example 0.5.

Description

Die Erfindung betrifft ein Verfahren und eine Vorrichtung zur Gewinnung von Argon, wobei in dem Verfahren Luft in einem Rektifiziersystem mit mindestens einer Luftzerlegersäule und einer Rohargonsäule zerlegt wird, wobei eine argonhaltige Sauerstofffraktion aus der Luftzerlegersäule entnommen und in eine Rohargonsäule eingeleitet wird, im oberen Bereich der Rohargonsäule eine Rohargonfraktion entnommen und eine erste Rücklaufflüssigkeit aufgegeben werden und im unteren Bereich der Rohargonsäule eine erste Restfraktion entnommen wird.The invention relates to a method and a device for the production of argon, wherein in the process air in a rectification system with at least one Air separation column and a raw argon column is disassembled, one containing argon Oxygen fraction removed from the air separation column and into a crude argon column a raw argon fraction is initiated in the upper area of the raw argon column removed and a first reflux liquid to be added and in the lower A first residual fraction is taken from the area of the crude argon column.

Derartige Verfahren und Anlagen zur Gewinnung von Rohargon sind allgemein aus der Fachliteratur bekannt (beispielsweise aus Hausen/Linde, Tieftemperaturtechnik, 2. Auflage, Kapitel 4.5.4.1; Winnacker/Küchler, Chemische Technologie, Band 2, 3. Auflage, Kapitel 5.231.; Latimer, Distillation of Air, Chem. Eng. Progr., 63, Seiten 35 bis 59). Bei solchen Prozessen wird im Anschluß an eine zweistufige Luftzerlegung Rohargon in einer Rohargonsäule gewonnen, die mit der Niederdrucksäule des Luftzerlegers verbunden ist. Seltener wird die Rohargongewinnung mit einer Einzelsäule zur Stickstoff- und/oder Sauerstoffgewinnung gekoppelt. Die Rücklaufflüssigkeit für die Rohargonsäule wird in einem Kopfkondensator erzeugt, der am oberen Ende dieser Säule angeordnet ist.Such methods and plants for the production of raw argon are generally known from the specialist literature (for example from Hausen / Linde, low temperature technology, 2nd edition, chapter 4.5.4.1; Winnacker / Küchler, Chemische Technologie, volume 2, 3rd edition, chapter 5.231 .; Latimer, Distillation of Air, Chem. Eng. Progr., 63 , pages 35 to 59). In such processes, after a two-stage air separation, raw argon is obtained in a raw argon column, which is connected to the low pressure column of the air separator. Rarely, crude argon production is coupled with a single column for nitrogen and / or oxygen production. The return liquid for the crude argon column is generated in a top condenser, which is arranged at the upper end of this column.

Aus der EP-B-377 117 ist ein spezielles Verfahren dieser Art bekannt, das eine besonders hohe Anzahl von theoretischen Böden in der Rohargonsäule sowie den Einsatz von Füllkörpern oder Packungen in der Rohargonsäule vorsieht. Auf diese Weise ist es möglich, sehr niedrige Sauerstoffkonzentrationen im Rohargonprodukt zu erlangen. Allerdings wird die Bauhöhe einer Rohargonsäule einschließlich Kopfkondensator beim Einsatz von Packungen, die einer hohen Anzahl von theoretischen Böden entsprechen, sehr groß, so daß sie unter Umständen die Höhe der Luftzerlegersäule(n) zur Sauerstoff- und Stickstoffgewinnung erreicht oder sogar überschreitet. Abgesehen davon, daß solch hohe Säulen zusätzlichen Aufwand für Stabilisierung und exakte vertikale Ausrichtung erfordern, kann dadurch eine aufwendige Gestaltung der isolierenden Ummantelung der Rektifiziersäulen (Cold box) notwendig werden. From EP-B-377 117 a special method of this type is known, the one particular high number of theoretical plates in the raw argon column as well as the Use of packing elements or packings in the raw argon column. To this It is possible to produce very low oxygen concentrations in the crude argon product to get. However, the overall height of a crude argon column including overhead condenser when using packs that have a high number of theoretical Soils correspond to very large, so that they may be the height of the Air separation column (s) for oxygen and nitrogen extraction reached or even exceeds. Apart from the fact that such high pillars require additional effort for Require stabilization and exact vertical alignment can be a complex process Design of the insulating sheathing of the rectification columns (cold box) become necessary.

