DE566151C - Extraction of air components with a higher boiling point than oxygen - Google Patents

Extraction of air components with a higher boiling point than oxygen

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Publication number
DE566151C
DE566151C DEG81157D DEG0081157D DE566151C DE 566151 C DE566151 C DE 566151C DE G81157 D DEG81157 D DE G81157D DE G0081157 D DEG0081157 D DE G0081157D DE 566151 C DE566151 C DE 566151C
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DE
Germany
Prior art keywords
krypton
oxygen
column
liquid
washing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
DEG81157D
Other languages
German (de)
Inventor
Dr Paul Schuftan
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Linde GmbH
Original Assignee
Gesellschaft fuer Lindes Eismaschinen AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to NL39016D priority Critical patent/NL39016C/xx
Priority to BE403024D priority patent/BE403024A/xx
Priority to NL42092D priority patent/NL42092C/xx
Priority to BE391302D priority patent/BE391302A/xx
Priority to FR743380D priority patent/FR743380A/fr
Application filed by Gesellschaft fuer Lindes Eismaschinen AG filed Critical Gesellschaft fuer Lindes Eismaschinen AG
Priority to DEG81157D priority patent/DE566151C/en
Priority to DEG83534D priority patent/DE629297C/en
Priority to ES0127972A priority patent/ES127972A1/en
Priority to US634779A priority patent/US1963809A/en
Priority to GB26710/32A priority patent/GB390069A/en
Application granted granted Critical
Publication of DE566151C publication Critical patent/DE566151C/en
Priority to DEG85530D priority patent/DE631639C/en
Priority to GB24841/33A priority patent/GB413518A/en
Priority to FR44782D priority patent/FR44782E/en
Priority to GB13802/34A priority patent/GB438196A/en
Priority to US724821A priority patent/US2060940A/en
Priority to DEG90034D priority patent/DE641715C/en
Expired legal-status Critical Current

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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
    • F25J3/04763—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
    • F25J3/04842—Intermittent process, so-called batch process
    • 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
    • F25J3/04624—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 integrated mass and heat exchange, so-called non-adiabatic rectification, e.g. dephlegmator, reflux exchanger
    • 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
    • F25J3/04745—Krypton and/or Xenon
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/04—Processes or apparatus using separation by rectification in a dual pressure main column system
    • 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
    • F25J2200/52—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
    • 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
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/12—Particular process parameters like pressure, temperature, ratios
    • 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
    • Y10S62/925—Xenon or krypton

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Description

Gewinnung der Luftbestandteile mit höherem Siedepunkt als Sauerstoff Es ist bekannt, daß sich von den Luftbestandteilen, die einen höheren Siedepunkt als Sauerstoff besitzen, in der folgenden Beschreibung werden diese kurz mit Krypton bezeichnet, nur ein geringer Teil bei der Zerlegung der Luft durch Tiefkühlung in dem flüssigen Sauerstoff des Verdampfungsgefäßes wiederfindet. Der überwiegende Teil des Kryptons ist in dem abziehenden gasförmigen Sauerstoff enthalten, und zwar in etwa fünffacher Konzentration gegenüber der atmosphärischen Luft. Es ist bereits vorgeschlagen worden, das Krypton aus dem gasförmigen Sauerstoff durch selektive Adsorption an Kohle oder Silica Gel zu gewinnen; doch hat dieses Verfahren erhebliche Nachteile, von denen nur die Diskontinuierlichkeit desVerfahrens, die verhältnismäßig geringe Aufnahmefähigkeit der Adsorptionsmittel für Krypton bei dessen geringen Partialdruck und die schwierige Austreibung und Aufarbeitung des Adsorbates genannt seien. Es ist auch bereits vorgeschlagen worden, das Krypton aus dem flüssigen Sauerstoff zu gewinnen, der in dem Verdampfungsgefäß des L uftzerlegungsapparates anfällt; dabei läßt sich aber aus den obengenannten Gründen keine quantitative Gewinnung des Kryptons erzielen, ferner treten bei der Rektifikation der Flüssigkeit Schwierigkeiten auf durch schnelle Verlegung der Böden mit den im flüssigen Ausgangssauerstoff enthaltenen festen Verunreinigungen, wie Eis und feste Kohlensäure.Obtaining air components with a higher boiling point than oxygen It is known that air constituents have a higher boiling point as oxygen, in the following description these are briefly referred to as krypton referred to, only a small part in the breakdown of air by freezing into the liquid oxygen in the evaporation vessel. The vast majority Part of the krypton is contained in the withdrawing gaseous oxygen, namely about five times the concentration of atmospheric air. It is already It has been suggested that the krypton be selective from the gaseous oxygen To gain adsorption on charcoal or silica gel; yet this procedure has significant Disadvantages, of which only the discontinuity of the process, which is proportionate low absorption capacity of the adsorbent for krypton at its low Partial pressure and the difficult expulsion and processing of the adsorbate called be. It has also already been proposed to extract krypton from liquid oxygen to win, which is obtained in the evaporation vessel of the air separation apparatus; however, for the reasons given above, no quantitative recovery can be made of the krypton, and difficulties arise in the rectification of the liquid by quickly laying the floors with the oxygen contained in the initial liquid solid impurities such as ice and solid carbon dioxide.

