DE1922956B1 - Process for the production of argon-free oxygen by the rectification of air - Google Patents

Process for the production of argon-free oxygen by the rectification of air

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Publication number
DE1922956B1
DE1922956B1 DE19691922956D DE1922956DA DE1922956B1 DE 1922956 B1 DE1922956 B1 DE 1922956B1 DE 19691922956 D DE19691922956 D DE 19691922956D DE 1922956D A DE1922956D A DE 1922956DA DE 1922956 B1 DE1922956 B1 DE 1922956B1
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Prior art keywords
stage
rectification
argon
column
product
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DE19691922956D
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German (de)
Inventor
Voigt Dipl-Ing Hartmut
Streich Dipl-Phys Martin
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Hoechst AG
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Hoechst AG
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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
    • F25J3/02—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
    • F25J3/04436—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 at least a triple pressure main column system
    • F25J3/04454—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 at least a triple pressure main column system a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
    • 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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F25J3/04303—Lachmann expansion, i.e. expanded into oxygen producing or low 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/34—Processes or apparatus using separation by rectification using a side column fed by a stream from the low 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • 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
    • 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
    • F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
    • F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
    • 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
    • F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
    • 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
    • F25J2235/42—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream 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
    • 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
    • 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
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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

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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)

Description

Gegenstand der Erfindung ist ein Verfahren zur Mitteldruckstufe und in der Niederdruckstufe Drücke Erzeugung von argonfreiem Sauerstoff durch mehr- wie beim klassischen Verfahren aufrechterhalten. Die stufige Tieftemperatur-Rektifikation, bei dem in einer Drücke in der Argonrektifikationsstufe entsprechen ersten Rektifikationsstufe verdichtete, bis etwa zum etwa den Drücken in der Niederdruckstufe. Die Taupunkt gekühlte Luft in Stickstoff und ein mit 5 Argonausbeute beträgt etwa 30 bis 60%. Über den Sauerstoff angereichertes Gemisch vorzerlegt wird, in Kopf der Argonsäule geht ein Gemisch aus etwa 45 °/0 einer zweiten Stufe ein praktisch argon- und stickstoff- Argon, 50 % Sauerstoff und 5 % Stickstoff ab. Als freies Sauerstoffprodukt anfällt und in einer dritten besonderer Vorteil des Verfahrens wird angegeben, daß Stufe ein argonhaltiges Seitenprodukt der zweiten es etwa den gleichen Energieaufwand erfordert wie das Rektifikationsstufe in ein argonfreies Sauerstoffprodukt ίο klassische Verfahren.The invention relates to a process for the medium-pressure stage and, in the low-pressure stage, pressures to generate argon-free oxygen by maintaining more than that in the conventional process. The stage low-temperature rectification, in which the first rectification stage is compressed in one of the pressures in the argon rectification stage, up to approximately the pressures in the low-pressure stage. The dew point cooled air in nitrogen and one with 5 argon yield is about 30 to 60%. Vorzerlegt is via the oxygen enriched mixture, in the top of the argon column is a mixture of about 45 ° / 0 of a second stage a substantially argon and nitrogen, argon, 50% oxygen and 5% nitrogen from. The free oxygen product is obtained and in a third special advantage of the process it is stated that an argon-containing side product of the second stage requires about the same energy expenditure as the rectification stage in an argon-free oxygen product ίο classical processes.

und in ein argonangereichertes Kopfprodukt getrennt Es wurde nun gefunden, daß der Energieaufwandand separated into an argon-enriched top product. It has now been found that the energy expenditure

wird, und bei dem die beiden Sauerstoffprodukte aus zur Luftzerlegung erheblich gesenkt wird, wenn den Sümpfen der zweiten und der dritten Rektifika- erfindungsgemäß der Druck in der dritten Rektifitionsstufe entnommen werden. kationsstufe um 0,3 bis 0,5 at kleiner ist als der Druckis, and in which the two oxygen products from air separation is considerably reduced, if the sumps of the second and third rectifiers - according to the invention, the pressure in the third rectification stage can be removed. cation level is 0.3 to 0.5 at less than the pressure