Die bekannten Verfahren und Vorrichtungen sind daher nicht in allen Fällen zufriedenstellend, insbesondere bei großer Anzahl von theoretischen Böden und/oder dem Einsatz von Füllkörpern oder Packungen in der Rohargonsäule.The known methods and devices are therefore not satisfactory in all cases, especially with a large number of theoretical floors and / or the use of packing or packing in the raw argon column.

GB-A-2107597 betrifft die destillative Trennung von Komponenten, deren Siedepunkte sehr dicht zusammenliegen, insbesondere einen Prozeß zur Anreicherung von schwerem Wasser. Es wird vorgeschlagen, diesen Prozeß anstatt in bis zu vier Kolonnen in nur zwei seriell verbundenen Trennsäulen durchzuführen. Flüssigkeit aus der ersten der beiden Säulen wird auf die zweite Säule aufgegeben. Dampf aus der zweiten Säule wird über einen Verdichter und einen Wärmetauscher in die erste Säule zurückgeführt.GB-A-2107597 relates to the separation by distillation of components whose Boiling points are very close together, especially a process for Heavy water enrichment. It is suggested to use this process instead to be carried out in up to four columns in only two serially connected separation columns. Liquid from the first of the two columns is applied to the second column. Steam from the second column is passed through a compressor and a heat exchanger returned to the first pillar.

Der Erfindung liegt die Aufgabe zugrunde, ein Verfahren und eine Vorrichtung der eingangs genannten Art zu entwickeln, die sich durch besonders hohe Wirtschaftlichkeit auszeichnen, insbesondere durch relativ geringen apparativen Aufwand für die Rohargongewinnung.The invention has for its object a method and an apparatus to develop the type mentioned above, which is characterized by particularly high efficiency distinguish, in particular by relatively little equipment for raw argon production.

Diese Aufgabe wird dadurch gelöst, daß die Rohargonfraktion in den unteren Bereich einer Halbreinsäule eingeleitet wird, wobei im oberen Bereich der Halbreinsäule eine an Sauerstoff abgereicherte Argonfraktion entnommen und eine zweite Rücklaufflüssigkeit aufgegeben werden und im unteren Bereich der Halbreinsäule eine zweite Restfraktion entnommen wird, welche die erste Rücklaufflüssigkeit für die Rohargonsäule bildet.This object is achieved in that the crude argon fraction is in the lower range a semi-pure column is introduced, being in the upper region of the semi-pure column one oxygen-depleted argon fraction was taken and a second Return liquid to be added and in the lower area of the semi-pure column a second residual fraction is removed, which the first return liquid for forms the raw argon column.

Die Rücklaufflüssigkeit wird also durch die Flüssigkeit einer weiteren Rektifiziersäule gebildet, in die umgekehrt das Rohargonprodukt eingeleitet wird. Dadurch kann auf einen Kopfkondensator für die Rohargonsäule verzichtet werden.The return liquid is therefore the liquid of another rectification column formed, into which the crude argon product is conversely introduced. This can help a head capacitor for the raw argon column can be dispensed with.

