DE764953C - Process for separating mixture components - Google Patents

Process for separating mixture components

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Publication number
DE764953C
DE764953C DEG107972D DEG0107972D DE764953C DE 764953 C DE764953 C DE 764953C DE G107972 D DEG107972 D DE G107972D DE G0107972 D DEG0107972 D DE G0107972D DE 764953 C DE764953 C DE 764953C
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Germany
Prior art keywords
cold
gas
countercurrent
warm
heated
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DEG107972D
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German (de)
Inventor
Walther Dipl-Ing Ruckdeschel
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Linde GmbH
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Gesellschaft fuer Lindes Eismaschinen AG
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Priority to DEG107972D priority Critical patent/DE764953C/en
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Publication of DE764953C publication Critical patent/DE764953C/en
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0276—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 characterised by the separated product stream separation of H2/N2 mixtures, i.e. of ammonia synthesis gas
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/09—Purification; Separation; Use of additives by fractional condensation
    • 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
    • F25J3/0204—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 characterised by the feed stream
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0233—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 characterised by the separated product stream separation of CnHm with 1 carbon atom or more
    • 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
    • F25J3/0228—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 characterised by the separated product stream
    • F25J3/0238—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 characterised by the separated product stream separation of CnHm with 2 carbon atoms or more
    • 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
    • F25J2200/80—Processes or apparatus using separation by rectification using integrated mass and heat exchange, i.e. non-adiabatic rectification in a reflux exchanger or dephlegmator
    • 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
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • 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
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/14—Coke-ovens gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/62—Ethane or ethylene
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-hydrocarbons

Description

Verfahren zum Abscheiden von Gemischbestandteilen Es ist bekannt, daß sich bei der Tiefkühlung von Gasgemischen in Wärmeaustaus,ch!ern, infolge Teilkondensation Gemischbestandteile ausscheiden. So wird z. B. bei der Tiefkühlung von Koksofengas in den Gegenströmern eine Methan-hal;tige Äthylenfraktion ausgeschieden. Die Gewinnung einer hochprozentigen Fraktion, in der z. B. praktisch. das gesamte Äthylen des Ausgangsgemisches enthalten ist, ist bei dem bekannten Tiefkühlverfahren nicht möglich.Process for separating mixture components It is known that in the deep freezing of gas mixtures in heat exchange, ch! ern, as a result of partial condensation Eliminate mixture components. So z. B. in the freezing of coke oven gas a methane-containing ethylene fraction was deposited in the countercurrents. The extraction a high percentage fraction in which z. B. practical. all of the ethylene des Starting mixture is contained, is not possible with the known deep-freezing process.