Alle diese Nachteile werden durch das vorliegende Verfahren vermieden. Es wurde nämlich gefunden, daß man das Krypton in höchster Konzentration und Ausbeute gewinnen kann, wenn man es aus dem bei der Zerlegung von Luft durch Tiefkühlung entweichenden gasförmigen Sauerstoff mit kryptonfreiem flüssigem Sauerstoff im Gegenstrom auswäscht. Dieses Resultat war um so überraschender, als es von vornherein unwahrscheinlich war, einen in einem Gase in der äußerst geringen Konzentration von nur etwa 5 Teilen pro Million enthaltenen Stoff mit technischen Waschmethoden mit guter Ausbeute -zu gewinnen.All of these disadvantages are avoided by the present method. It has been found that krypton can be found in the highest concentration and yield can be gained if it is obtained from the decomposition of air by freezing escaping gaseous oxygen with krypton-free liquid oxygen in countercurrent washes out. This result was all the more surprising as it was improbable from the outset was, one in a gas in the extremely low concentration of only about 5 parts per million substance contained with technical washing methods with good yield -zu to win.

Trotzdem gelingt die Kryptonauswaschung in sehr befriedigender Weise, wenn man sie erfindungsgemäß in einer sehr gut wirkenden Rektifikationssäule durchführt. Dabei wird nach vorliegendem Verfahren ein wesentlich besseres und gleichmäßigeres Arbeiten der Waschvorrichtung dadurch erzielt, daß als Ausgangsstoff gasförmiger, durch Zerlegung von Luft mittels Tiefkühlung entweichender Sauerstoff zur Anwendung gelangt, denn dieser enthält keinerlei Verunreinigungen mehr, die sich in fester Form auf den Rektifikationsböden abscheiden können.Nevertheless, the krypton leaching succeeds in a very satisfactory way, if it is carried out according to the invention in a very effective rectification column. According to the present method, a significantly better and more uniform one is achieved Working of the washing device achieved that as a starting material gaseous, oxygen escaping through the decomposition of air by means of deep freezing is used because it no longer contains any impurities that can be solidified Can deposit form on the rectification trays.

Wesentlich für das Gelingen des Verfahrens ist die Verwendung von kryptonfreiem oder praktisch kryptonfreiem Sauerstoff als Waschflüssigkeit. Dieser wird erfindungsgemäß dadurch erzeugt, daß ein Teil des Sauerstoffes bei der Zerlegung von Luft mittels Tiefkühlung im oberen Teile der Waschvorrichtung verflüssigt wird.The use of is essential for the success of the procedure krypton-free or practically krypton-free oxygen as washing liquid. This is produced according to the invention in that some of the oxygen in the Separation of air liquefied by means of deep freezing in the upper part of the washing device will.