Die Produktfraktion aus der Rohargonsäule wird in der Halbreinsäule weiter an Sauerstoff abgereichert. Durch die Verwendung einer Halbreinsäule kann ein im wesentlichen sauerstofffreies Argonprodukt gewonnen werden, wobei die Bauhöhe der Rohargonsäule nicht nur durch den Verzicht auf einen Kopfkondensator verringert werden, sondern auch insgesamt sehr flexibel an die Gegebenheiten der gesamten Luftzerlegungsanlage angepaßt werden kann. Es wird bewußt darauf verzichtet, schon in der Rohargonsäule die kleinstmögliche Sauerstoffkonzentration zu erreichen. Im Rahmen der Erfindung hat es sich herausgestellt, daß das erfindungsgemäße Verfahren wirtschaftliche Vorteile durch die Verringerung der Größe der Rohargonsäule bietet, die in vielen Fällen gegenüber den Kosten der zusätzlichen Säule überwiegen.The product fraction from the crude argon column is further oxygenated in the semi-pure column depleted. By using a semi-pure column, one can essentially oxygen-free argon product can be obtained, the overall height of the Crude argon column is not only reduced by dispensing with a top condenser be, but overall very flexible to the circumstances of the whole Air separation plant can be adapted. It is deliberately avoided to achieve the lowest possible oxygen concentration in the raw argon column. In the context of the invention, it has been found that the invention Process economic benefits by reducing the size of the raw argon column offers, in many cases, against the cost of the additional pillar prevail.

Die sauerstoffabgereicherte Argonfraktion wird als Produkt oder Zwischenprodukt gasförmig oder flüssig abgezogen. Sie kann, beispielsweise in einer Reinargonsäule, weiter gereinigt, insbesondere von Stickstoff befreit werden. The oxygen-depleted argon fraction is used as a product or intermediate withdrawn in gaseous or liquid form. It can, for example in a pure argon column, further cleaned, in particular freed of nitrogen.

Vorzugsweise ist der Druck im unteren Bereich der Halbreinsäule im wesentlichen gleich dem Druck im oberen Bereich der Rohargonsäule.The pressure in the lower region of the semi-pure column is preferably essentially equal to the pressure in the upper area of the raw argon column.

In beiden Säulen herrscht also praktisch derselbe Druck. Die Forderung nach im wesentlichen gleichem Druck am Kopf der Rohargonsäule und am Boden der Halbreinsäule schließt gewisse Differenzen (beispielsweise durch den Druckabfall längs der Rohargonleitung) nicht aus. Insgesamt sollen sie jedoch nicht so groß sein, daß in der Rohargonleitung vom Kopf der Rohargonsäule zum Boden der Halbreinsäule spezielle Vorrichtungen zur Druckerhöhung oder -Verminderung (beispielsweise Verdichter oder Drosselventile) eingesetzt werden müssen. Gegebenenfalls muß eine Pumpe zur Förderung der ersten Rücklaufflüssigkeit verwendet werden.So there is practically the same pressure in both pillars. The call for essentially same pressure at the top of the raw argon column and at the bottom of the semi-pure column closes certain differences (e.g. due to the pressure drop along the Raw argon line) is not sufficient. Overall, however, they should not be so large that in the Raw argon line from the top of the raw argon column to the bottom of the semi-pure column special devices for increasing or reducing pressure (for example Compressors or throttle valves) must be used. If necessary, a Pump used to deliver the first return liquid.

Die Rücklaufflüssigkeit für die Halbreinsäule kann grundsätzlich durch Kondensation der entsprechenden Kopffraktion erzeugt oder aus einer anderen Quelle zugeführt werden.The return liquid for the semi-pure column can basically by condensation the corresponding top fraction generated or supplied from another source will.

Vorzugsweise wird mindestens ein Teil der Argonfraktion aus dem oberen Bereich der Halbreinsäule durch indirekten Wärmeaustausch kondensiert, wobei mindestens ein Teil des Kondensats die zweite Rücklaufflüssigkeit bildet. Dazu wird in der Regel oberhalb des Rektifizierbereichs der Halbreinsäule ein Kopfkondensator angeordnet.Preferably at least part of the argon fraction is from the upper region the semi-pure column condensed by indirect heat exchange, at least part of the condensate forms the second return liquid. This is usually done A top condenser is arranged above the rectification area of the semi-pure column.

