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EP2122282B1 - Verfahren und vorrichtung zur trennung einer mischung aus kohlenmonoxid, methan, wasserstoff und stickstoff durch kryogene destillation - Google Patents

Verfahren und vorrichtung zur trennung einer mischung aus kohlenmonoxid, methan, wasserstoff und stickstoff durch kryogene destillation Download PDF

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Publication number
EP2122282B1
EP2122282B1 EP07871946.5A EP07871946A EP2122282B1 EP 2122282 B1 EP2122282 B1 EP 2122282B1 EP 07871946 A EP07871946 A EP 07871946A EP 2122282 B1 EP2122282 B1 EP 2122282B1
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Prior art keywords
column
cycle
carbon monoxide
methane
separating
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EP07871946.5A
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English (en)
French (fr)
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EP2122282A2 (de
Inventor
Arthur Darde
Natacha Haik-Beraud
Antoine Hernandez
Guillaume Teixeira
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Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Priority to PL07871946T priority Critical patent/PL2122282T3/pl
Publication of EP2122282A2 publication Critical patent/EP2122282A2/de
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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
    • F25J3/0204—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
    • F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis 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
    • 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
    • F25J3/0252—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 hydrogen
    • 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
    • F25J3/0257—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 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
    • 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
    • F25J3/0261—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 carbon monoxide
    • 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
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2205/30—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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal 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
    • F25J2270/04—Internal refrigeration with work-producing gas expansion 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
    • F25J2270/08—Internal refrigeration by flash gas recovery 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
    • F25J2270/24—Quasi-closed internal or closed external carbon monoxide refrigeration cycle
    • 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
    • Y10S62/92—Carbon monoxide

Definitions

  • the present invention relates to a method and an installation for separating a mixture of carbon monoxide, methane, hydrogen and nitrogen by cryogenic distillation.
  • Figure 6 of Berninger's article presents a method and an installation according to the preambles of claims 1 and 14 respectively.
  • Other documents describing methane scrubbing processes include: EP-A-0928937 , US4478621 , Tieftemperaturtechnik, page 418.
  • Carbon monoxide from cold boxes H 2 / CO carries with it a large fraction of the nitrogen present in the feed gas. This phenomenon is related to the difficulty of separating the two components CO and N 2 , their bubble points being very close. Nevertheless, depending on the use made of the CO downstream of the cold box, it is sometimes necessary to reduce its nitrogen content before exporting it.
  • denitrogenation column whose function is to produce carbon monoxide tank at the required purity.
  • a nitrogen purge containing a fraction of CO is recovered.
  • the denitrogenation column is located either upstream or downstream of the CO / CH 4 separation column.
  • the first advantage of the invention is that the lowest CO vaporization pressure is about 2.6 bar abs, and the highest pressure around 35 bar abs. This most often makes it possible to compress the CO cycle by a centrifugal compressor with five stages (six maximum).
  • the HP cycle pressure corresponds fairly well with the CO pressures often required (especially for the production of acetic acid).
  • the sending of carbon monoxide medium pressure from the turbine to the denitrogen tank saves a lot on the investment of the heat exchanger 9.
  • a flow containing carbon monoxide, hydrogen, methane and nitrogen 45 cools in exchanger 9 by heat exchange with a flow of carbon monoxide 1 and is sent to a methane scrubber column.
  • a flow of synthesis gas is sent to a methane washing column C1 fed at the top by a flow of liquid methane 4.
  • the tank liquid (not shown) is sent to the exhaust column C2 in a known manner and a fluid hydrogen-free is sent from the exhaust column C2 to the CO / CH 4 C3 separation column.
  • a flow rate enriched with carbon monoxide is withdrawn at the top of column C3 is sent to denitrogenation column C4 to remove nitrogen.
  • a flow of pure carbon monoxide 1 at a low pressure is sent to a compressor stage V1.
  • Part 3 of carbon monoxide compressed at between 3.5 and 5 bar, for example 4.3 bar in V1 cools in exchanger 9 and is sent to the bottom of the denitrogenation column C4 in gaseous form.
  • the rest of the carbon monoxide is compressed again in a compressor V2 to a pressure between 25 and 45 bar, preferably between 32 and 35 bar to form the flow 5.
  • This flow is divided into a portion 7 which constitutes a production and another flow that is sent to the exchanger 9.
  • a fraction 13 passes entirely through the exchanger before being divided into three.
  • a first flow 19 serves to reboil the exhaust column C2
  • a second flow 23 serves to reboil the CO / methane C3 column and the two cooled flow rates 19, 23 are sent with the third flow 21 to a heat exchanger 17 where they liquefy .
  • the flow 23 is divided in two, a portion 25 being expanded in a valve 27 and then vaporized in the exchanger 17 and sent in gaseous form in the tank of the denitrogenation column C4.
