EP3992560A1 - Method for designing a cryogenic separation plant with argon production - Google Patents
Method for designing a cryogenic separation plant with argon production Download PDFInfo
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- EP3992560A1 EP3992560A1 EP21020277.6A EP21020277A EP3992560A1 EP 3992560 A1 EP3992560 A1 EP 3992560A1 EP 21020277 A EP21020277 A EP 21020277A EP 3992560 A1 EP3992560 A1 EP 3992560A1
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- Prior art keywords
- argon
- column
- crude argon
- crude
- waste
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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
- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
- F25J3/04812—Different modes, i.e. "runs" of operation
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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
- F25J3/04406—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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04721—Producing pure argon, e.g. recovered from a crude argon column
- F25J3/04727—Producing pure argon, e.g. recovered from a crude argon column using an auxiliary pure argon column for nitrogen rejection
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
- F25J2200/94—Details relating to the withdrawal point
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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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/58—Processes or apparatus involving steps for recycling of process streams the recycled stream being argon or crude argon
Definitions
- the invention relates to a method for designing a cryogenic decomposition plant with argon production according to the preamble of patent claim 1.
- Such plants are usually designed in such a way that all of the argon contained in the air, at least at least 80% of it, is obtained at the top of the crude argon column as practically oxygen-free crude argon with an oxygen content of about 1 ppm.
- This oxygen-free crude argon then only has to be fed into a pure argon column, in which the remaining nitrogen is removed. High purity argon product can then be obtained from the pure argon column.
- a fake crude argon column also known as a dummy crude argon column
- This is then actually treated as waste and removed from the plant without being used as a material. It's just a matter of keeping the argon out of the oxygen product.
- WO 2016058666 A1 deals with varying argon requirements with constant oxygen or nitrogen requirements.
- a waste argon stream is occasionally removed from the top of the crude argon column or from an intermediate draw, in order to still carry out the argon separation when the argon requirement is relatively low, since the argon that has not been separated would otherwise back up into the low-pressure column and lead to higher energy consumption. In this case, this additional argon must be separated off in the low-pressure column.
- the object of the present invention is to find a particularly cost-effective solution for a permanently reduced argon requirement.
- the complete amount of argon (or the same amount compared to the usual design) is drawn off from the crude argon column during operation.
- the capacity of the crude argon column is only dimensioned for a smaller amount of argon.
- WO 2016058666 A1 a crude argon column with a significantly smaller diameter or with a significantly smaller number of theoretical plates or with both a smaller diameter and a reduced number of plates.
- the air separation plant which was designed by the process according to the invention, appears similar to that in WO 2016058666 A1 ; with the same design air quantity, however, the invention results in a significantly reduced crude argon rectification, which leads to corresponding savings in the construction and operation of the system.
- the rectification in the uppermost part of the crude argon column in the invention can take place with a higher reflux ratio than the recovery of the low-oxygen crude argon product. This reduces the conversion in the crude argon column and the top condenser of the crude argon column can be designed for a correspondingly lower conversion and can therefore be made smaller.
- the number of theoretical plates in the crude argon column (single-part or multi-part) in the invention is 140 to 200 theoretical plates, preferably 150 to 180 theoretical plates, for example 160 to 175 theoretical plates. Further details of the effect of the invention are explained according to the exemplary embodiments using a diagram. The invention also brings about advantages in terms of equipment complexity. The top condenser and the crude argon column can thus be made smaller.
- the intermediate point at which the argon waste vent is located is preferably between the 20th and the 90th theoretical plate (counting from the bottom of the crude argon column).
- the crude argon column is designed in one piece, for example, ie all theoretical plates are arranged in a continuous container.
- the crude argon column can be constructed in several parts and have a first and a second part which are arranged in different containers. The argon waste draw is then arranged on the first part, which has, for example, 60 to 90 theoretical plates.
- the two or more parts of the crude argon column are connected in series in terms of distillation technology, but can be arranged mechanically next to one another.
- the oxygen content in the waste argon is between 0.1 and 10 mol%.
- a gaseous crude argon fraction 71 is removed from the top of the crude argon column 81, more precisely from the liquefaction space of the top condenser 90, and introduced into the pure argon column 83 in gaseous form.
- a liquid pure argon product stream 72 (LAR) is removed from the bottom of the pure argon column 83 .
- a residual gas stream 73 is drawn off from the top condenser 91 (designed here as a bath evaporator) of the pure argon column 83 and blown off into the atmosphere (ATM).
- a gaseous argon waste stream 103 is formed by some or all of the crude argon fraction 71 and removed from the system.
