DE1643757A1 - Process for the joint separation of acetylene and ethylene from fission gases - Google Patents

Process for the joint separation of acetylene and ethylene from fission gases

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Publication number
DE1643757A1
DE1643757A1 DE19681643757 DE1643757A DE1643757A1 DE 1643757 A1 DE1643757 A1 DE 1643757A1 DE 19681643757 DE19681643757 DE 19681643757 DE 1643757 A DE1643757 A DE 1643757A DE 1643757 A1 DE1643757 A1 DE 1643757A1
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Germany
Prior art keywords
ethylene
acetylene
gas
gas mixture
separation
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DE19681643757
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German (de)
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DE1643757C3 (en
DE1643757B2 (en
Inventor
Axel Dr Danneil
Otto Dr Nagel
Rolf Dr Platz
Kurt Dipl-Ing Taglieber
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BASF SE
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BASF SE
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Priority to US798041A priority Critical patent/US3607963A/en
Priority to BE728312D priority patent/BE728312A/xx
Priority to SE01927/69A priority patent/SE348721B/xx
Priority to GB7522/69A priority patent/GB1248693A/en
Priority to FR6903294A priority patent/FR2001799A1/fr
Priority to AT147569A priority patent/AT288336B/en
Priority to ES363604A priority patent/ES363604A2/en
Publication of DE1643757A1 publication Critical patent/DE1643757A1/en
Publication of DE1643757B2 publication Critical patent/DE1643757B2/en
Application granted granted Critical
Publication of DE1643757C3 publication Critical patent/DE1643757C3/en
Expired legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—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
    • F25J3/0271—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/CO mixtures, i.e. of synthesis gas
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/005—Processes comprising at least two steps in series
    • 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
    • F25J3/0238—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
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead 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
    • 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
    • F25J2205/50—Processes or apparatus using other separation and/or other processing means using absorption, i.e. with selective solvents or lean oil, heavier CnHm and including generally a regeneration step for the solvent or lean oil
    • 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
    • F25J2210/12—Refinery or petrochemical off-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
    • 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
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Verfahren zur gemeinsamen Abtrennung von Acetylen und Athylen aus Spaltgasen Zusatz zu Patent . ... ... (Anmeldung B 88 454 IVb/120) Gegenstand des Hauptpatents . ... (Anmeldung B 88 454 IVb/120) ist ein Verfahren zur gemeinsamen Abtrennung von Acetylen und Äthylen aus Spaltgasen, die bei der Spaltung von Erdöl oder Erdölfraktionen durch eie unter der Flüssigkeitsoberfläche brennende Flamme erhalten werden, und aus denen Kohlendioxid und Schwefelwasserstoff entfernt worden sind, bei dem man aus den Spaltgasen nach deren Trocknung einen Teil des Methans und die gesamten übrigen Kohlenwasserstoffe durch Kondensation abscheidet und anschließend durch eine Druckdestillation das Acetylen und Äthylen zusammen mit Methan und Äthan von einer flüssigen Fraktion, die die gesamten C3- bis C5-Kohlenwasserstoffe und gegebenenfalls Kohlenoxysulfid und Schwefelwasserstoff enthält, abtrennt.Process for the joint separation of acetylene and ethylene from Fission gases addendum to patent. ... ... (Registration B 88 454 IVb / 120) Subject of the Main patent. ... (registration B 88 454 IVb / 120) is a procedure for joint Separation of acetylene and ethylene from fission gases, which are used in the cracking of petroleum or petroleum fractions by a flame burning under the surface of the liquid and from which carbon dioxide and hydrogen sulfide have been removed are, in which one from the fission gases after their drying a part of the methane and separates all the remaining hydrocarbons by condensation and then by pressure distillation the acetylene and ethylene together with methane and ethane of a liquid fraction containing all of the C3 to C5 hydrocarbons and optionally contains carbon oxysulfide and hydrogen sulfide, separates.

Bei der Durchführung des Verfahrens nach dem Hauptpatent .When carrying out the process according to the main patent.

(Anmeldung B 88 454 IVb/l20) hat sich gezeigt, daß unter bestimmten Bedingungen, z.B. wenn das Restgas aus den Abscheidern einen bestimmten Acetylen-Gehalt überschreitet, bei der weiteren Abkühlung Acetylen z. B. in den Entspannungsturbinen in fester Form aus fallen kann. Dadurch wird ein gelegentliches Abtauen der Turbine wie auch eventuell der folgenden Wärmeaustauscher notwendig. Durch das Auftauen kann der kontinuierliche Betrieb gestört werden.(Application B 88 454 IVb / 120) has shown that under certain Conditions, e.g. when the residual gas from the separators a certain Acetylene content exceeds, in the further cooling acetylene z. Tie Relaxation turbines in solid form can fall out. This makes an occasional It is necessary to defrost the turbine and possibly the following heat exchangers. Thawing can disrupt continuous operation.