  • the remainder 26 of the flow 23 is expanded to a pressure of 2.6 bar and sent to a separator pot 35 after expansion in a valve.
  • the flow rates 21, 19 are also expanded in valves and sent to the same separator pot 35.
  • the gas 43 formed in the separator pot 35 is returned to the compressor V1 after reheating in the exchanger 9.
  • the liquid of the separator pot 35 is divided into four. Part 1 is sent to a separator pot 33 where it forms a gaseous fraction 41 and a liquid fraction 31.
  • the liquid fraction 31 vaporizes in the exchanger 17.
  • the gaseous fraction 41 is heated in the exchanger 17 against the flow rates 19 , 21, 23 before being returned to the compressor V1.
  • Part 2 serves to sub-cool the methane wash column C1 before being mixed at the flow rate 41.
  • Part 3 serves to condense the head of the column CO / methane C3 where it vaporizes and is then returned to the compressor V1.
  • the fourth portion 37 is mixed with the bottom liquid 29 of the denitrogenation column and serves to cool the head thereof.
  • the formed flow 39 is returned to the compressor V1.
  • a flow 11 cools partially in the exchanger 9, is expanded in a turbine T, cools in the exchanger 17 as flow 15 and is sent to the bottom of the denitrogenation column C4.
  • a separating pot C1 a depletion column C2, a CO / CH 4 C3 separation column and a CO C4 denitrogenation column are recognized.
  • a separating pot C1 a depletion column C2, a CO / CH 4 C3 separation column and a CO C4 denitrogenation column are recognized.
  • synthesis gas inlet and the carbon monoxide cycle are shown.
  • a flow rate 45 containing carbon monoxide, hydrogen, methane and nitrogen is cooled in exchanger 9 by heat exchange with a flow of carbon monoxide 1 and then in exchanger 17 and is sent to the separator pot.
  • the tank liquid of the pot C1 is sent to the top of the depletion column C2.
  • the overhead gas of the C1 column enriched in hydrogen leaves the installation.
  • the bottom liquid of the exhaustion column C2 is cooled in the exchanger 17 and sent to a CO / methane C3 separation column.
  • This tank liquid cools in the exchanger 17, is divided in two, a part 57 is sent to the CO / methane separation column and the remainder 55 is expanded, heated in the exchanger 17 to an intermediate temperature and then sent to the CO / methane C3 separation column.
  • a flow of impure carbon monoxide 1 at a low pressure is sent to a compressor stage V1.
  • Medium pressure carbon monoxide is divided in half.
  • the medium pressure flow 3 cools in the exchanger 9 and mixed with carbon monoxide from the turbine T and is sent to the bottom of the denitrogenation column C4.
  • a portion 11 at an intermediate temperature is expanded in a turbine T and sent to the denitrogenation column.
  • a fraction 13 completely crosses the exchanger before being divided into three.
  • a first flow 19 serves to reboil the exhaust column C2
  • a second flow 23 serves to reboil the CO / methane C3 column and the two cooled flow rates 19, 23 are sent with the third flow 21 to a heat exchanger 17 where they liquefy .
  • the flow 23 is divided in two, a portion 25 being expanded in a valve 27 and then vaporized in the exchanger 17 and sent in gaseous form to the denitrogenation column C4.
  • the remainder 26 of the flow 23 is expanded to a pressure of 2.6 bar and sent to a separator pot 35 after expansion in a valve.
  • the flow rates 21, 19 are also expanded in valves and sent to the same separator pot 35.
  • the gas 43 formed in the separator pot 35 is returned to the compressor V1 after reheating in the exchanger 9.
  • the liquid of the separator pot 35 is divided into three.
  • a part 1 is sent to a separator pot 33 where it forms a gaseous fraction 41 and a liquid fraction 31.
  • the liquid fraction 31 vaporizes in the exchanger 17.
  • the gaseous fraction 41 is heated in the exchanger 17 against the flow rates 19 , 21, 23 before being returned to the compressor V1.
  • Part 2 serves to cool the head of the column CO / CH 4 C3.
  • the formed flow 39 is returned to the compressor V1.
  • the third part 37 serves to cool the head of the denitrogenation column C4.
  • the formed flow 39 is returned to the compressor V1.