Es ist bekannt, bei diesen und anderen Rektifika- 15 in der zweiten Stufe, und wenn das der dritten Rektifitionsverfahren das Prinzip der Wärmepumpe anzu- kationsstufe entnommene Kopfprodukt dem Verstärwenden und dabei die zu zerlegende Luft als Arbeits- kerteil der zweiten Rektifikationsstufe an einer bereits mittel zu verwenden. Zur Erzeugung von Sauerstoff sauerstoffarmen Stelle zugeführt wird,
und Stickstoff in für technische Verwendung aus- Dadurch wird gegenüber dem klassischen zweireichender Reinheit werden in modernen Produktions- 20 stufigen Verfahren und gegenüber dem konventionellen anlagen zweistufige Rektifikationsverfahren angewandt. dreistufigen Verfahren erreicht, daß auch die erste Mehr als zwei Stufen werden in der Regel angeordnet, Rektifikationsstufe bei niedrigeren Drücken arbeiten wenn eine Komponente der Luft besonders rein ge- kann. Der Verdichtungsdruck der eingehenden Luft wonnen werden muß, oder wenn eine Edelgaskompo- kann 1,5 at niedriger sein. Die Energieersparnis beträgt, nente als weiteres Erzeugnis abgetrennt werden soll. 25 bezogen auf das gasförmige Produkt, rund 10 %, undIt is known that with these and other rectifications in the second stage and when the top product, which is taken from the third rectification process using the principle of the heat pump ancation stage, is used to amplify the air to be broken down as the working part of the second rectification stage at an already medium level to use. Oxygen-poor point is supplied to generate oxygen,
and nitrogen in for technical use. This means that compared to the classic two-rich purity, 20-stage processes are used in modern production and two-stage rectification processes are used compared to the conventional systems. three-stage process ensures that the first More than two stages are usually arranged, rectification stage work at lower pressures if one component of the air can become particularly pure. The compression pressure of the incoming air must be recovered, or if a noble gas compo- can be 1.5 at lower. The energy saving amounts to nent to be separated as a further product. 25 based on the gaseous product, around 10%, and

Der Arbeitsaufwand zur Luftzerlegung in Sauerstoff bleibt auch nach Rückrechnung auf den Produkt- und Stickstoff ist fünf- bis zehnmal größer als er sich zustand des klassischen Verfahrens noch beträchtlich, theoretisch mit einem umkehrbaren Zerlegungsprozeß Die Sauerstoffverluste sind gegenüber dem konvenerrechnet. Der Mehraufwand ist durch Verluste bei der tionellen dreistufigen Verfahren erheblich reduziert. Kompression, durch Wärmeeinströmung aus der 3° Besonders überraschend ist, daß trotz des erniedrigten Umgebung, durch unvollkommenen Wärmeaustausch, Rektifikationsdruckes ein argonfreies Produkt mit durch Druckverluste in Rohren und Ventilen sowie 99,5 °/0 Sauerstoff erzielt wird,
durch Verluste in den Rektifikationssäulen bedingt. In der dritten Rektifikationsstufe wird zwar, wie anThe amount of work involved in breaking up air into oxygen remains, even after calculating back to the product and nitrogen, five to ten times greater than it would be with the classical method, theoretically with a reversible decomposition process. The additional effort is considerably reduced due to losses in the conventional three-stage process. Compression, due to the inflow of heat from the 3 ° It is particularly surprising that despite the reduced environment, an argon-free product is achieved through pressure losses in pipes and valves as well as 99.5 ° / 0 oxygen due to imperfect heat exchange and rectification pressure.
caused by losses in the rectification columns. In the third rectification stage, how on