Es wurde nun gefunden, daß man eine Störung der kontinuierlichen Arbeitsweise durch Abscheidung von Acetylen in fester Form vermeidet, wenn man in Abänderung des Verfahrens nach dem Hauptpatent die Kondensation der Kohlenwasserstoffe unterteilt, wobei man zunächst in einer oder mehreren Kondensationsstufen auf eine Temperatur, die noch oberhalb der Festpunkttemperatur des Acetylens im Gemisch mit den weiteren kondensierten Bestandteilen liegt, auf -82 bis -1200C abkühlt, nach Abtrennung des dabei anfallenden Kondensates das verbleibende, noch geringe Mengen Acetylen enthaltende Gasgemisch in einer Waschkolonne durch Auswaschen mit flüssigem Äthylen und/oder Xthan vom Acetylen befreit und darauf das acetylenfreie Gasgemisch weiter auf -140 bis -1700C abkühlt.It has now been found that there is a disruption of the continuous operation by separating acetylene in solid form if one avoids in modification the process according to the main patent divides the condensation of hydrocarbons, where one first in one or more condensation stages to a temperature, those still above the fixed point temperature of the acetylene in a mixture with the others condensed constituents is, cools to -82 to -1200C, after separation of the the resulting condensate contains the remaining, still small amounts of acetylene Gas mixture in a scrubbing column by scrubbing with liquid ethylene and / or Xthane freed from acetylene and then the acetylene-free gas mixture further to -140 cools down to -1700C.

Bei dem erfindungsgemäßen Verfahren treten die oben beschriebenen Nachteile nicht ein, da der Acetylengehalt durch eine Unterteilung der Kondensation und Einschaltung einer Äthylenwäsche so weit herabgesetzt wird, daß die Abscheidung von festem Acetylen nicht mehr eintreten kann.In the method according to the invention, those described above occur Disadvantages are not a, since the acetylene content by a subdivision of the condensation and switching on an ethylene scrubber is reduced so far that the separation of solid acetylene can no longer enter.

Bei der Durchführung des Verfahrens kann die notwendige Vorabtrennung der Kohlendioxidanteile sowie gegebenenfalls des Schwefels z.B. in Form von Schwefelwasserstoff in bekannter Weise durch eine Wäsche, z.B. mit einer wäßrigen Lösung von Alkalisalzen von Aminosäure, vorgenommen werden. Im allgemeinen kann man hierfür Verfahren verwenden, auf die bereits im Hauptpatent hingewiesen ist.When carrying out the process, the necessary preliminary separation the carbon dioxide content and possibly the sulfur, e.g. in the form of hydrogen sulfide in a known manner by washing, e.g. with an aqueous solution of alkali salts of amino acid. In general, one can use methods for this purpose, which is already referred to in the main patent.

Dies gilt auch für eine eventuelle Feinreingung von Kohlendioxid sowie die nachfolgende Trocknung der von Kohlendioxid und Schwefelwasserstoff befreiten Spaltgase vor der Kondensation. Neben der im Hauptpatent genannten Trocknung hat sich auch die Wäsche mit wasserfreiem Methanol oder aber eine Sättigung mit Methanoldampf als geeignet erwiesen.This also applies to any fine cleaning of carbon dioxide as well the subsequent drying of the freed from carbon dioxide and hydrogen sulfide Fission gases before condensation. In addition to the drying mentioned in the main patent washing with anhydrous methanol or saturation with methanol vapor proved suitable.

Die Kondensation selbst wird im allgemeinen bei einem Druck von 5 bis 40 at vorgenommen. Eine besondere Durchführungsform des Verfahrens besteht darin, daß man das nach der Äthylenwäsche auf -140 bis 17000 abgekühlte Gas nach erneuter Kondensatabscheidung im Gegenstrom zu dem die Athylenwäsche verlassenden Gas auf -130 bis-loO0C erwärmt. Das in dieser Weise erwärmte Gasgemisch kann in einer Entspannungsmaschine unter Leistung äußerer Arbeit entspannt werden, wobei sich das Gasgemisch abkühlt und zur Gegenstromkühlung in den Kondensationsstufen Verwendung findet.The condensation itself is generally at a pressure of 5 made to 40 at. A special form of implementation of the procedure consists in that after the ethylene scrubbing to -140 to 17000 cooled gas after renewed Separation of condensate in countercurrent to the gas leaving the ethylene scrubbing -130 to -10O0C warmed. The gas mixture heated in this way can be used in an expansion machine be relaxed while performing external work, whereby the gas mixture cools down and is used for countercurrent cooling in the condensation stages.