Die Erfindung ermöglicht es, eine hochprozentige Fraktion bei praktisch vollständiger Ausbeute des ausscheidenden Stoffes im Verlaufe der Tiefkühlung von Gasgemischen zu erzielen und besteht in dem Verfahren, während des Wärmeaustausches in einem Gegenströmer diesen zusätzlich am warmen, unteren Ende zu erwärmen und am kalten, oberen Ende- zu kühlen. Hierdurch wird einerseits vom kalten Ende zum warmen Ende des Gegenströmers ein so starker Kondensatrücklauf mit rektifizierender Wirkung erzielt, daß das Durchbrechen des auszuscheidenden Stoffes am kalten Ende des Gegenströmers verhindert wird, und anderer- seits :ine hohe Eindanipfung der Fraktion am warin:ti Ende -bewirkt. wo die Fraktion dann flüssig abgezogen werden kann. Eine Ausführungsform des Verfahrens nach der Erfindung bestellt z. B. darin. dali mittels eines an sieh lielcaiiiit@°n Kältelkreis- ]aufs eitle: Hilfsstoffe:. z. D. Stickstoff oder Methan. das untere. «-arme Ende des Gegen- strömers vor der Entspannung des Hilfs- stoffes beheizt und (las obere, kalte Ende nach der Entspannung des Hilfsstoffes ge- kühlt wird. Das Verfahren nach der Erfindung kann auch ohne Zuhilfenahme eines zusätzlichen Kältekreislaufs z. B. in der \\'eise durch- geführt «-erden, (Iala den dem Rollgas ent- gegenströmenden Zerlegungsprodukten am kalten Ende des Gegenströmers ein kaltes Gas zwecks Herabsetzung der Temperatur zugesetzt und das warme Ende des Gegen- strömers durch Zwischenentnahme eines Teil der kalun Zerlegtuigsprodulcte erwärmt wird, sofern davon abgesehen wird. etwa ein wärmeres Gas zuzusetzen. Bei beiden Ausführungsfällen wir<] die Kondensation am kalten Ende und die Ein- dampfung ain warmen Ende innerliall) der ans d:ni Rollgas anfallenden Fraktion ver- stärkt und die erfindungsgemäße rektifi- zierende Wirkung erreicht. Zwecks weiterer Verstärkung der rektifizierenden Wirkung kann der Gegenströmer auf der Roligasseite auch mit Zwischenlxiden (Rektiflzierliiden) od. dgl. versehen tverden. Bei der Gewinnung voti Ätlivlen aus Koks- ofengas mittels des Verfahrens nach der Er- findung wird z. B. durch den Rücklauf fliissigen Methans praktisch das gesamte :\thvIen einschließlich der sonstigen KcAilen- wasserstoffe mit zu-ei oder mehr C Atomen ausgewaschen, wodurch gleichzeitig die Ge- winnung von Methan und Wasserstoff hoher Reinheit vorbereitet wird. Durch die Er- wärmung des unteren Endes wird eine stärkere Eindampfung der Äthvlenfraktion in -an sich bekannter Weise erreicht. Inner- halb des Gegenströmers Besteht dabei ein rektifizierender Stoffaustausch zwischen der Rücldatifflüssigt;cit finit den aufsteigenden Dämpfen, der es ermöglicht, am unteren, warmen Ende des Gegenströniers eine Äthylenfraktion hofier Anreicherung (bis über 65070 C#-lH4. ) bei höchster Ausbeute zu entnehmen. Zwei Ausführungsbeispiele des Verfahrens nach der Erfindung werden nachstehend an Hand der Abbildungen, die eine Koksgas- zerle`'ungsanlage in stark vereinfachtem Schema darstellen. beschrieben: Das Koksgas tritt durch L eitung i (Abl).i j in die Gegenstriinier _-1, D. C ein. die e: der Reihe nach (lurclistr;itnt, 111111 wird hierbei im \\'ä rmeaustausch finit den Zerlegungspro- <lukteii abgekühlt. Aus dein h,-iksgas wird in dein Kondensator d. Methan al)geschieden. das die Anlage über Leitung 3 durch die Gegenströmer _-i, B. C verläßt. Aus dein am Iwopf der Säule d. abziehenden Gasgemisch wird in der Sätile; unter Zugabe von kaltem. entspanntem Stickstoff ein Synthesegas (1-I, -?- \.,) ge«-onnen. das über die Lei- tungell t;, a und i= entnommen wird. Das Restgas, in der Hauptsache Kolilenosvd und Stickstoff. wird am Boden der Säule fliissig entnommen, über Leittl"g ; zunächst dein Gegenstrriiner C ztlgefiilirt. wo es ver- dampft wird. und darauf über die Gegen- strönier D und P geleitet. Der als Kälte- träger dienende Stickstoff wird über Lei- tung 8, Gegenströrner D und F_ nach Vorent- spannung dein Kondensator .l zugeführt. iv,i dieVerfliissigung der -\letlianfraktion erfolgt. \zicli weiterer 1;tit#pannutig wird der flüssig anfallende Stickstoa zur Berieselung der Säule ; verwendet: der ent#pannte gas- förinige Stickstoff wird über Leitung (Gegetiströnier P» der erneuten Verdichtung zugeführt. Die Anwendung des Verfahrens nach der Erfindung wird gelcennzeiclinet durch die Anordnung der Leitung io mit Ventil i i und der Leitung 12 finit \-entil 13- Die Leitung 1o ermöglicht eine Umgehung des Gegen- ströniers C durch einen Teil des Sviltliese- gases (IH.., -(- Na). Je mehr Gas iil)er die LeituiMg io aligezwe@igt wird. inn so kälter wird das obere Ende des Gegenströmers D. Infolgedessen stellt sich im Koksgas chic verhältnismäl.ig starke Kondensation von Uetlian ein, das als Rücklaufflüssigkeit das Äthylen aus (]ein Gas auswäscht. -Mit Hilfe (I-> Äthylen i i läßt sich die günstigste Tein- peratur am kalten Ende des Gegenströniers l; einstellen. Andererseits wird am Punkt 14 aus I_eitllllg 2 ein Teil des in Säule 3 ge- @v,iinienen Svntlie:egases über Leitung 12 ab- reguliert und dein Gegenströnier P ztigefülirt, w ähi # -end e# normalerweise die Anlage iil>tr Gegetiströnier A verlassen wurde. Je mehr v@@u diesem Gas finit Hilfe des Ventils 13 ab- reguliert wird, umso tv@irmer wird der Gegen- strömer A am unteren Ende und um so wiiriner tritt also das Rollgas auch unten in den Gegenströmer D ein, so daß eine starke Verdampfung des als Waschflüssigkeit dienenden --\letlians eintritt. Auf diese Weise werden die günstigsten Temperaturverhä It- nisse im Gegenströnier D nach der Erfindung geschaffen, um eine hocliwertihe :lthv@en- fraktion zti erhalten. Das zum Teil Bereits im Gegenstr;>tner .