- an argon waste stream is taken from the lower region, in particular at 20 to 90 theoretical plates, for example at 50 theoretical plates.
- This waste stream is also continuously removed. It preferably contains 5 to 70%, for example 52%, of the argon contained in the feed air and has an oxygen concentration of 0.1 to 10 mol%, for example 2.5 mol%.
- the argon waste stream is preferably fed to the main heat exchanger (not shown), either separately or mixed with an impure nitrogen stream from the low pressure column, and then vented to atmosphere or used as regeneration gas.
- the crude argon column of Fig.2b is no different from Fig. 1b .
- the column has a diameter that is hardly smaller than that of Figure 2a is, but significantly fewer internals in the form of packing sections, namely a reduced by about 29% theoretical plate number.
- approximately 52% of the argon contained in the feed air is removed via the argon waste stream 103.
- the crude argon column of Figure 3b has in this embodiment the same diameter as that of the Figure 3a , but has even fewer internals in the form of packing sections compared to the Fig. 1b .
- the discharge of the waste argon via the intermediate draw can also be combined with blowing off a partial amount of oxygen-free argon at the top of the crude argon column.
- the advantage of the invention can only be used in part; In return, argon production can be increased in the future or operated flexibly while still operating in an energy-efficient manner.
- figure 4 is the result of a specific case study created with simulation tools. However, the diagram is also generally useful for description the effect of the invention. It shows the general relationship between the amount of impure argon to be removed (argon waste stream), conversion in the crude argon column (Y-axis) and plate number in the crude argon column (X-axis).
- the curve at the top right describes a waste withdrawal at the top of the crude argon column (with 1 ppm oxygen), the curve at the bottom left describes the case of venting impure argon (72% by mass of the gas rising in the crude argon column when 28% by mass is removed as oxygen-free Crude argon from the top of the crude argon column.
- the physical background is the surprising fact that the withdrawal of waste argon at an intermediate point of the crude argon column can allow a significantly more efficient recovery of an oxygen-poor crude argon product through an increased reflux ratio F/D in the upper part of the crude argon rectification.
- a crude argon product with an oxygen content of about 1 ppm or even less can be realized.
- the invention uses this hitherto unknown relationship and is thus able to separate the same amount of argon with a significantly smaller crude argon column.
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- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
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Abstract
Das Verfahren dient zum Herstellen einer Tieftemperaturzerlegungsanlage mit Argonproduktion. Diese Anlage umfasst ein Destilliersäulensystem, das eine Hochdrucksäule und eine Niederdrucksäule (11) und eine Rohargonsäule. Bei dem Verfahren die Hochdrucksäule und die Niederdrucksäule (11) für eine Design-Einsatzluftmenge ausgelegt, die in einem Normalbetriebsfall in das Destilliersäulensystem eingeleitet wird. Die Rohargonsäule (81) wird für die Gewinnung von höchstens 70 % der in der Design-Einsatzluftmenge enthaltenen Argonmenge am Kopf der Rohargonsäule ausgelegt wird. Der Normalbetriebsfall umfasst das Abziehen eines Teils des in der Rohargonsäule (81) aufsteigenden Gases als Abfallargon (103) an einer Zwischenstelle über einen Argonabfallabzug. The method is used to manufacture a cryogenic decomposition plant with argon production. This plant comprises a distillation column system comprising a high pressure column and a low pressure column (11) and a crude argon column. In the method, the high-pressure column and the low-pressure column (11) are designed for a design input air quantity that is introduced into the distillation column system in normal operating conditions. The crude argon column (81) is designed to extract at most 70% of the amount of argon contained in the design input air volume at the top of the crude argon column. The normal operating case includes withdrawing part of the gas rising in the crude argon column (81) as waste argon (103) at an intermediate point via an argon waste vent.
Description
Die Erfindung betrifft Verfahren zum Auslegen einer Tieftemperaturzerlegungsanlage mit Argonproduktion gemäß dem Oberbegriff von Patentanspruch 1.The invention relates to a method for designing a cryogenic decomposition plant with argon production according to the preamble of patent claim 1.
Solche Anlagen werden üblicherweise so ausgelegt, dass das gesamte in der Luft enthaltene Argon, jedenfalls mindestens 80 % davon, am Kopf der Rohargonsäule als praktisch sauerstofffreies Rohargon mit einem Sauerstoffgehalt von etwa 1 ppm gewonnen wird. Dieses sauerstofffreie Rohargon muss dann nur noch einer Reinargonsäule zugeführt werden, in der verbleibender Stickstoff entfernt wird. Aus der Reinargonsäule kann dann hochreines Argonprodukt gewonnen werden.Such plants are usually designed in such a way that all of the argon contained in the air, at least at least 80% of it, is obtained at the top of the crude argon column as practically oxygen-free crude argon with an oxygen content of about 1 ppm. This oxygen-free crude argon then only has to be fed into a pure argon column, in which the remaining nitrogen is removed. High purity argon product can then be obtained from the pure argon column.