Für die Wäsche des Gasgemisches nach Abkühlung auf -82 bis 12000 kann man das Kondensat verwenden, das bei der Abkühlung nach der Äthylenwäsche auf -140 bis -170°C erhalten wird. Man kann dieser Waschflüssigkeit aber gegebenenfalls auch zusätzliche Mengen von Äthylen und/oder Äthan zuführen, die aus anderer Quelle stammen.For washing the gas mixture after cooling to -82 to 12000 can you can use the condensate that cools down after washing with ethylene to -140 to -170 ° C is obtained. You can do this But washing liquid optionally also supply additional amounts of ethylene and / or ethane, the come from another source.

Zur Abkühlung des Gasgemisches kann man die in den Kondensationsstufen oder gegebenenfalls in einer einzigen Kondensationsstufe vor der Äthylenwäsche abgeschiedenen Kondensate entspannen und im Gegenstromwärmeaustausch verdampfen.To cool down the gas mixture, one can use the in the condensation stages or optionally deposited in a single condensation stage before the ethylene scrubbing Relax condensates and evaporate in countercurrent heat exchange.

Beispiel In einer Anlage, die in der Abbildung wiedergegeben ist, treten durch Leitung (1) 14 000 Nm3/h Spaltgas, das von CO2 und H2S befreit und durch eine vorgeschaltete Nethanolwäsche getrocknet wurde, unter einem Druck von 8 at und mit einer Temperatur von +20°C in den Wärmeaustauscher (2) ein. Das Gas hat folgende Zusammensetzung: H2 29,37 Vol. Example In a system shown in the figure, pass through line (1) 14,000 Nm3 / h cracked gas, which frees from CO2 and H2S and was dried by an upstream ethanol wash, under a pressure of 8 at and at a temperature of + 20 ° C in the heat exchanger (2). The gas has the following composition: H2 29.37 vol.

N2 0,59" CO 40,10 " 02 0,20 " CH4 3,96 " C2H4 6,46 " C2H6 0,49 " C3H6 3,84 " C5H8 2,46 " C4Hlo 4,89 " C2112 6,95 " CH3OH 0,69 ". N2 0.59 "CO 40.10" 02 0.20 "CH4 3.96" C2H4 6.46 "C2H6 0.49" C3H6 3.84 "C5H8 2.46" C4Hlo 4.89 "C2112 6.95" CH3OH 0.69 ".