  • the liquid of the separator pot 35 can also ensure the cooling of the methane intended for the washing column C1.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Carbon And Carbon Compounds (AREA)

Claims (22)

  1. Verfahren zum Trennen eines Gemisches, welches mindestens Kohlenmonoxid, Wasserstoff, Stickstoff und Methan umfasst, wobei das Gemisch über ein erstes Trennmittel (C1) getrennt wird, welches eventuell aus einer Methanwaschkolonne besteht, mindestens eine flüssige Fraktion aus dem Sumpf des Trennmittels zu einer Strippkolonne (C2) geleitet wird, mindestens ein Teil der flüssigen Fraktion aus der Strippkolonne zu einer CO/CH4-Trennkolonne (C3) geleitet wird, um einen methanangereicherten flüssigen Strom und einen kohlenmonoxidangereicherten gasförmigen Strom zu erzeugen, und der kohlenmonoxidangereicherte gasförmige Strom zu einer Entstickungskolonne (C4) geleitet wird, und ausgehend von der Entstickungskolonne ein kohlenmonoxidreicher flüssiger Strom (29) und ein stickstoffreicher gasförmiger Strom erzeugt werden, wobei das Verfahren mindestens teilweise über einen Kohlenmonoxidkreislauf kalt gehalten wird, wobei der Kreislauf mindestens teilweise die Kondensation im Entstickungskolonnenkopf, und mindestens einen der folgenden Schrittesicherstellt:
    - das Kondensieren im Kopf der CO/CH4-Trennkolonne,
    - das Nachverdampfen im Sumpf der Strippkolonne, das Nachverdampfen im Sumpf der CO/CH4-Trennkolonne, das Kühlen des für das erste Trennmittel vorgesehenen Gemisches,
    - gegebenenfalls das Kühlen des für die Methanwaschkolonne vorgesehenen Methans, und
    - gegebenenfalls das Unterkühlen der Methanwaschkolonne,
    dadurch gekennzeichnet, dass das Kreislauf-Kohlenmonoxid in einem ersten Kreisverdichter (V1) auf einen mittleren Druck verdichtet wird und anschließend ein erster Teil (3) des Kreislauf-Kohlenmonoxids in den Sumpf der Entstickungskolonne (C4) geleitet wird, und ein zweiter Teil des Kohlenmonoxids auf einen hohen Druck verdichtet wird.
  2. Verfahren nach Anspruch 1, wobei das Kohlenmonoxid aus dem Kreislauf über einen Kreisverdichter (V1, V2) auf einen hohen Druck verdichtet, danach in einer Turbine (T) entspannt und in gasförmiger Form in den Sumpf der Entstickungskolonne (C4) geleitet wird.
  3. Verfahren nach Anspruch 2, wobei das Kreislauf-Kohlenmonoxid in einem ersten Kreisverdichter (V1) auf einen mittleren Druck verdichtet und anschließend zum Teil über den Kreisverdichter (V2) auf einen hohen Druck verdichtet wird, und ein Teil (3) des Kohlenmonoxids auf dem mittleren Druck in gasförmiger Form zur Entstickungskolonne (C4) geleitet wird.
  4. Verfahren nach einem der vorstehenden Ansprüche, wobei ein CO-Kreislaufstrom auf zwischen 25 und 45 bar, vorzugsweise auf zwischen 32 und 35 bar, den Sumpf der Strippkolonne (C2) und/oder den Sumpf der CO/CH4-Trennkolonne (C3) heizt.
  5. Verfahren nach einem der vorstehenden Ansprüche, wobei ein CO-Kreislaufstrom auf zwischen 25 und 45 bar, vorzugsweise auf zwischen 32 und 35 bar auf den Druck der Entstickungskolonne (C4) entspannt wird (T).
  6. Verfahren nach einem der vorstehenden Ansprüche, wobei ein CO-Kreislaufstrom (25) auf zwischen 3,5 und 5 bar in den Sumpf der Entstickungskolonne geleitet wird.
  7. Verfahren nach einem der vorstehenden Ansprüche, wobei sich ein CO-Kreislaufstrom (25) in einer Austauschleitung verflüssig, danach verdampf, und in den Sumpf der Entstickungskolonne geleitet wird.
  8. Verfahren nach einem der vorstehenden Ansprüche, wobei das erste Trennmittel eine Methanwaschkolonne (C1) ist.
  9. Verfahren nach Anspruch 8, wobei sich das zu trennende Gemisch (45) in der Methanwaschkolonne (C1) über Wärmeaustausch mit einem Kreislauf-Kohlenmonoxidstrom auf mindestens 2 bar, vorzugsweise zwischen 2 und 3 bar, abkühlt.
  10. Verfahren nach Anspruch 8 oder 9, wobei der CO-Kreislaufstrom die Kühlung des für die Methanwaschkolonne vorgesehenen Methans und/oder die Unterkühlung der Methanwaschkolonne (C1) sicherstellt.
  11. Verfahren nach einem der Ansprüche 1 bis 7, wobei das erste Trennmittel ein Phasentrenner (C1) ist.
  12. Verfahren nach einem der vorstehenden Ansprüche, wobei kohlenmonoxidangereicherte Ströme (2, 39) auf im Wesentlichen demselben Druck, vorzugsweise zwischen 2 und 4 bar, ja sogar 2 und 3 bar, mindestens zwei der folgenden Funktionen sicherstellen: Kältezufuhr zu einem Kopfkondensator der Entstickungskolonne (C4), Unterkühlung der Entstickungskolonne (C4) und Kühlung der Waschkolonne (C1), Kältezufuhr zu einem Kopfkondensator der CO/CH4-Trennkolonne (C3).