Dabei ist es insbesondere günstig, wenn bei dem indirekten Wärmeaustausch ein Prozeßstrom des Verfahrens, vorzugsweise eine flüssige Fraktion aus einer der Luftzerlegersäulen, verdampft wird. Externe Kälte für die Kühlung der Halbreinsäule wird damit nicht benötigt.It is particularly advantageous if an indirect heat exchange Process stream of the process, preferably a liquid fraction from one of the Air separation columns, is evaporated. External cooling for cooling the semi-pure column is therefore not required.

Im Falle eines Doppelsäulen-Luftzerlegungsverfahrens, falls also die Luftzerlegersäule zweistufig ausgebildet ist und eine Drucksäule und eine Niederdrucksäule aufweist (hierbei wird die argonhaltige Sauerstofffraktion der Niederdrucksäule entnommen), wird die gegen kondensierende Argonfraktion verdampfende flüssige Fraktion vorzugsweise durch sauerstoffangereicherte Flüssigkeit aus der Drucksäule gebildet. Die verdampfte flüssige Fraktion wird anschließend in die Niederdrucksäule eingespeist.In the case of a double column air separation process, i.e. if the air separation column is formed in two stages and a pressure column and a low pressure column (the argon-containing oxygen fraction of the low pressure column removed), the liquid evaporating against the condensing argon fraction Fraction preferably through oxygen-enriched liquid from the pressure column educated. The evaporated liquid fraction is then in the low pressure column fed.

Diese Variante des erfindungsgemäßen Verfahrens, bei der beispielsweise Sumpfflüssigkeit aus der Drucksäule zur Kondensation der abgereicherten Argonfraktion verwendet wird, ist energetisch besonders günstig. Die Verdampfung der flüssigen Fraktion findet in diesem Fall vorzugsweise unter im wesentlichen Niederdrucksäulendruck oder unter einem geringfügig höheren Druck statt.This variant of the method according to the invention, for example in the case of sump liquid from the pressure column for condensation of the depleted argon fraction is particularly energetically favorable. The evaporation of the liquid In this case, fraction preferably takes place under essentially low-pressure column pressure or under a slightly higher pressure.

Vorzugsweise werden in Rohargon- und/oder Halbreinsäule Füllkörper und/oder geordnete Packungen als Stoffaustauschelemente eingesetzt. Wegen ihres besonders geringen Druckverlustes werden dabei geordnete Packungen bevorzugt. Auch in den übrigen in dem Verfahren eingesetzten Rektifiziersäulen, beispielsweise in der Niederdrucksäule eines zweistufigen Luftzerlegers können Füllkörper oder Packungen, insbesondere geordnete Packungen, eingesetzt werden.Packings and / or ordered ones are preferably used in the crude argon and / or semi-pure column Packs used as mass transfer elements. Because of her special Orderly packs are preferred with low pressure loss. Even in the other rectification columns used in the process, for example in the Low-pressure column of a two-stage air separator can fill or packing, in particular ordered packs can be used.

Beim erfindungsgemäßen Verfahren kann grundsätzlich jede geordnete Packung verwendet werden. Günstig ist beispielsweise der Einsatz von Einbauten, wie sie in den nicht vorveröffentlichten Dokumenten WO 93/19335 oder WO 93/19336 beschrieben sind.In the method according to the invention, in principle any ordered pack can be used will. For example, the use of internals such as those in the not previously published documents WO 93/19335 or WO 93/19336 are.

Auch der kombinierte Einsatz verschiedener Arten von Stoffaustauschelementen (konventionelle Rektifizierböden, ungeordnete Füllkörper, geordnete Packungen) ist in jeder der in dem Verfahren eingesetzten Säulen möglich. Dadurch kann beispielsweise der Druckverlust längs einer Säule genau den spezifischen Bedürfnissen des jeweiligen Prozesses angepaßt werden.Also the combined use of different types of mass transfer elements (conventional rectification trays, disordered packing, ordered packing) is in any of the columns used in the process possible. This can, for example the pressure loss along a column exactly the specific needs be adapted to the respective process.