Das Gas wird auf -200C abgekühlt. Das anfallende Kondensat wird im Abscheider (3) abgetrennt; das verbleibende Gas wird über Leitung (4) durch Wärmetauscher (5) geführt, auf -1100C gekühlt und im Abscheider (6) von Kondensat befreit. Das Restgas strömt durch Leitung (7) in die Kolonne (8), wo es durch eine Gegenstromwäsche mit einem im wesentlichen aus flüssigem Äthylen und Äthan bestehenden Gemisch von Acetylen so weit befreit wird, daß der Acetylen-Gehalt in Leitung (9), bezogen auf das Gemisch von Acetylen und Äthylen, unter 1 % liegt, so da# bei der weiteren Abkühlung auf -165°C im Wärmetauscher (10) keine Ausscheidung von festem Acetylen auftreten kann. Im Abscheider (11) wird Gas und Flüssigkeit getrennt. Das Gas mit einem Restgehalt an Äthylen und 2 000 ppm und an Acetylen von weniger als 10 ppm wird mit Leitung (12) durch den Wärmetauscher (10) geleitet und im Gegenstrom zum Gasstrom in Leitung (9) auf eine Temperatur von -1250C erwärmt und der Entspannungsturbine (1)) zugeführt. In ihr wird das Gas unter Leistung äußerer Arbeit von 7,8 at auf 1,4 at entspannt, wobei es sich auf 1690C abkühlt. Dieses kalte Gas wird durch Leitung (14), durch die Wärmetauscher (10), (5) und (2) im Gegenstrom zu den durch Leitung (1, 4 und 9) strömenden Medien, auf eine Temperatur von +100C erwärmt. Die in Abscheider (11) anfallende Kondensatmenge wird mit Pumpe (15) und durch Leitung (16) in den Wärmetauscher (10) zur Abgabe der fühlbaren Wärme gerührt und mit einer Temperatur von -1230C auf die Waschkolonne (8) gegeben. Zusätzlich zu dieser Waschflüssigkeit werden durch Leitung (17) 280 Nm3/h Äthylen-Äthan-Gemisch als Flüssigkeit von außen zugeführt und ebenfalls auf die Kolonne (8) gegeben, nachdem sie in den Wärmetauschern (2) und (5) auf -1200C abgekühlt wurden. Die beladene Waschflüssigkeit aus dem Sumpf der Kolonne (8) wird mit dem in dem Abscheider (6) anfallenden Kondensat gemischt und nach Entspannung auf 1,4 at durch Leitung (18) durch den Wärmetauscher (5) geleitet, anschließend mit dem aus Abscheider (3) durch Leitung (19) kommenden Kondensat gemischt und durch Leitung (20) zur weiteren Abgabe von latenter und fühlbarer Wärme durch Wärmetauscher (2) im Gegenstrom zu den eintretenden Gasströmen gerührt. In dem Kompressor (21) wird dieses Kohlenwasserstoffgemisch auf 18 at verdichtet und der Druckdestillation zugeführt.The gas is cooled to -200C. The resulting condensate is in the Separator (3) separated; the remaining gas is passed through a heat exchanger via line (4) (5), cooled to -1100C and freed of condensate in the separator (6). That Residual gas flows through line (7) into column (8), where it is washed through a countercurrent with a mixture consisting essentially of liquid ethylene and ethane Acetylene is freed so far that the acetylene content in line (9), based on the mixture of acetylene and ethylene is below 1%, so that # during further cooling at -165 ° C in the heat exchanger (10) no precipitation of solid acetylene occurs can. Gas and liquid are separated in the separator (11). The gas with a residual content of ethylene and 2,000 ppm and of acetylene of less than 10 ppm is with line (12) passed through the heat exchanger (10) and in countercurrent to the gas flow in line (9) heated to a temperature of -1250C and fed to the expansion turbine (1)). In it, the gas is expanded from 7.8 at to 1.4 at with the performance of external work, where it cools down to 1690C. This cold gas is passed through line (14) the heat exchangers (10), (5) and (2) in countercurrent to the through line (1, 4 and 9) flowing media, heated to a temperature of + 100C. The in separator (11) Accumulating amount of condensate is pumped (15) and through line (16) into the heat exchanger (10) stirred to give off the sensible heat and kept at a temperature of -1230C added to the wash column (8). In addition to this washing liquid are through management (17) 280 Nm3 / h ethylene-ethane mixture as a liquid of fed externally and also given to the column (8) after they have been in the heat exchangers (2) and (5) were cooled to -1200C. The loaded washing liquid from the sump the column (8) is mixed with the condensate obtained in the separator (6) and after relaxation to 1.4 at passed through line (18) through the heat exchanger (5), then mixed with the condensate coming from separator (3) through line (19) and through line (20) for the further release of latent and sensible heat Heat exchanger (2) stirred in countercurrent to the incoming gas streams. In the compressor (21) this hydrocarbon mixture is compressed to 18 atm and the pressure distillation fed.

Dieses Gasgemisch hat folgende Zusammensetzung: H2 0,28 Vol,-% N2 0,06 " CO 1,70 " 02 0,03 " CH4 1,10 " C2H4 33,43 " C2H6 1,30 C3H6 14,00 " C3H8 8,90 " C4H10 17,60 " C2H2 21, " -Bei der beschriebenen Arbeitsweise der Trennanlage mit einer Zwischenwäsche mit Äthylen in der Kolonne (8) wird auch beim Dauerbetrieb keine Festausscheidung von Acetylen beobachtet.This gas mixture has the following composition: H2 0.28% by volume N2 0.06 "CO 1.70" 02 0.03 "CH4 1.10" C2H4 33.43 "C2H6 1.30 C3H6 14.00" C3H8 8.90 "C4H10 17.60" C2H2 21, " -With the described mode of operation of the Separation plant with an intermediate wash with ethylene in the column (8) is also used No solid precipitation of acetylene observed in continuous operation.