Die Gegenstromauswaschung des Kryptons aus dem gasförmigen Sauerstoff erfolgt am einfachsten in einem senkrecht stehenden Röhrenbündel, in das der aus dem Verdampfungsgefäß des Luftzerlegungsapparates austretende Sauerstoff unten mit etwa Siedetemperatur dampfförmig eintritt. Das Röhrenbündel wird von außen in geeigneter Weise gekühlt, zweckmäßig durch den abziehenden kalten Stickstoff, dessen Menge und Temperatur zur Bildung genügender Mengen von Waschflüssigkeit (Sauerstoff) ausreicht. Mit der gleichen Wirkung kann die Bildung der Waschflüssigkeit auch in einem Kondensator bewirkt werden, der sich am Kopfe der Waschsäule befindet und mit flüssiger Luft oder mit flüssigem Stickstoff usw. beschickt wird.The countercurrent leaching of krypton from the gaseous oxygen takes place most easily in a vertical tube bundle into which the the oxygen escaping from the evaporation vessel of the air separation apparatus at the bottom about boiling point occurs in vapor form. The tube bundle is more suitable from the outside Cooled wisely, expediently by the withdrawing cold nitrogen, its amount and temperature is sufficient to form sufficient amounts of washing liquid (oxygen). The formation of the washing liquid in a condenser can also have the same effect be effected, which is located at the head of the washing column and with liquid air or charged with liquid nitrogen, etc.

Mit besonderem Vorteil wird als Waschvorrichtung eine gut wirkende Rektifikationssäule verwendet, in die der vom Verdampfungsgefäß kommende Sauerstoffdampf von unten eintritt, während sich am Kopfe der Säule ein Kondensator befindet. In diesem Falle ist die Auswaschung durch kondensierten flüssigen Sauerstoff infolge des höheren Wirkungsgrades der Säule noch besser.A well-functioning washing device is particularly advantageous Rectification column used, in which the oxygen vapor coming from the evaporation vessel enters from below, while there is a condenser at the top of the column. In in this case the leaching is due to condensed liquid oxygen the higher efficiency of the column even better.

Die weitere Anreicherung der erhaltenen Waschflüssigkeit an Krypton kann am einfachsten in der Weise erfolgen, daß man die Waschflüssigkeit aus der Waschvorrichtung wieder in das Sauerstoffverdampfungsgefäß des Luftzerlegungsapparates zurückführt. Dabei reichert sich das Krypton mehr und mehr in dem flüssigen Sauerstoff des Verdampfungsgefäßes an, der am Ende der Betriebsperiode des Zerlegungsapparates abgezogen und auf reines Krypton verarbeitet wird.The further enrichment of the washing liquid obtained in krypton can be done most easily in such a way that the washing liquid from the Wash device back into the oxygen evaporation vessel of the air separation apparatus returns. The krypton accumulates more and more in the liquid oxygen of the evaporation vessel at the end of the operating period of the dismantling apparatus is deducted and processed on pure krypton.

Eine andere Möglichkeit der-Anreicherung' die den Vorteil hat, kontinuierlich Krypton von willkürlich einstellbarer Konzentration zu liefern, besteht darin, daß man den kryptonhaltigen flüssigen Sauerstoff nach Verlassen der `Vaschsäule auf eine zweckmäßig unter der Waschsäule befindliche Rektifikationssäule aufgibt, die unten beheizt wird. Die aus dieser Zusatzsäule entweichenden Dämpfe werden unten wieder in die Waschsäule zurückgeleitet. In diesem Falle ist zwecks quantitativer Gewinnung des Kryptons am Ende der Betriebsperiode des Zerlegungsapparates auch der flüssige Sauerstoff des Verdampfungsgefäßes in der Rektifikationssäule einzudampfen, oder man läßt dauernd eine kleine Menge von flüssigem Sauerstoff aus dem Verdampfungsgefäß mit in die Zusatzsäule eintreten, um eine Anreicherang von Krypton im Kondensator zu verhindern.Another possibility of enrichment - which has the advantage of being continuous To deliver krypton of arbitrarily adjustable concentration consists in that the krypton-containing liquid oxygen is released after leaving the `Vaschsäule a rectification column conveniently located under the washing column gives up the is heated below. The vapors escaping from this additional column are below returned to the washing column. In this case it is more quantitative Extraction of the krypton at the end of the operating period of the decomposition apparatus as well to evaporate the liquid oxygen from the evaporation vessel in the rectification column, or a small amount of liquid oxygen is continuously let out of the evaporation vessel to enter the additional column in order to increase the concentration of krypton in the condenser to prevent.