Die Erfindung betrifft außerdem eine Vorrichtung zur Gewinnung von Argon nach den Patentansprüchen 8 bis 13.The invention also relates to a device for the production of argon according to the Claims 8 to 13.

Im folgenden werden die Erfindung sowie weitere Einzelheiten der Erfindung anhand eines in der Zeichnung schematisch dargestellten Ausführungsbeispiels näher erläutert.The invention and further details of the invention are described below of an embodiment schematically illustrated in the drawing.

Im linken Teil der Zeichnung ist ein Luftzerlegungsverfahren zur Erzeugung von Sauerstoff und Stickstoff mit einer Doppelsäule 1, die aus einer Drucksäule 2 und einer Niederdrucksäule 3 besteht, angedeutet. Die Erfindung hängt jedoch nicht von der speziellen Gestaltung dieses Verfahrensabschnittes ab, sondern ist auch auf andere Ausprägungen dieses Teils des Verfahrens beziehungsweise der Vorrichtung anwendbar, beispielsweise auf eine Anlage mit einer Einzelsäule oder auf abweichende Arten der Produktentnahme von Stickstoff und Sauerstoff. Details wie Turbinen zur kälteleistenden Entspannung von Prozeßströmen oder die Direkteinspeisung von Luft in die Niederdrucksäule sind in dem stark vereinfachten Schema nicht dargestellt.In the left part of the drawing is an air separation process for the generation of Oxygen and nitrogen with a double column 1 consisting of a pressure column 2 and a low-pressure column 3, indicated. However, the invention does not depend on the special design of this process section, but is also based on other versions of this part of the method or the device applicable, for example to a system with a single column or to different ones Types of product extraction of nitrogen and oxygen. Details like Turbines for low-temperature relaxation of process streams or direct feed of air into the low pressure column are in the highly simplified scheme not shown.

Im vorliegenden Ausführungsbeispiel wird an einer Stelle relativ hoher Argonkonzentration in der Niederdrucksäule 3 ein argonhaltiger Sauerstoffstrom 4 entnommen, der außerdem Verunreinigungen in Form von Stickstoff und anderen Luftbestandteilen enthält, und in einer Rohargonsäule 5 in Rohargon 6 und eine erste Restfraktion 8 getrennt. Letztere wird - gegebenenfalls mittels einer nicht gezeigten Pumpe - zur Niederdrucksäule 3 zurückgeführt und etwas unterhalb der Entnahmestelle für den argonhaltigen Sauerstoffstrom zurückgespeist.In the present exemplary embodiment there is a relatively high argon concentration at a point in the low-pressure column 3, an argon-containing oxygen stream 4 is removed, the also contaminants in the form of nitrogen and other air components contains, and in a raw argon column 5 in raw argon 6 and a first residual fraction 8 Cut. The latter - if necessary by means of a pump, not shown - for Low pressure column 3 returned and slightly below the point of removal for the oxygen flow containing argon is fed back.

Erfindungsgemäß wird am Kopf der Rohargonsäule 5 gewonnenes Rohargon 6 in einer Halbreinsäule 9 einem weiteren Rektifizierschritt zur Entfernung schwererflüchtiger Anteile, insbesondere von Sauerstoff, unterzogen. Das Rohargon wird dazu vorzugsweise gasförmig in den unteren Bereich dieser Säule 9 eingespeist. An Sauerstoff abgereichertes Argon wird aus dem oberen Bereich der Halbreinsäule 9 gasförmig (10) und/oder flüssig (15) abgezogen.According to the invention, crude argon 6 obtained at the top of the crude argon column 5 a semi-pure column 9 a further rectification step for the removal of less volatile Proportions, especially of oxygen, subjected. The raw argon becomes this preferably fed into the lower region of this column 9 in gaseous form. Of oxygen depleted argon is from the upper area of the semi-pure column 9 withdrawn in gaseous (10) and / or liquid (15).