Wird das Argonprodukt nicht benötigt, soll aber das Sauerstoffprodukt einen sehr niedrigen Argongehalt aufweisen, wird häufig eine unechte Rohargonsäule (auch Dummy-Rohargonsäule genannt) eingesetzt, die kein verwertbares Argonprodukt erzeugt, sondern ein Abfallargonprodukt mit etwa 1 bis 25 % Sauerstoffgehalt. Dieses wird dann tatsächlich als Abfall behandelt und aus der Anlage entfernt, ohne stofflich genutzt zu werden. Es geht nur darum, das Argon aus dem Sauerstoffprodukt herauszuhalten.If the argon product is not required, but the oxygen product is to have a very low argon content, a fake crude argon column (also known as a dummy crude argon column) is often used, which does not produce a usable argon product but produces a waste argon product with around 1 to 25% oxygen content. This is then actually treated as waste and removed from the plant without being used as a material. It's just a matter of keeping the argon out of the oxygen product.
Die vorliegende Erfindung hat zur Aufgabe, für einen dauerhaft erniedrigten Argonbedarf eine besonders kostengünstige Lösung zu finden.The object of the present invention is to find a particularly cost-effective solution for a permanently reduced argon requirement.
Diese Aufgabe wird durch die kennzeichnenden Merkmale des Patentanspruchs 1 gelöst.This object is solved by the characterizing features of claim 1.
Dabei wird zwar im Betrieb die vollständige (bzw. die gleiche im Vergleich zur üblichen Auslegung) Argonmenge aus der Rohargonsäule abgezogen. Die Kapazität der Rohargonsäule wird aber nur für eine kleinere Argonmenge dimensioniert. Dies ergibt im Vergleich zu
Im Rahmen der Erfindung hat sich überaschenderweise herausgestellt, dass die Rektifikation im obersten Teil der Rohargonsäule bei der Erfindung mit höherem Rücklaufverhältnis als die Gewinnung des sauerstoffarmen Rohargonprodukts erfolgen kann. Damit wird der Umsatz in der Rohargonsäule reduziert und der Kopfkondensator der Rohargonsäule kann für einen entsprechend niedrigeren Umsatz ausgelegt und damit kleiner gebaut werden.In the context of the invention, it has surprisingly been found that the rectification in the uppermost part of the crude argon column in the invention can take place with a higher reflux ratio than the recovery of the low-oxygen crude argon product. This reduces the conversion in the crude argon column and the top condenser of the crude argon column can be designed for a correspondingly lower conversion and can therefore be made smaller.
Die theoretische Bodenzahl in der Rohargonsäule (einteilig oder mehrteilig) beträgt bei der Erfindung 140 bis 200 theoretische Böden, vorzugsweise 150 bis 180 theoretische Böden, beispielsweise 160 bis 175 theoretische Böden. Weitere Details der Wirkung der Erfindung werden nach den Ausführungsbeispielen anhand eines Diagramms erläutert.
Die Erfindung bewirkt auch Vorteile beim apparativen Aufwand. So können der Kopfkondensator und die Rohargonsäule kleiner gebaut werden.The number of theoretical plates in the crude argon column (single-part or multi-part) in the invention is 140 to 200 theoretical plates, preferably 150 to 180 theoretical plates, for example 160 to 175 theoretical plates. Further details of the effect of the invention are explained according to the exemplary embodiments using a diagram.
The invention also brings about advantages in terms of equipment complexity. The top condenser and the crude argon column can thus be made smaller.
Die Zwischenstelle, an welcher der Argonabfallabzug angeordnet ist, liegt vorzugsweise zwischen dem 20. und dem 90. theoretischen Boden (vom Sumpf der Rohargonsäule her gezählt).The intermediate point at which the argon waste vent is located is preferably between the 20th and the 90th theoretical plate (counting from the bottom of the crude argon column).