Die Ausführung des Verfahrens sei im folgenden an Hand von zwei Beispielen beschrieben, wobei zwei Spezialfälle herausgegriffen worden sind.The execution of the method is given below using two examples described, whereby two special cases have been singled out.

In Fig. i bedeutet i die Drucksäule, 2 die obere Säule und 3 das Verdampfungsgefä.ß mit Kondensator eines Luftzerlegungsapparates. Der bei q. aus dem Verdampfungsgefäß austretende gasförmige kryptonhaltige Sauerstoff wird in das senkrecht stehende Röhrenbündel 5 geleitet, dessen Mantelrohr 6 von dem erzeugten kalten gasförmigen Stickstoff durchströmt wird, der bei 8 austritt. Da der Stickstoff um 13' kälter ist als der Sauerstoff und da dessen Menge etwa das Vierfache der Sauerstoffmenge beträgt, findet im oberen Teil von 5 eine reichliche Kondensation von Sauerstoff statt. Die entgegen dem Gasstrom zurückfließende Flüssigkeit wäscht aus dem aufsteigenden gasförmigen Sauerstoff das Krypton aus und wird dabei zum größten Teil wieder verdampft und so an Krypton angereichert. Da der in den oberen Teil des Röhrenbündels gelangende gasförmige Sauerstoff durch die beschriebene Auswaschung von Krypton befreit worden war, gelingt es durch die beschriebene Anordnung also, im oberen Teil des Kondensators eine kry ptonfreie Waschflüssigkeit zu erzeugen. Die das Krypton enthaltende Waschflüssigkeit fließt durch 4. in das Verdampfungsgefäß 3 zurück; dort findet eine weitere progressive Anreicherung des Kryptons statt. Am Ende der Betriebsperiode des Zerlegungsapparates wird die praktisch das gesamte Krypton der verarbeiteten Luft enthaltende Flüssigkeit des Verdampfungsgefäßes bei 9 abgezogen und in bekannter Weise auf Reinkrypton verarbeitet.In Fig. I i denotes the pressure column, 2 the upper column and 3 the evaporation vessel with condenser of an air separation apparatus. The one at q. from the evaporation vessel exiting gaseous krypton-containing oxygen is converted into the vertical Tube bundle 5 passed, the jacket tube 6 of the generated cold gaseous Nitrogen is flowed through, which exits at 8. Because the nitrogen is 13 'colder is than oxygen and there its amount about four times the amount of oxygen , there is abundant condensation of oxygen in the upper part of 5 instead of. The liquid flowing back against the gas flow washes out of the rising one gaseous oxygen removes the krypton and is mostly evaporated again in the process and so enriched in krypton. Because the one reaching the upper part of the tube bundle gaseous oxygen has been freed from krypton by the leaching process described the arrangement described succeeds in the upper part of the capacitor to generate a crypton-free washing liquid. The washing liquid containing the krypton flows through 4. back into the evaporation vessel 3; there is another progressive Enrichment of the krypton takes place. At the end of the cutting machine's operating period becomes the liquid containing virtually all of the krypton in the air being processed of the evaporation vessel withdrawn at 9 and processed in a known manner on pure krypton.