-1. ini übrigen im (;egetistr@nier D attifallen(le Äthylen wird dem Abscheider 15 zugeführt: die gewonnene flüssige Äthylenfräktion wird über Leitung 16 und Gegenströmer E und D herausgeführt.The invention makes it possible to achieve a high percentage fraction with a practically complete yield of the precipitating substance in the course of the freezing of gas mixtures and consists in the process of additionally heating the warm, lower end and the cold, upper end during the heat exchange in a countercurrent - to cool. As a result, on the one hand, a condensate return flow with a rectifying effect from the cold end to the warm end of the countercurrent is so strong that the material to be separated out is prevented from breaking through at the cold end of the countercurrent, and on the other hand - on the other hand: a high level of pressure on the parliamentary group at warin: ti end - effected. where the faction can then be withdrawn in liquid form. One embodiment of the method according to the invention ordered z. B. in it. dali by means of a see lielcaiiiit @ ° n refrigeration cycle ] on vain: auxiliary materials :. z. D. nitrogen or Methane. the lower. «-Arm end of the opposite- strömers before the relief of the auxiliary heated material and (read upper, cold end after the auxiliary substance has relaxed is cooled. The method according to the invention can even without the help of an additional Refrigeration cycle z. B. in the ice led «-erden, (Iala the countercurrent decomposition products on cold end of the countercurrent a cold one Gas to lower the temperature added and the warm end of the counter strömers by temporarily removing a part the kalun dismantled product is heated, unless otherwise. about a add warmer gas. In both cases we <] the Condensation at the cold end and the steaming at the warm end inside to the d: ni rolling gas fraction strengthens and the rectifi- decorative effect achieved. For the sake of further Enhancement of the rectifying effect can the countercurrent on the Roligasseite also with intermediate oxides (rectiflorals) or the like. In the extraction of the Ätlivlen from coke furnace gas by means of the process finding is z. B. by the return liquid methane practically all of it : \ thvIen including the other KcAilen- Hydrogen with one or more C atoms washed out, whereby at the same time the production of methane and hydrogen is higher Preparing for purity. Through the warming of the lower end becomes a stronger evaporation of the ether fraction achieved in a manner known per se. Inner half of the countercurrent there is a rectifying exchange of substances between the Reverse fluid; cit finite the ascending Steaming, which makes it possible to counterflow one warm end Ethylene fraction court enrichment (up to via 65070 C # -lH4. ) at the highest yield remove. Two embodiments of the method according to the invention are hereinafter referred to Hand of figures representing a coke gas dismantling plant in a greatly simplified Represent scheme. described: The coke gas passes through line i (Abl) .ij in the Gegenstriinier _-1, D.C a. the e: the One after the other (lurclistr; itnt, 111111 is here in the exchange of arms finite the decomposition pro- <lukteii cooled down. Your h, -iksgas becomes into your capacitor d. Methane al) divorced. that the system via line 3 through the Countercurrent _-i, B. C leaves. From your am Iwopf of the column d. withdrawing gas mixture is in the Sätile; with the addition of cold. expanded nitrogen a synthesis gas (1-I, -? - \.,) Won. that about the line tungell t;, a and i = is taken. That Residual gas, mainly Kolilenosvd and Nitrogen. will be at the bottom of the pillar Taken in liquid form, initially via duct your counterflow C is partially filled. where it is is steaming. and then about the opposite Strönier D and P headed. As cold Nitrogen, which serves as a carrier, is device 8, countercurrents D and F_ after preliminary discharge voltage your capacitor .l supplied. iv, i the liquidation of the - \ letlian fraction takes place. \ zicli another 1; tit # pannily it becomes liquid accruing stickstoa for irrigation of the Pillar ; used: the relaxed gas Fine nitrogen is piped over (Gegetiströnier P »the renewed compression fed. The application of the procedure according to the Invention is labeled by the Arrangement of the line io with valve ii and of the line 12 finite valve 13- The line 1o allows bypassing the opposite ströniers C through part of the Sviltliese- gases (I H .., - (- Na). The more gas iil) he the LeituiMg io is branched. inn so colder the upper end of the counterflow D. As a result, coke gas is chic relatively strong condensation of Uetlian, which uses the Ethylene washes out (] a gas. -With help (I-> ethylene ii can be the cheapest component temperature at the cold end of the counterflow l; to adjust. On the other hand, at point 14 from I_eitllllg 2 a part of the in pillar 3 @ v, iinienen Svntlie: egases via line 12 regulated and your countercurrent pounded, w ähi # -end e # normally the plant iil> tr Gegetiströnier A was left. The more v @@ u from this gas finitely with the help of valve 13 is regulated, the more tv @ irmer the counter stream A at the lower end and so on The rolling gas also kicks in below the counterflow D a, so that a strong Evaporation of the washing liquid serving - \ letlians enters. In this way the most favorable temperature ratios nisse in Gegenströnier D according to the invention created to a hocliwertihe: lthv @ en- faction zti received. That partly already in the counterflow;> tner.-1. ini rest of the (; egetistr @ nier D attifallen (le Ethylene is fed to separator 15: the liquid ethylene fraction obtained is discharged via line 16 and countercurrent E and D.