Bei der Erfindung ist die Rohargonsäule beispielsweise einteilig ausgebildet, das heißt alle theoretischen Böden sind in einem durchgängigen Behälter angeordnet. Alternativ kann die Rohargonsäule mehrteilig ausgebildet sein und einen ersten und einen zweiten Teil aufweisen, die in verschiedenen Behältern angeordnet sind. Der Argonabfallabzug ist dann am ersten Teil angeordnet, der beispielsweise 60 bis 90 theoretische Böden aufweist. Die zwei oder mehr Teile der Rohargonsäule sind destillationstechnisch seriell verbunden, können aber mechanisch nebeneinander angeordnet werden.In the case of the invention, the crude argon column is designed in one piece, for example, ie all theoretical plates are arranged in a continuous container. Alternatively, the crude argon column can be constructed in several parts and have a first and a second part which are arranged in different containers. The argon waste draw is then arranged on the first part, which has, for example, 60 to 90 theoretical plates. The two or more parts of the crude argon column are connected in series in terms of distillation technology, but can be arranged mechanically next to one another.
Außerdem ist es günstig, wenn gemäß der erfindungsgemäßen Auslegung der Sauerstoffgehalt im Abfallargon zwischen 0,1 und 10 mol% liegt.In addition, it is favorable if, according to the design according to the invention, the oxygen content in the waste argon is between 0.1 and 10 mol%.
Die Erfindung sowie weitere Einzelheiten der Erfindung werden im Folgenden anhand von in der Zeichnungen schematisch dargestellten Ausführungsbeispielen näher erläutert. Die Zeichnungen zeigen nur den Argonteil einer Luftzerlegungsanlage nach dem Stand der Technik und nach der erfindungsgemäßen Auslegung. Der warme Teil, der Hauptwärmetauscher und das Destilliersystem mit Hochdrucksäule und Niederdrucksäule ist jeweils so ausgestaltet, wie es in dem Ausführungsbeispiel zu
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Figuren 1a ,2a ,3a eine konventionelle Argongewinnung mit Abzug von Argonabfall als Rohargon am Kopf der Rohargonsäule, -
Figuren 1b ,2b ,3b jeweils entsprechende Anlagen zur Argongewinnung, die nach der erfindungsgemäßen Methode ausgelegt sind, und -
Figur 4 ein Diagramm zur Erläuterung der Wirkungen der Erfindung.
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Figures 1a ,2a ,3a a conventional argon recovery with withdrawal of argon waste as crude argon at the top of the crude argon column, -
figures 1b ,2 B ,3b in each case corresponding systems for argon production, which are designed according to the method according to the invention, and -
figure 4 a diagram for explaining the effects of the invention.
Die folgende Beschreibung des Argonsystems trifft auf alle Ausführungsbeispiele der
Von dem an sich konventionellen Destilliersäulensystem ist in den Zeichnungen nur ein kleiner Ausschnitt der Niederdrucksäule 11 dargestellt. Ein argonangereicherter Strom 80 aus der Niederdrucksäule 11 wird in eine Rohargonsäule 81 eingeleitet, die in dem Beispiel einteilig ausgebildet ist und 180 theoretische Böden aufweist. Im Kopfkondensator 90 wird Rücklaufflüssigkeit erzeugt. Er ist in den hier dargestellten Ausführungsbeispielen als Rücklaufkondensator ausgebildet, kann aber auch alternativ als Badverdampfer oder Forced-Flow-Verdampfer konstruiert sein. Die Flüssigkeit 84, die sich im Sumpf der Rohargonsäule 81 sammelt, wird gepumpt und über Leitung 6 in die Niederdrucksäule 11 zurückgeleitet.Only a small section of the low-
Vom Kopf der Rohargonsäule 81, genauer aus dem Verflüssigungsraum des Kopfkondensators 90, wird eine gasförmige Rohargonfraktion 71 entnommen und gasförmig in die Reinargonsäule 83 eingeleitet. Vom Sumpf der Reinargonsäule 83 wird ein flüssiger Reinargon-Produktstrom 72 (LAR) entnommen. Vom Kopfkondensator 91 (hier als Badverdampfer ausgebildet) der Reinargonsäule 83 wird ein Restgasstrom 73 abgezogen und in die Atmosphäre (ATM) abgeblasen.A gaseous
In dem System von
Bei dem erfindungsgemäß ausgelegten Verfahren von
Hauptunterschied ist jedoch die unterschiedliche Auslegung der Rohargonsäule bei der Erfindung. Sie wird nur nach der Gasmenge ausgelegt, die nach der Entnahme des Abfallstroms in der Rohargonsäule verbleibt. Dadurch wird sie in dem Beispiel in doppeltem Sinne kleiner, nämlich
- 1. durch eine um ca. 8 % verminderte theoretische Bodenzahl und
- 2. durch einen um ca. 20 % verringerten Durchmesser.
- 1. by a theoretical plate number reduced by approx. 8% and
- 2. By reducing the diameter by around 20%.