Bei der Arbeitsweise nach Fig. 2 erfolgt die Auswaschung und Anreicherung des Kryptons in Rektifikationssäulen. Der aus dem Verdampfungsgefäß 3 des Zerlegungsapparates austretende kryptonhaltige Sauerstoff wird in die mit Rektifikationsböden ausgestattete Waschsäule 4. eingeleitet. Die Kondensation der kryptonfreien Waschflüssigkeit erfolgt hier in dem aufgesetzten Kondensator 5, der mit flüssigem Stickstoff gekühlt wird. Dieser wird durch Ventil 8 zugeführt. Die Wirkung der Säule q. entspricht im Prinzip der beschriebenen `Virkung des Rohrbündels 5 (Fig. z). Der das Krypton enthaltende, am Fuße der Säule q. ankommende flüssige Sauerstoff wird auf die unter q. befindliche Anreicherungssäule 6 aufgegeben und dort weiterkonzentriert. Die Heizung dieser Säule erfolgt mit komprimierter Luft, deren Menge durch Ventil 9 geregelt wird. Das hochkonzentrierte Krypton kann aus dem Verdampfungsgefäß 7 im gasförmigen Zustand bei io oder auch im flüssigen Zustand abgezogen «erden. Bei der zuletzt beschriebenen Arbeitsweise ist es möglich, das Krypton in kontinuierlichem Strom und in beliebig regelbarer Konzentration zu erhalten.In the procedure according to FIG. 2, the leaching and enrichment takes place of krypton in rectification columns. The one from the evaporation vessel 3 of the decomposition apparatus escaping krypton-containing oxygen is fed into the rectification trays Wash column 4th initiated. The krypton-free washing liquid is condensed here in the attached condenser 5, which is cooled with liquid nitrogen. This is fed through valve 8. The effect of the column q. corresponds in principle the described `action of the tube bundle 5 (Fig. z). The one containing the krypton, at the foot of the pillar q. incoming liquid oxygen is transferred to the under q. located Abandoned enrichment column 6 and further concentrated there. The heating of this The column uses compressed air, the amount of which is regulated by valve 9. The highly concentrated krypton can from the evaporation vessel 7 in the gaseous state subtracted when io or in the liquid state "earth. In the The last-described mode of operation makes it possible to use the krypton continuously Electricity and in any controllable concentration.

Die Wirkung der Säule 4 mit Kondensator 5 soll nun an einem Beispiel noch näher erläutert werden.The effect of column 4 with condenser 5 will now be illustrated using an example will be explained in more detail.

Es soll anenommen werden, daß in Fig. 2 aus j in die' Säule 4 ioo cbm dampfförmiger kryptonhaltiger Sauerstoff eintreten und daß mit diesem Dampf eine Flüssigkeit mit der rofachen Kryptonkonzentration im Gleichgewicht steht. Wenn die aus Säule 4 in Säule 6 leerunterlaufende Flüssigkeit alles Krypton enthalten soll, so muß deren Menge io cbm betragen, d. h. bei Annahme gleicher Verdampfungs«#ärmen von Krypton und Sauerstoff müssen in dem Kondensator 5 iö cbm Sauerstoff kondensiert werden.It should be assumed that in Fig. 2 from j in the 'column 4 ioo cbm vaporous krypton-containing oxygen enter and that with this vapor a liquid is in equilibrium with the rof the krypton concentration. if the underflowing liquid from column 4 to column 6 contain all of the krypton should, their quantity must be 10 cbm, i.e. H. if the same evaporation «# is assumed of krypton and oxygen must condense in the condenser 5 10 cbm oxygen will.

Wird die Vorrichtung in Betrieb gesetzt, so kondensiert zunächst in 5 eine kry ptonhaltige Flüssigkeit, und zwar wird der erste kondensierende Tropfen entsprechend dem Gleichgewicht die iofache Kryptonkondensation besitzen wie der Ausgangssauerstoff; im Laufe der weiteren Kondensation muß jedoch infolge der fortschreitenden Verarmung der Gasphase an Krypton ein immer kry ptonärmeres Kondensat anfallen. Im ganzen wird also gleich nach der Inbetriebsetzung die im Kondensator anfallende Flüssigkeit zwar kryptonhaltig sein, aber das Krypton in geringerer Konzentration enthalten, als dem Gleichgewicht mit dem in der Säule eintretenden kryptonhaltigen Sauerstoff entspricht. Beim Herunterrieseln durch die Säule muß sich diese Flüssigkeit mit aufsteigenden Dämpfen ins Gleichgewicht setzen, d. h. aus dem Dampf Krypton aufnehmen, während gleichzeitig die äquivalente Menge Sauerstoff verdampft wird. Die nunmehr in den Kondensator 5 gelangenden Dämpfe werden also bereits kryptonärmer sein als zuerst, infolgedessen auch das entstehende Kondensat. Die Verarmung der aufsteigenden Dämpfe an Krypton geht fortschreitend immer weiter, bis im Beharrungszustand schließlich nur noch kryptonfreier Sauerstoff in den Kondensator 5 gelangen kann, in dem io cbm kryptonfreier Sauerstoff kondensiert werden, während ioTeile Sauerstoff mit dem gesamten Krypton, das im Ausgangssauerstoff vorhanden war, die Säule unten verlassen.When the device is put into operation, it initially condenses in 5 a crypton-containing liquid, namely becomes the first condensing drop in accordance with the equilibrium, have the 10-fold krypton condensation as the Starting oxygen; in the course of further condensation, however, must be due to the progressive Depletion of krypton in the gas phase results in a condensate with less and less crypton. On the whole, the accumulating in the condenser becomes immediately after the start-up Liquid may contain krypton, but the krypton in lower concentration contained than the equilibrium with the krypton-containing entering the column Corresponds to oxygen. When trickling down through the column, this liquid must equilibrate with rising vapors, d. H. from the steam krypton while at the same time the equivalent amount of oxygen is evaporated. The vapors now entering the condenser 5 are therefore already lower in krypton be first, and consequently also the resulting condensate. The impoverishment of rising vapors of krypton continues progressively until it is at a steady state finally only krypton-free oxygen can get into the condenser 5, in which io cbm of krypton-free oxygen are condensed, while io parts of oxygen with all of the krypton present in the starting oxygen, the column below leaving.