Es ist nicht unbedingt erforderlich, die Beeinflussung der Temperaturen des Gegenströmers b' mit Hilfe des Synthesegases vorzunehmen. Gegebenenfalls können auch andere Zerlegungsprodukte hierfür herangezogen werden.It is not absolutely necessary to influence the temperatures of the countercurrent b 'to be carried out with the aid of the synthesis gas. If necessary, can other decomposition products can also be used for this purpose.

Trotzdem erfindungsgemäß dem Gegenströmersystem A, B, C an einer Stelle ein zu kaltes Zerlegungsprodukt - zugesetzt wird, und an anderer Stelle ein Teil eines Zer-.lea,-ungsproduktes wieder entnommen wird, läßt sich die Einregulierung der Temperaturen im allgemeinen doch so durchführen, daß am warmen Ende des Gegenströmers A die Temperaturdifferenz nicht nennenswert erhöht wird. Sollte in gewissen Fällen trotzdem der Kälteverlust steigen, so entspricht eben dem höheren Energieaufwand der Gewinn einer, besonders wertvollen Äthylenfraktion.Despite the fact that, according to the invention, a decomposition product that is too cold is added to the countercurrent system A, B, C at one point, and part of a decomposition product is withdrawn at another point, the temperature can generally be regulated as follows: that at the warm end of the countercurrent A, the temperature difference is not significantly increased. If, in certain cases, the loss of cold should nevertheless increase, the gain in a particularly valuable ethylene fraction corresponds to the higher expenditure of energy.