Entropiebetrachtungen führten in den letzten Jahr- sich bekannt ist, ein argonhaltiges Gemisch in eine zehnten zu zahlreichen konstruktiven Verbesserungen 35 argonfreie und in eine argonreiche Sauerstoff-Fraktion an Kompressoren, Turbinen, Wärmeaustauschern und zerlegt, doch dient diese Maßnahme nicht zur Argon-Rektifikationssäulen sowie zu verbesserten Verfahrens- gewinnung, sondern zur Erleichterung des Argontechnischen Maßnahmen; so hat Lachmann vorge- austrittes aus der zweiten Rektifikationsstufe und ist schlagen, emen Teil der zu zerlegenden Luft mit nur ein Mittel zur Absenkung des Druckniveaus,
geringem Überdruck in die Säule der zweiten Rektifi- 40 In der Zeichnung ist das Verfahren gemäß der kationsstufe einzublasen und damit den Arbeitsauf- Erfindung in einem Fließbild wiedergegeben,
wand zu verringern. Von Lachmann stammt auch die Die erste Rektifikationsstufe ist durch die Säule 1,Entropy considerations in the last few years - it is known that an argon-containing mixture is broken down into a tenth to numerous structural improvements 35 argon-free and an argon-rich oxygen fraction at compressors, turbines, heat exchangers and decomposed, but this measure is not used for argon rectification columns as well improved process acquisition, but to facilitate argon technical measures; Lachmann has come out of the second rectification stage and is able to beat a part of the air to be broken down with only one means of lowering the pressure level,
a slight overpressure in the column of the second rectification 40 In the drawing, the process is to be blown in according to the cation stage and thus the work is shown in a flow diagram,
wall decrease. Lachmann also produced the The first rectification stage is through column 1,

Idee, aus der Säule der zweiten Rektifikationsstufe eine die zweite durch die Säule 2 und die dritte Rektifi-10 bis 15 °/„ der Luftmenge entsprechende Dampfmenge kationsstufe durch die Säule 3 dargestellt. Die verabzublasen; die Maßnahme dient nicht der Arbeits- 45 dichtete, vorgekühlte Luft tritt über Leitung 6 in die ersparnis, sondern vielmehr der Produktreinheit, weil Rektifikationssäule 1 und wird dort in Stickstoff und beim Abblasen ein erheblicher Anteil des störenden ein mit Sauerstoff angereichertes Gemisch vorzerlegt. Argons — allerdings unter Produktverlusten ·— aus Im Sumpf der zweiten Rektifikationssäule 2 fällt ein der Säule entfernt wird.. praktisch argon- und stickstofffreies Produkt an.Idea, from the column of the second rectification stage one the second through the column 2 and the third rectification 10 Up to 15 ° / "of the amount of steam corresponding to the amount of air, represented by the column 3 in the cation stage. The blown off; The measure does not serve the work- 45 Dense, pre-cooled air enters via line 6 into the savings, but rather the product purity, because rectification column 1 and is there in nitrogen and When blowing off, a significant proportion of the disruptive oxygen-enriched mixture is pre-decomposed. Argon - albeit with product losses - from the bottom of the second rectification column 2 falls the column is removed .. practically argon- and nitrogen-free product.

Die Entwicklung der Luftzerlegung zur Erzeugung 5° Tn der Rektifikationssäule 3 wird ein argonhaltiger von Stickstoff und Sauerstoff hat nach Beschränkung Seitenabzug 9 der Rektifikationssäule 2 in ein argoneines Teiles der Nichtumkehrbarkeiten bereits vor freies Sumpfprodukt und in ein argonreiches Kopf-Jahrzehnten zum sogenannten Mitteldruckverfahren produkt getrennt. Das Produkt wird zu einem Teil geführt, das mit zwei Rektifikationsstufen — einer über Leitung 10 aus dem Sumpf der Säule 2 und zum Mitteldruckstufe und einer Niederdruckstufe — arbei- 55 anderen Teil über Leitung 11 aus dem Sumpf der tet. Dieses Verfahren wird häufig angewendet, und die Säule 3 entnommen.The development of air separation to produce 5 ° Tn of the rectification column 3 becomes an argon-containing one of nitrogen and oxygen has, according to restriction, side draw 9 of rectification column 2 into an argon one Part of the irreversibility already before free sump product and in an argon-rich head decades separated from the so-called medium pressure process. The product becomes a part out, with two rectification stages - one via line 10 from the bottom of column 2 and to Medium-pressure stage and a low-pressure stage - working 55 other part via line 11 from the sump of the tet. This procedure is often used and column 3 is removed.