Die Arbeitsweise nach Fig. i ist nur in baulicher Hinsicht verschieden, die Wirkung aber dieselbe.The mode of operation according to Fig. I is only different in structural terms, but the effect is the same.

Bei einem älteren Verfahren wird der kry ptonhaltige Sauerstoff in flüssiger Form oben auf eine Säule aufgegeben. Die abziehenden Dämpfe müssen mit dieser Flüssigkeit im Gleichgewicht stehen, also kryptonhaltig sein, so daß ein erheblicher Teil des Kryptons mit den Dämpfen verlorengehen muß. Demgegenüber ist es erstmalig mit dem neuen Verfahren möglich, das gesamte in der Luft enthaltene Krypton zu gewinnen.In an older method, the crypton-containing oxygen is stored in abandoned liquid form on top of a column. The evacuating vapors must be with this liquid are in equilibrium, i.e. contain krypton, so that a a significant part of the krypton must be lost with the fumes. In contrast is For the first time, the new process makes it possible to use all of the air contained in the air To win krypton.

Ein weiterer Vorteil des neuen Verfahrens besteht darin, daß bei der Benutzung gasförmigen Sauerstoffes als Ausgangsmaterial eine Verlegung der Böden durch Verunreinigung nicht erfolgen kann, weil dieser keine nachweisbaren Spuren von störenden Verunreinigungen mehr enthält.Another advantage of the new method is that in the Use of gaseous oxygen as a raw material for laying the floors due to contamination cannot occur because this has no detectable traces contains more of disturbing impurities.

Das beschriebene Verfahren gestattet eine kontinuierliche und quantitative Gewinnung des Kryptons aus der Luft in bisher unerreichter Konzentration; es kann mit den einfachsten Mitteln und ganz geringen Betriebskosten ausgeführt werden. 1lit dem Krypton zusammen werden die eingangs erwähnten Stoffe gewonnen, die einen höheren Siedepunkt als Sauerstoff besitzen, insbesondere auch das Xenon.The method described allows a continuous and quantitative Extraction of krypton from the air in unprecedented concentrations; it can can be carried out with the simplest means and very low operating costs. The substances mentioned at the beginning are obtained together with the krypton have a higher boiling point than oxygen, especially xenon.

Claims (2)

PATENTAXSPRÜCHE: i. Verfahren zur Gewinnung der Luftbestandteile mit höherem Siedepunkt als Sauerstoff bei der Luftzerlegung durch Tiefkühlung, dadurch gekennzeichnet, daß man den bei der Zerlegung von Luft mittels Tiefkühlung gewonnenen gasförmigen, z. B. Krypton und Xenon enthaltenden Sauerstoff einer Gegenstromwaschung mit praktisch kryptonfreiem flüssigem Sauerstoff unterwirft, der durch Rektifikation des Ausgangssauerstoffes unter Kondensation des kryptonhaltigen Sauerstoffs im oberen Teil der Waschvorrichtung gewonnen wird. PATENT CLAIMS: i. Process for extracting the air components with higher boiling point than oxygen in the air separation by deep freezing, thereby characterized in that one obtained in the decomposition of air by means of deep freezing gaseous, e.g. B. krypton and xenon containing oxygen countercurrent washing with practically krypton-free liquid oxygen subjected to rectification of the starting oxygen with condensation of the krypton-containing oxygen in the upper Part of the washing device is obtained. 2. Verfahren nach Anspruch i, dadurch gekennzeichnet, daß die Anreicherung der erhaltenen Waschflüssigkeit durch Rückführung dieser in das Verdampfungsgefäß des Zerlegungsapparates oder in einer besonderen Zusatzsäule erfolgt, die zweckmäßig unterhalb der Waschsäule steht und aus der die Dämpfe wieder in die Waschsäule zurückgeleitet werden.2. The method according to claim i, characterized in that that the enrichment of the washing liquid obtained by recycling this in the evaporation vessel of the decomposition apparatus or in a special additional column takes place, which is expediently below the washing column and from which the vapors again be returned to the washing column.
DEG81157D 1931-11-14 1931-11-14 Extraction of air components with a higher boiling point than oxygen Expired DE566151C (en)