Rücklaufflüssigkeit 11 für die Halbreinsäule wird durch Kondensation der Kopffraktion mittels indirektem Wärmeaustausch 13 gegen entspannte Sumpfflüssigkeit aus der Drucksäule 2 des Luftzerlegers 1 erzeugt. Der dabei entstehende Dampf wird über Leitung 16 abgeführt und an geeigneter Stelle in die Niederdrucksäule 3 eingeleitet.Return liquid 11 for the semi-pure column is obtained by condensation of the top fraction by means of indirect heat exchange 13 against relaxed sump liquid from the Pressure column 2 of the air separator 1 generated. The resulting steam is over Line 16 discharged and introduced into the low-pressure column 3 at a suitable point.

Die Rohargonsäule 5 bedarf dagegen keines Kopfkondensators. Ihr Bedarf an Rücklaufflüssigkeit 7 wird durch Sumpfflüssigkeit 12 gedeckt, die in der Halbreinsäule 9 anfällt. In der Regel muß eine Pumpe 17 eingesetzt werden, um den Höhenunterschied in der Leitung 7 zu überwinden.In contrast, the crude argon column 5 does not require a top condenser. Your need for return liquid 7 is covered by sump liquid 12, which is in the semi-pure column 9 arises. As a rule, a pump 17 must be used to compensate for the height difference to overcome in line 7.

Die in der Zeichnung durchgehend dargestellten Rektifizierbereiche bestehen in der Realität aus mehreren Abschnitten. Als Stoffaustauschelemente werden - vor allem in Rohargon- und Halbreinsäule vorzugsweise geordnete Packungen eingesetzt. Es können jedoch auch Teile der Säulen mit konventionellen Rektifizierböden ausgestattet sein.The rectification areas shown throughout in the drawing consist of Reality from multiple sections. As mass transfer elements - especially in Crude argon and semi-pure column preferably used ordered packs. It However, parts of the columns with conventional rectification trays can also be used be equipped.

In dem konkreten Beispiel der Zeichnung weist die Rohargonsäule einen Rektifizierabschnitt auf, die Halbreinsäule drei. Die Zahl dieser Abschnitte kann jedoch variieren, in der Rohargonsäule von eins bis etwa drei, in der Halbreinsäule etwa von zwei bis sechs.In the concrete example of the drawing, the crude argon column has a rectification section on, the semi-pure column three. The number of these sections can, however vary in the crude argon column from one to about three, in the semi-pure column about from two to six.

Die Rohargonsäule 5 enthält beispielsweise 30 bis 120, vorzugsweise etwa 60 bis 90 theoretische Böden. Die Anzahl an theoretischen Böden in der Halbreinsäule 9 beträgt beispielsweise 60 bis 150, vorzugsweise etwa 90 bis 120. Das Verhältnis der theoretischen Bodenzahlen (Rohargonsäule 5 zu Halbreinsäule 9) beträgt beispielsweise 0,5 .The crude argon column 5 contains, for example, 30 to 120, preferably about 60 to 90 theoretical floors. The number of theoretical plates in the semi-pure column 9 is, for example, 60 to 150, preferably about 90 to 120. The ratio of theoretical plate numbers (crude argon column 5 to semi-pure column 9) is, for example 0.5.