dazu erforderlichen Anlagen werden praktisch unver- In der Säule 3 werden Rektifizierdrücke angewandt,The systems required for this are practically un- In column 3, rectifying pressures are used,

ändert immer wieder neu gebaut, so daß sie in Fach- die um 0,3 bis 0,5 at kleiner sind als der Druck in der kreisen als »klassisch« bezeichnet werden. Durch den Säule 2. Das Kopfprodukt der Säule 3 wird über Nachbau kommt aber auch zum Ausdruck, daß man 60 Leitung 4 entnommen und dem Verstärkerteil der sich mit dem zur Durchführung des Verfahrens Säule 2 an einer oberen, bereits sauerstoffarmen Stelle erforderlichen Energieaufwand abgefunden hat. mittels einer Fördereinrichtung 12 zugeführt.changes over and over again, so that they are 0.3 to 0.5 at less than the pressure in the circles are called "classic". Through column 2. The top product of column 3 is over But replica is also expressed that you removed 60 line 4 and the amplifier part of the with the column 2 to carry out the process at an upper, already oxygen-poor point has accepted the required energy expenditure. supplied by means of a conveyor 12.

Zur Gewinnung eines Teiles des in der Luft Ursprung- Aus der Zeichnung ist weiter erkennbar, wie dieTo obtain a part of the origin in the air. From the drawing it can also be seen how

lieh enthaltenen Argons wurde dieses klassische Wärmezufuhr und die Wärmeabfuhr an der Säule 3 Verfahren bekanntlich durch Anordnung einer Argon- 65 sowie die Wärmezufuhr und die Wärmeabfuhr an der rektifikationsstufe zu dem dreistufigen Rektifikations- Säule 3 sowie die Wärmezufuhr zur Säule 2 auf vorteilverfahren abgewandelt, das eingangs beschrieben ist. hafte Weise vorgenommen werden können. Der Sumpf Zur Durchführung dieses Verfahrens werden in der der Säule 3 steht mit dem Kopfprodukt der Säule 1Borrowed argon, this classic heat supply and heat dissipation at the column 3 Process known by the arrangement of an argon 65 as well as the heat supply and the heat dissipation at the rectification stage to the three-stage rectification column 3 and the supply of heat to column 2 on advantageous processes modified, which is described at the beginning. liable way can be made. The swamp To carry out this process, the top product of column 1 is in the column 3

und das Kopfprodukt der Säule 3 mit dem Sumpfprodukt der Säule 1 in indirektem Wärmeaustausch; der Sumpf der Säule 2 steht in indirektem Wärmeaustausch mit der zu zerlegenden Luft. Der Wärmeaustausch erfolgt über die Wärmeübertrager 5. Der Wärmeübertrager am Sumpf der Säule 2 wird mittels einer Regeleinrichtung so gefahren, daß der Sumpf gerade stickstofffrei bleibt. Dadurch wird ein argonreicherer Seitenabzug 9 erzielt.and the top product of column 3 with the bottom product of column 1 in indirect heat exchange; the bottom of column 2 is in indirect heat exchange with the air to be broken down. The heat exchange takes place via the heat exchanger 5. The heat exchanger at the bottom of column 2 is by means of a control device driven so that the sump just remains nitrogen-free. This makes it richer in argon Side trigger 9 achieved.

Es ist weiter vorteilhaft, die Säule 3 mit Drücken zwischen 0,8 und 1,1 ata zu betreiben. Für einen Betriebsdruck der Säule 3 von 1 ata kommt dann nach einem im folgenden näher ausgeführten Beispiel für die Säule 2 ein Betriebsdruck von 1,5 ata und für die Säule 1 ein Betriebsdruck von 4,2 ata zustande. Die Drücke sind unmittelbar über den Sümpfen gemessen.It is also advantageous to operate the column 3 with pressures between 0.8 and 1.1 ata. For one Operating pressure of column 3 of 1 ata then comes after an example for the column 2 has an operating pressure of 1.5 ata and for the column 1 an operating pressure of 4.2 ata. the Pressures are measured just above the swamps.