Priority Applications (16)

Application Number Priority Date Filing Date Title
NL39016D NL39016C (en) 1931-11-14
BE403024D BE403024A (en) 1931-11-14
NL42092D NL42092C (en) 1931-11-14
BE391302D BE391302A (en) 1931-11-14
FR743380D FR743380A (en) 1931-11-14
DEG81157D DE566151C (en) 1931-11-14 1931-11-14 Extraction of air components with a higher boiling point than oxygen
DEG83534D DE629297C (en) 1931-11-14 1932-09-09 Process for eliminating the hydrocarbon-related difficulties in the recovery of krypton and xenon from air by rectification
ES0127972A ES127972A1 (en) 1931-11-14 1932-09-22 PROCEDURE FOR OBTAINING AIR ELEMENTS WITH A BOILING POINT HIGHER THAN OXYGEN.
US634779A US1963809A (en) 1931-11-14 1932-09-24 Process of obtaining constituents of air having a higher boiling point than oxygen
GB26710/32A GB390069A (en) 1931-11-14 1932-09-26 Method for the extraction of those constituents of air which have a higher boiling point than oxygen
DEG85530D DE631639C (en) 1931-11-14 1933-05-14 Extraction of krypton and xenon
GB24841/33A GB413518A (en) 1931-11-14 1933-09-07 Method for obtaining krypton and xenon from air
FR44782D FR44782E (en) 1931-11-14 1934-05-04 Process for obtaining constituents of air with a higher boiling point than oxygen
GB13802/34A GB438196A (en) 1931-11-14 1934-05-07 Process for obtaining krypton and xenon
US724821A US2060940A (en) 1931-11-14 1934-05-09 Process for obtaining krypton and xenon
DEG90034D DE641715C (en) 1931-11-14 1935-03-20 Extraction of krypton and xenon from air

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DEG81157D DE566151C (en) 1931-11-14 1931-11-14 Extraction of air components with a higher boiling point than oxygen
DEG83534D DE629297C (en) 1931-11-14 1932-09-09 Process for eliminating the hydrocarbon-related difficulties in the recovery of krypton and xenon from air by rectification
DE438196X 1933-05-13

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DE566151C true DE566151C (en) 1932-12-16

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DEG81157D Expired DE566151C (en) 1931-11-14 1931-11-14 Extraction of air components with a higher boiling point than oxygen
DEG83534D Expired DE629297C (en) 1931-11-14 1932-09-09 Process for eliminating the hydrocarbon-related difficulties in the recovery of krypton and xenon from air by rectification
DEG85530D Expired DE631639C (en) 1931-11-14 1933-05-14 Extraction of krypton and xenon
DEG90034D Expired DE641715C (en) 1931-11-14 1935-03-20 Extraction of krypton and xenon from air

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DEG83534D Expired DE629297C (en) 1931-11-14 1932-09-09 Process for eliminating the hydrocarbon-related difficulties in the recovery of krypton and xenon from air by rectification
DEG85530D Expired DE631639C (en) 1931-11-14 1933-05-14 Extraction of krypton and xenon
DEG90034D Expired DE641715C (en) 1931-11-14 1935-03-20 Extraction of krypton and xenon from air