Claims (5)

Patentansprüche 1, Verfahren zur gemeinsamen Abtrennung von Acetylen und Äthylen aus Spaltgases nach Patent . ... ... (Anmeldung B 88 454 I'b,42o), dadurch Rekennzelthnet daß man in Abanderung des Verfahrens nach dem Hauptpatent die Kondensation der Kohlenwasserstoffe unterteilt, wobei man zunächst in einer oder mehreren Kondensationsstufen auf eine Temperatur, die noch oberhalb der Festpunkttemperatur des Acetylens im Gemisch mit den weiteren kondensierten Bestandteilen liegt, auf 82 bis -120°C abkühlt, nach Ab trennung des dabei erhaltenen Kondensats das verbleiben de, noch geringe Mengen Acetylen enthaltende Gasgemisch in einer Waschkolonne durch Auswaschen mit flüssigem Athylen und/ oder Athan vom Acetylen befreit und darauf das aeetylenfreie Gasgemisch weiter auf -140 bis -1700C abkühlt.Claims 1, a process for the joint separation of acetylene and ethylene from cracked gas according to patent. ... ... (registration B 88 454 I'b, 42o), thereby Rekennzelthnet that in a modification of the process according to the main patent, the condensation divided into hydrocarbons, initially in one or more condensation stages to a temperature which is still above the fixed point temperature of the acetylene in the Mixture with the other condensed components cools to 82 to -120 ° C, after separation of the resulting condensate the remaining de, still low Amounts of acetylene-containing gas mixture in a scrubbing column by washing with liquid ethylene and / or ethane freed from acetylene and then the aeetylene-free Gas mixture cools further to -140 to -1700C. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß man das auf -140 bis -1700C abgekühlte Gas nach erneuter Kondensatabscheidung im Gegenstrom zu dem die Äthylenwäsche verlassenden Gas auf -130 bis -100°C erwärmt.2. The method according to claim 1, characterized in that the Gas cooled to -140 to -1700C after renewed condensate separation in countercurrent warmed to the gas leaving the ethylene scrubbing to -130 to -100 ° C. 3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß man das auf -130 bis -1000C erwärmte Gasgemisch in einer Entspannungsmaschine unter Leistung äußerer Arbeit entspannt, wobei sich das Gasgemisch abkühlt und zur Gegenstromkühlung in den Kondensationsstufen verwendet wird.3. The method according to claim 2, characterized in that the Gas mixture heated to -130 to -1000C in an expansion machine under power external work relaxes, whereby the gas mixture cools and for countercurrent cooling is used in the condensation stages. 4. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß man als Äthylen und/oder Athan enthaltende Waschflüssigkeit das bei der Abkühlung auf -140 bis -1700C enthaltene Kondensat, gegebenenfalls unter Zusatz weiterer aus anderen Quellen stammenden Mengen von Äthylen md/oder Äthan, verwendet.4. The method according to claim 1 to 3, characterized in that one as washing liquid containing ethylene and / or athan on cooling -140 to -1700C condensate contained, if necessary with the addition of others from others Sources derived amounts of ethylene md / or ethane, used. 5. Verfahren nach Anspruch 1 bis 4, dadurch gekennzeichnet, daß man zur Abkühlung des Gasgemisches die in den Kondensationsstufen abgeschiedenen Kondensate entspannt und im Gegenstromwärmeaustausch verdampft.5. The method according to claim 1 to 4, characterized in that one the condensates separated in the condensation stages to cool the gas mixture relaxed and evaporated in countercurrent heat exchange. LeerseiteBlank page
DE19681643757 1968-02-13 1968-02-13 Process for the production of a condensate containing acetylene, xthane, ethylene and C deep 3 to C deep 5 hydrocarbons Expired DE1643757C3 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US798041A US3607963A (en) 1968-02-13 1969-02-10 Separation of acetylene and ethylene from cracked gas
SE01927/69A SE348721B (en) 1968-02-13 1969-02-12
GB7522/69A GB1248693A (en) 1968-02-13 1969-02-12 Joint separation of acetylene and ethylene from cracked gases
FR6903294A FR2001799A1 (en) 1968-02-13 1969-02-12
BE728312D BE728312A (en) 1968-02-13 1969-02-12
AT147569A AT288336B (en) 1968-02-13 1969-02-13 Process for the joint separation of acetylene and ethylene from fission gases
ES363604A ES363604A2 (en) 1968-02-13 1969-02-13 Separation of acetylene and ethylene from cracked gas

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DEB0088454 1966-08-12
DEB0096628 1968-02-13
DEB0096628 1968-02-13

Publications (3)

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DE1643757A1 true DE1643757A1 (en) 1972-04-27
DE1643757B2 DE1643757B2 (en) 1973-03-08
DE1643757C3 DE1643757C3 (en) 1976-07-22

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2917505A1 (en) * 1979-04-30 1980-11-13 Linde Ag Ethylene sepn. from gas-stream contg. hydrogen and methane - by rectifying with reflux prodn. by multistep partial condensn.

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2917505A1 (en) * 1979-04-30 1980-11-13 Linde Ag Ethylene sepn. from gas-stream contg. hydrogen and methane - by rectifying with reflux prodn. by multistep partial condensn.

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