Im Beispiel der Abb.2 wirr. die Durchführung des Verfahrens nach der Erfindung mit Hilfe: eines zusätzlichen Käl'"tkikreislaufs z. B. Methan gezeigt. Es kann sich, dabei um eine gleichartige Gaszerlegungsandage handeln wie im Beispiel der Abb. i. Das verdichtete, gasförmige Kühlmittel tritt durch Leitung 17 in den Gegenströmer F ein, in dem es sich im Wärmeaustausch mit dem entspannten kalten Kühlmittel abkühlt, das über Leitung i8 zu dem nicht gezeichneten Verdichter zurückgeführt wird. Die Heizung des Gegenströmers B durch das noch nicht entspannte Kühlmittel erfolgt über das am unteren Ende des Gegenströmers eingebaute Rohrsystems i9, die Kühlung erfolgt nach Entspannung des Kühlmittels im Venti12o über das am oberen Ende eingebaute Rohrsystem 21. Der Kältebedarf ist verhältnismäßig gering, da er sich im wesentlichen auf die Kondensabion.skälte für die Äthylenfraktion beschränkt, ohne daß die Kälteverluste der Anlage nennenswert erhöht werden.In the example of Fig. 2 confused. the implementation of the procedure according to the Invention with the aid of an additional refrigeration cycle, e.g. methane, is shown. It can be a gas decomposition bandage of the same type as in the example of fig. i. The compressed, gaseous coolant passes through line 17 into the Countercurrent F a, in which it is in heat exchange with the relaxed cold Coolant cools, which is returned via line i8 to the compressor, not shown will. The heating of the counterflow B by the coolant that has not yet been expanded takes place via the pipe system i9 installed at the lower end of the counterflow, the Cooling takes place after the coolant has been released in the Venti12o via the one at the top End of built-in pipe system 21. The cooling requirement is relatively low, since it is essentially limited to the condensation cold for the ethylene fraction, without the cooling losses of the system being significantly increased.

Das erfindungsgemäße Verfahren ermöglicht es, durch Veränderung der maßgebenden Temperaturen in dem als Rücklaufgegenströmer ausgebildeten Wärmeaustauscher B die Konzentration des Äthylens in der gewonnenen Fraktion weitgehend, und zwar etwa innerhalb der Grenzen von 25 biis 65'/o oder bis ztt noch höherer Anreicherung zu beeinflussen. Im wesentlichen liegt der Nutzen der Erfindung natürlich in der Erzeugung einer möglichst hohen Anreicherung des Äthylens bei gleichzeitig hoher Ausbeute. Die Temperabur-regulierungen müssen entsprechend der Zusammensetzung des Rohgases vorgenommen, werden. Es braucht sich bei der Anwendung der Erfindung' nicht nur um Koksofengas normaler Zusammensetzung zu handeln, sondern es können auch ähnliche Gase, z. B. Hydrierabgase oder Konvertgase, mit. gleichem Erfolg zur Verarbeitung kommen. Bei Koksofengas normaler Zusammensetzung beträgt die Temperaturerhöhung am warmen Ende etwa 15°, die Temperatursenkung am kalten Ende etwa Sc, so daß 'heim Geaglenströmer B statt der üblichen Temperaturen von -1.f5° am oberen (kalten) Ende und von --i oo° am unteren (warmen) Ende die Terni)eraturen etwa -150° und. -R5° betragen.The inventive method makes it possible by changing the decisive temperatures in the heat exchanger designed as a return countercurrent B the concentration of ethylene in the fraction obtained largely, namely approximately within the limits of 25 to 65% or up to an even higher enrichment to influence. Essentially, of course, the utility of the invention resides in that Generation of the highest possible enrichment of ethylene with a high concentration at the same time Yield. The temperature regulations must correspond to the composition of the Raw gas are made. There is no need to apply the invention only to act around coke oven gas of normal composition, but it can also be similar Gases, e.g. B. hydrogenation gases or convert gases, with. same success for processing come. In the case of coke oven gas of normal composition, the temperature increase is at the warm end about 15 °, the temperature drop at the cold end about Sc, so that 'home Geaglenströmmer B instead of the usual temperatures of -1.5 ° at the upper (cold) end and from --i oo ° at the lower (warm) end the terni) eratures about -150 ° and. -R5 ° be.