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US (2) US1963809A (en)
BE (2) BE403024A (en)
DE (4) DE566151C (en)
ES (1) ES127972A1 (en)
FR (2) FR44782E (en)
GB (3) GB390069A (en)
NL (2) NL42092C (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1099564B (en) * 1959-09-09 1961-02-16 Linde S Eismaschinen Ag Zweign Process and device for the enrichment of high-boiling substances during the decomposition of gas mixtures by low-temperature rectification
DE1158534B (en) * 1961-07-05 1963-12-05 Inst Chemie Und Kaelteausruest Process for obtaining a highly concentrated krypton-xenon mixture
EP1429099A1 (en) * 2002-12-12 2004-06-16 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon

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BE487786A (en) * 1943-05-27
US2464891A (en) * 1943-08-28 1949-03-22 Linder Air Products Company Process of and apparatus for producing compressed oxygen
US2514921A (en) * 1944-11-16 1950-07-11 Linde Air Prod Co Process and apparatus for separating gas mixtures
US2423274A (en) * 1945-07-06 1947-07-01 Air Reduction Recovery of the components of air
US2497589A (en) * 1947-04-18 1950-02-14 Air Reduction Separation and recovery of the constituents of air
US2587820A (en) * 1947-05-16 1952-03-04 Independent Engineering Compan Vapor oxygen recondenser
US2509044A (en) * 1947-07-03 1950-05-23 Standard Oil Dev Co Separation of low molecular weight hydrocarbons from petroleum mixtures
US2615312A (en) * 1949-05-07 1952-10-28 Union Carbide & Carbon Corp Process and apparatus for eliminating impurities during the separation of gas mixtures
US2698523A (en) * 1950-04-28 1955-01-04 Carthage Hydrocol Inc Manufacture of krypton and xenon
US2962868A (en) * 1956-02-17 1960-12-06 Air Reduction Method of concentrating kryptonxenon
US2990690A (en) * 1958-10-27 1961-07-04 Spencer Chem Co Argon purification process
US3191393A (en) * 1959-12-30 1965-06-29 Air Reduction Krypton-xenon separation from a gas mixture
GB969799A (en) * 1962-02-27 1964-09-16 Roman Stoklosinski Improvements in the recovery of krypton and xenon from air separation plants
GB1371327A (en) * 1970-10-12 1974-10-23 British Oxygen Co Ltd Air separation
DE2055099A1 (en) * 1970-11-10 1972-05-18 Messer Griesheim Gmbh, 6000 Frankfurt Process for the enrichment of krypton and xenon in air separation plants
JPS5743186A (en) * 1980-08-29 1982-03-11 Nippon Oxygen Co Ltd Production of krypton and xenon
GB8610766D0 (en) * 1986-05-02 1986-06-11 Colley C R Yield of krypton xenon in air separation
GB2453141A (en) * 2007-09-27 2009-04-01 Hd Inspiration B V Method of forming a visor
US20160197669A1 (en) * 2014-12-11 2016-07-07 Tesla Wireless Company LLC Communication method and system that uses low latency/low data bandwidth and high latency/high data bandwidth pathways

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1099564B (en) * 1959-09-09 1961-02-16 Linde S Eismaschinen Ag Zweign Process and device for the enrichment of high-boiling substances during the decomposition of gas mixtures by low-temperature rectification
DE1158534B (en) * 1961-07-05 1963-12-05 Inst Chemie Und Kaelteausruest Process for obtaining a highly concentrated krypton-xenon mixture
EP1429099A1 (en) * 2002-12-12 2004-06-16 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon
US6829907B2 (en) 2002-12-12 2004-12-14 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon
US6848269B2 (en) 2002-12-12 2005-02-01 Air Products And Chemicals, Inc. Process and apparatus for the recovery of krypton and/or xenon

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DE629297C (en) 1936-04-27
GB413518A (en) 1934-07-19
US1963809A (en) 1934-06-19
US2060940A (en) 1936-11-17
NL39016C (en)
GB390069A (en) 1933-03-30
DE641715C (en) 1937-02-11
FR743380A (en) 1933-03-29
ES127972A1 (en) 1932-11-01
FR44782E (en) 1935-04-06
NL42092C (en)
BE403024A (en)
DE631639C (en) 1936-06-24
BE391302A (en)
GB438196A (en) 1935-11-07

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