Beispiel auf Basis 100 Nm3/h LufteintrittExample based on 100 Nm 3 / h air inlet

Die zu zerlegende Luft tritt, abgekühlt auf —176° C, mit einem Druck von 4,24 ata über Leitung 6 ein. Ein Teilstrom von 13 Nm3/h wird über Leitung 7 zur Expansionsmaschine 8 und mit einer Temperatur von —168° C zur Säule 2 geführt. Der Hauptstrom tritt nach Passieren des Wärmeübertragers 5 am Sumpf der Säule 2 mit —178° C in die Säule 1.The air to be separated enters, cooled to −176 ° C., at a pressure of 4.24 ata via line 6. A substream of 13 Nm 3 / h is fed via line 7 to expansion machine 8 and to column 2 at a temperature of -168 ° C. After passing through heat exchanger 5, the main stream enters column 1 at the bottom of column 2 at -178 ° C.

Vom Kopf der Säule 1 strömen 32,8 Nm3/h nach Wärmeaustausch mit dem Kopfprodukt der Säule 2 im Wärmeübertrager 5 in den oberen Teil der Säule 2. Die Eintrittstemperatur beträgt —189°C. Vom Sumpfprodukt der Säule 1 strömen 54,2 Nm3/h nach Wärmeaustausch mit dem Kopfprodukt der Säule 2 im Wärmeübertrager 5 zur Säule 2; ein Teilstrom von 32 Nm3/h geht über den Wärmeübertrager 5 der Säule 3 und tritt etwa in der Mitte der Säule 2 ein, der Rest von 22,2 Nm3/h tritt weiter oberhalb in die Säule 2 ein. Am Kopf der Säule 1 wird eine Temperatur von —181° C aufrechterhalten. Dies geschieht durch Wärmeaustausch mit dem Sumpf der Säule 3 und Zwischenheizung eines rücklaufenden Kopfproduktzweiges von 4,8 Nm3/h im Wärmeübertrager 5 an der Säule 2.From the top of column 1, after heat exchange with the top product of column 2 in heat exchanger 5 , 32.8 Nm 3 / h flow into the upper part of column 2. The inlet temperature is -189 ° C. From the bottom product of column 1, 54.2 Nm 3 / h flow after heat exchange with the top product of column 2 in heat exchanger 5 to column 2; a partial flow of 32 Nm 3 / h goes through the heat exchanger 5 of column 3 and enters approximately in the middle of column 2, the remainder of 22.2 Nm 3 / h enters column 2 further above. A temperature of -181 ° C. is maintained at the top of column 1. This is done by heat exchange with the bottom of column 3 and intermediate heating of a returning top product branch of 4.8 Nm 3 / h in heat exchanger 5 on column 2.

Von der Säule 2 wird ein argonhaltiger Seitenstrom von 14,2 Nm3/h über den Seitenabzug 9 zur Säule 3 geführt. In der Säule 3 wird eine Kopftemperatur von —185,5°C und eine Sumpf temperatur von —183°C aufrechterhalten. 2 Nm3/h Kopfprodukt der Säule 3 werden in den oberen Teil der Säule 2 gefördert. Das Produkt wird zu 7,8 Nm3/h aus dem Sumpf der Säule 2 und zu 12,2 Nm3/h als 99,5%iger Sauerstoff aus der Säule 3 entnommen. Die über den Kopf der Säule 2 abgehende argonverunreinigte Stickstoffmenge beträgt 80 Nm3/h. Das Sauerstoffprodukt fällt mit — 183°C unter atmosphärischem Druck an, der Stickstoff mit —178°C unter 1,2 ata.An argon-containing side stream of 14.2 Nm 3 / h is passed from column 2 via side take-off 9 to column 3. In column 3, a top temperature of -185.5 ° C and a bottom temperature of -183 ° C is maintained. 2 Nm 3 / h top product from column 3 are conveyed into the upper part of column 2. The product is withdrawn from the bottom of column 2 at 7.8 Nm 3 / h and as 99.5% oxygen from column 3 at 12.2 Nm 3 / h. The amount of argon-contaminated nitrogen leaving the top of column 2 is 80 Nm 3 / h. The oxygen product is obtained at -183 ° C under atmospheric pressure, the nitrogen at -178 ° C under 1.2 ata.