Claims (3)

PATENTANSPRÜCHE: i. Verfahren zur Abscheidung einer Fraktion aus Gasgemischen, z. B. einer Äthylenfr a'ltion aus Kokso,fe,tiga,s, im Verlaufe der Tiefkühlung des Gasgemisches in Wärmeaustauschern, dadurch gekennzeichnet, daß während des Wärmeaustausches in einem Gegenströmer dieser zusätzlich am warmen Ende erwärmt und am kalten Ende gekühlt wird. PATENT CLAIMS: i. Process for separating a fraction from gas mixtures, z. B. an Äthylenfr a'ltion from Kokso, fe, tiga, s, in the course of the freezing of the Gas mixture in heat exchangers, characterized in that during the heat exchange in a countercurrent this is additionally heated at the warm end and at the cold end is cooled. 2. Verfahren nach Anspruch i, dadurch gedaennzeichnet, daß mittels eines an sich bekannten Kältekreislaufs eines Hilfsstoffes, z. B. Methan, das untere (warme) Ende des Gegenströmers (B) vor der Entspannung des Hilfsstoües beheizt und das obere (kalte) Ende nach der 1-7ntspannüng des Hilfsstoffes gekühlt wird. 2. The method according to claim i, characterized in that means a known refrigeration cycle of an auxiliary material, e.g. B. Methane, the lower one (warm) end of the countercurrent (B) heated and before the expansion of the auxiliary substance the upper (cold) end is cooled after the 1-7 relaxation of the excipient. 3. Verfahren nach Anspruch i, dadurch a kennzeichnet, daß den dem Rotgas entgegenströmenden Zerlegungsprodukten am kalten Ende des Gegensbrömers ein kaltes Gas zugesetzt und das warme Ende des Gegensbrömers durch Zwischenentnahnie eines Teils der kalten Zerle-,C Y u Ilgsprodulde erwärmt wird. Vorrichtung zur Durchführung der Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß der @egenströmer auf der Rohgaisseite mit Zwischenböden (Rektifizierböden) od. dgl. versehen ist.3. Method according to claim i, characterized in that the flow counter to the red gas A cold gas is added to the decomposition products at the cold end of the counterbreamer and the warm end of the Gegenbrömers by taking part of the cold in between Zerle-, C Y u Ilgsprodulde is heated. Device for carrying out the process according to claims 1 to 3, characterized in that the egenströmer is on the raw gas side is provided with intermediate floors (rectification floors) or the like.
DEG107972D 1943-07-31 1943-07-31 Process for separating mixture components Expired DE764953C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2844944A (en) * 1954-12-07 1958-07-29 Linde Eismasch Ag Process for obtaining a gas fraction which is highly rich in carbon monoxide from a carbon monoxide containing gas mixture

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2844944A (en) * 1954-12-07 1958-07-29 Linde Eismasch Ag Process for obtaining a gas fraction which is highly rich in carbon monoxide from a carbon monoxide containing gas mixture

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