Das Beispiel von
Die Rohargonsäule von
Das Beispiel von
Die Rohargonsäule von
Es gilt hier:
1. Um ca. 17 % verminderte theoretische Bodenzahl.
Hier wird ca. 51 % des in der Einsatzluft enthaltenen Argons über den Argonabfallstrom 103 entnommen.It applies here:
1. Theoretical number of plates reduced by approx. 17%.
About 51% of the argon contained in the feed air is removed here via the
Anhand der Ausführungsbeispiele wurde die Ausführung mit dem Rohargon-Zwischenabzug am 50. Boden dargestellt. Es sind jedoch Ausführungen vorstellbar, bei denen der Argonabfallstrom gleich nach dem 20. oder 30. Boden mit etwas höherem Sauerstoffgehalt oder nach dem 70. oder 90. Boden mit etwas niedrigerem Sauerstoffgehalt abgezogen wird. Die genannten Bodenzahlen sind als theoretische Böden zu verstehen.The design with the crude argon intermediate draw-off on the 50th tray was shown on the basis of the exemplary embodiments. However, configurations are conceivable where the argon waste stream is withdrawn just after the 20th or 30th tray with a slightly higher oxygen content, or after the 70th or 90th tray with a slightly lower oxygen content. The plate numbers given are to be understood as theoretical plates.
Das Ableiten vom Abfallargon via Zwischenabzug kann auch mit dem Abblasen einer Teilmenge an sauerstofffreiem Argon am Kopf der Rohargonsäule kombiniert werden. Bei einer solchen Auslegung kann der Vorteil der Erfindung zwar nur zum Teil genutzt werden; dafür kann die Argonproduktion in Zukunft erhöht oder auch flexibel betrieben werden bei einem trotzdem energieeffizientem Anlagenbetrieb.The discharge of the waste argon via the intermediate draw can also be combined with blowing off a partial amount of oxygen-free argon at the top of the crude argon column. With such a design, the advantage of the invention can only be used in part; In return, argon production can be increased in the future or operated flexibly while still operating in an energy-efficient manner.
Physikalischer Hintergrund ist die überraschende Tatsache, dass die Entnahme von Abfallargon an einer Zwischenstelle der Rohargonsäuleeine deutlich effizientere Gewinnung eines sauerstoffarmen Rohargonprodukts durch ein erhöhtes Rücklaufverhältnis F/D im oberen Teil der Rohargonrektifikation erlauben kann. Es kann dabei ein Rohargonprodukt bis zu einem Sauerstoffgehalt von ca. 1 ppm oder auch weniger verwirklicht werden. Diesen bisher unbekannten Zusammenhang nutzt die Erfindung und ist damit in der Lage, gleich viel Argon abzutrennen mit einer wesentlich verkleinerten Rohargonsäule.The physical background is the surprising fact that the withdrawal of waste argon at an intermediate point of the crude argon column can allow a significantly more efficient recovery of an oxygen-poor crude argon product through an increased reflux ratio F/D in the upper part of the crude argon rectification. A crude argon product with an oxygen content of about 1 ppm or even less can be realized. The invention uses this hitherto unknown relationship and is thus able to separate the same amount of argon with a significantly smaller crude argon column.
Claims (5)
dadurch gekennzeichnet, dass
characterized in that
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69202307T2 (en) * | 1991-06-24 | 1996-01-04 | Praxair Technology Inc | Cryogenic rectification process for the production of purified argon. |
EP0841525A2 (en) * | 1996-11-11 | 1998-05-13 | The BOC Group plc | Air separation |
US5878597A (en) * | 1998-04-14 | 1999-03-09 | Praxair Technology, Inc. | Cryogenic rectification system with serial liquid air feed |
WO2016058666A1 (en) | 2014-10-16 | 2016-04-21 | Linde Aktiengesellschaft | Method and device for variably obtaining argon by means of low-temperature separation |
-
2021
- 2021-05-27 EP EP21020277.6A patent/EP3992560A1/en not_active Withdrawn
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE69202307T2 (en) * | 1991-06-24 | 1996-01-04 | Praxair Technology Inc | Cryogenic rectification process for the production of purified argon. |
EP0841525A2 (en) * | 1996-11-11 | 1998-05-13 | The BOC Group plc | Air separation |
US5878597A (en) * | 1998-04-14 | 1999-03-09 | Praxair Technology, Inc. | Cryogenic rectification system with serial liquid air feed |
WO2016058666A1 (en) | 2014-10-16 | 2016-04-21 | Linde Aktiengesellschaft | Method and device for variably obtaining argon by means of low-temperature separation |
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