Das Verfahren kann hinsichtlich der Drücke in dem gegebenen Rahmen abgewandelt werden, dementsprechend verändern sich die Mengenströme zwischen Ein- und Ausgang. Es eignet sich aber auch für die Anwendung der üblichen, bei dem klassischen Verfahren angewandten Methoden des AusgleichesThe method can be modified accordingly with regard to the pressures within the given framework the volume flows between input and output change. But it is also suitable for the use of the usual methods of balancing used in the classical procedure

.0 der Kälteverlust durch arbeitsleistende Stickstoff-Entspannung. Die Erzeugung von Reinstickstoff ist im Fließschema und im Verfahrensbeispiel nicht beschrieben, sie könnte in üblicher Weise geschehen, ohne daß die Druckverhältnisse dadurch wesentlich geändert würden..0 the loss of cold through work-performing nitrogen expansion. The production of pure nitrogen is not described in the flow diagram or in the process example, it could be done in the usual way without significantly changing the pressure conditions would.

Claims (3)

Patentansprüche:Patent claims: 1. Verfahren zur Erzeugung von argonfreiem Sauerstoff durch mehrstufige Tieftemperatur-Rektifikation, bei dem in einer ersten Rektifikationsstufe verdichtete, bis etwa zum Taupunkt gekühlte Luft in Stickstoff und ein mit Sauerstoff angereichertes Gemisch vorzerlegt wird, in einer zweiten Stufe ein praktisch argon- und stickstofffreies Sauerstoffprodukt anfällt und in einer dritten Stufe ein argonhaltiges Seitenprodukt der zweiten Rektifikationsstufe in ein argonfreies Sauerstoffprodukt und in ein argonreiches Kopfprodukt getrennt wird, und bei dem die beiden Sauerstoffprodukte aus den Sümpfen der zweiten und der dritten Rektifikationsstufe entnommen werden, dadurch gekennzeichnet, daß der Druck in der dritten Rektifikationsstufe um 0,3 bis 0,5 at kleiner ist als der Druck in der zweiten Stufe, und daß das der dritten Rektifikationsstufe entnommene Kopfprodukt dem Verstärkerteil der zweiten Rektifikationsstufe an einer bereits sauerstoffarmen Stelle zugeführt wird.1. Process for the production of argon-free oxygen through multi-stage low-temperature rectification, in the air that is compressed in a first rectification stage and cooled to approximately the dew point is pre-decomposed into nitrogen and an oxygen-enriched mixture, in a second stage a practically argon and nitrogen free oxygen product and in a third stage an argon-containing Side product of the second rectification stage into an argon-free oxygen product and into an argon-rich head product is separated, and in which the two oxygen products from taken from the sumps of the second and third rectification stages, thereby characterized in that the pressure in the third rectification stage is 0.3 to 0.5 at is less than the pressure in the second stage, and that that removed from the third rectification stage Head product to the amplifier part of the second rectification stage at an already low-oxygen one Body is fed. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Sumpf der dritten Rektifikationsstufe mit dem Kopfprodukt der ersten Rektifikationsstufe und der Sumpf der ersten Rektifikationsstufe mit dem Kopfprodukt der dritten Rektifikationsstufe sowie der Sumpf der zweiten Rektifikationsstufe mit der einströmenden Luft in indirektem Wärmeaustausch stehen.2. The method according to claim 1, characterized in that the bottom of the third rectification stage with the top product of the first rectification stage and the bottom of the first rectification stage with the top product of the third rectification stage and the bottom of the second Rectification stage are in indirect heat exchange with the incoming air. 3. Verfahren nach Anspruch 1 und 2, dadurch gekennzeichnet, daß die dritte Rektifikationsstufe bei Drücken zwischen 1,1 und 0.8 ata betrieben wird.3. The method according to claim 1 and 2, characterized in that the third rectification stage operated at pressures between 1.1 and 0.8 ata. Hierzu 1 Blatt Zeichnungen1 sheet of drawings COPYCOPY
DE19691922956D 1969-05-06 1969-05-06 Process for the production of argon-free oxygen by the rectification of air Pending DE1922956B1 (en)

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FR2042419A1 (en) 1971-02-12

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