Die Sauerstoffkonzentrationen haben in den verschiedenen Strömen beispielsweise folgende Werte:

Übergangsfraktion 4
82 bis 92, vorzugsweise etwa 86 bis 90 %
Rohargonfraktion 6
0,1 bis 2,0, vorzugsweise etwa 0,5 bis 1,0 %
Argonfraktion 10
0,01 bis 10, vorzugsweise etwa 0,01 bis 0,1 ppm
The oxygen concentrations in the different streams have, for example, the following values:
Transitional fraction 4
82 to 92, preferably about 86 to 90%
Raw argon fraction 6
0.1 to 2.0, preferably about 0.5 to 1.0%
Argon fraction 10
0.01 to 10, preferably about 0.01 to 0.1 ppm

Claims (13)

  1. Process for producing argon, in which air is fractionated in a rectifying system having at least one air fractionation column (1) and a crude argon column, an argon-containing oxygen fraction (4) being withdrawn from the air fractionation column (1) and introduced into a crude argon column (5), a crude argon fraction (6) being withdrawn and a first reflux liquid (7) being applied in the upper area of the crude argon column (5), and a first residue fraction (8) being withdrawn in the lower area of the crude argon column (5), characterized in that the crude argon fraction (6) is introduced into the lower area of a semipure column (9), an oxygen-depleted argon fraction being withdrawn (10, 15) and a second reflux liquid (11) being applied in the upper area of the semipure column (9) and a second residue fraction (12) being withdrawn in the lower area of the semipure column (9), which second residue fraction forms the first reflux liquid (7) for the crude argon column (5).
  2. Process according to Claim 1, characterized in that the pressure in the lower area of the semipure column (9) is essentially equal to the pressure in the upper area of the crude argon column (5).
  3. Process according to Claim 1 or 2, characterized in that at least a portion of the argon fraction from the upper area of the semipure column (9) is condensed by indirect heat exchange (13) and at least a portion of the condensate forms the second reflux liquid (11).
  4. Process according to Claim 3, characterized in that in the indirect heat exchange (13) a liquid fraction (14) from one of the air fractionation columns (1; 2) is evaporated.
  5. Process according to Claim 4, characterized in that the air fractionation column (1) is constructed as a double column and has a pressure column (2) and a low-pressure column (3), the argon-containing oxygen fraction (4) being withdrawn from the low-pressure column (3), the liquid fraction evaporating against condensing argon fraction being formed by oxygen-enriched liquid (14) from the pressure column (2) and the vaporized liquid fraction (16) being fed into the low-pressure column (3).
  6. Process according to one of Claims 1 to 5, characterized in that the crude argon column (5) comprises dumped packings and/or arranged packings.
  7. Process according to one of Claims 1 to 6, characterized in that the semipure column (9) comprises dumped packings and/or arranged packings.
  8. Apparatus for producing argon having a rectifying system which possesses at least one air fractionation column (1) and a crude argon column (5), air fractionation column (1) and crude argon column (5) being connected via a line (4) for an argon-containing oxygen fraction, characterized by a semipure column (9), a crude argon line (6) which leads from the upper area of the crude argon column (5) to the lower area of the semipure column (9), and means (7; 11) for feeding reflux liquid into the upper areas of crude argon column (5) and semipure column (9) and having residue fraction lines (8; 12) which lead out of the lower areas of crude argon column (5) and semipure column (9), respectively, the residue fraction line (12) of the semipure column (9) being connected to the means (7) for feeding reflux liquid into the crude argon column (5).
  9. Apparatus according to Claim 8, characterized in that the crude argon line (6) possesses no means for decreasing or increasing the pressure.
  10. Apparatus according to Claim 8 or 9, characterized by a top condenser (13) whose condensation side is connected to the upper area of the semipure column (9).
  11. Apparatus according to Claim 10, characterized by a liquid line which leads from the air fractionation column (1) to the evaporation side of the top condenser (13).
  12. Apparatus according to one of Claims 8 to 11, characterized in that the crude argon column (5) comprises dumped packings and/or arranged packings.
  13. Apparatus according to one of Claims 8 to 12, characterized in that the semipure column (9) comprises dumped packings and/or arranged packings.
EP94107374A 1993-05-28 1994-05-11 Process and apparatus for obtaining argon Expired - Lifetime EP0628777B1 (en)

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ES2125370T3 (en) 1999-03-01
DE4317916A1 (en) 1994-12-01

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