  13. Verfahren nach einem der vorstehenden Ansprüche, wobei ein Kohlenmonoxidverdichter einen Eingangsdruck von mindestens 1,5 bar, eventuell von mindestens 2 bar aufweist und Kohlenmonoxid empfängt, welches mindestens aus einem der folgenden Schritte stammt:
    o dem Kondensieren im Kopf der CO/CH4-Trennkolonne (C3),
    ∘ dem Kühlen des für die Methanwaschkolonne (C1) vorgesehenen Gemisches,
    ∘ dem Kühlen des für die Methanwaschkolonne vorgesehenen Methans,
    ∘ dem Unterkühlen der Methanwaschkolonne,
    ∘ dem Kondensieren im Kopf der Entstickungskolonne (C4).
  14. Anlage zum Trennen eines Gemisches, welches mindestens Kohlenmonoxid, Wasserstoff, Stickstoff und Methan umfasst, umfassend ein erstes Trennmittel (C1), welches eventuell eine Methanwaschkolonne ist, eine Strippkolonne (C2), eine CO/CH4-Trennkolonne (C3), und eine Entstickungskolonne (C4), eine Leitung, um das Gemisch in das erste Trennmittel zu leiten, eine Leitung, um mindestens eine flüssige Fraktion aus dem ersten Trennmittel zur Strippkolonne zu leiten, eine Leitung, um mindestens einen Teil der flüssigen Fraktion aus der Strippkolonne zur CO/CH4-Trennkolonne zu leiten, um einen methanangereicherten flüssigen Strom und einen kohlenmonoxidangereicherten gasförmigen Strom zu erzeugen, und eine Leitung, um den kohlenmonoxidangereicherten gasförmigen Strom aus der CO/CH4-Trennkolonne abzuziehen, eine Leitung, um den kohlenmonoxidangereicherten gasförmigen Strom zur Entstickungskolonne zu leiten, um einen kohlenmonoxidreichen flüssigen Strom und einen stickstoffreichen gasförmigen Strom zu erzeugen, wobei die Anlage mindestens teilweise über einen Kohlenmonoxidkreislauf (V1, V2, T) kalt gehalten wird, wobei der Kreislauf mindestens teilweise die Kondensation im Kopfkondensator der Entstickungskolonne, und eine der folgenden Funktionen sicherstellt:
    - das Kühlen eines Kopfkondensators der CO/CH4-Trennkolonne, das Aufheizen eines Sumpfnachverdampfers der Strippkolonne,
    - das Aufheizen eines CO/CH4-Trennkolonnen-Sumpfnachverdampfers.
    - das Kühlen des für das erste Trennmittel vorgesehenen Gemisches, gegebenenfalls das Kühlen des für die Methanwaschkolonne vorgesehenen Methans, und
    - gegebenenfalls das Unterkühlen der Methanwaschkolonne,
    dadurch gekennzeichnet, dass sie einen ersten Kreisverdichter (V1) umfasst, um das Kreislauf-Kohlenmonoxid auf einen mittleren Druck zu verdichten, und eine Leitung, um einen ersten Teil des Kreislauf-Kohlenmonoxids in den Sumpf der Entstickungskolonne (C4) zu leiten, und einen zweiten Verdichter (V2), um einen zweiten Teil des Kohlenmonoxids auf einen hohen Druck zu verdichten.
  15. Anlage nach Anspruch 14, die einen Kreisverdichter (V1, V2) und eine Turbine (T) umfasst, wobei das Kohlenmonoxid aus dem Kreislauf über den Kreisverdichter auf einen hohen Druck verdichtet, danach in der Turbine entspannt und in gasförmiger Form in den Sumpf der CO/CH4-Trennkolonne (C3) geleitet wird.
  16. Anlage nach Anspruch 14 oder 15, die einen Kreisverdichter (V1, V2) und eine Turbine (T) umfasst, wobei Kohlenmonoxid aus dem Kreislauf über den Kreisverdichter auf einen hohen Druck verdichtet, danach in der Turbine entspannt und in gasförmiger Form in den Sumpf der Entstickungskolonne geleitet wird.
  17. Anlage nach einem der Ansprüche 14 bis 16, die eine Leitung umfasst, um einen CO-Kreislaufstrom auf dem höchsten Druck des Kreislaufs zum Sumpfnachverdampfer der Strippkolonne (C2) und/oder zum Sumpfnachverdampfer der CO/CH4-Trennkolonne (C3) zu leiten.
  18. Anlage nach einem der Ansprüche 14 bis 17, die eine Turbine (T) zum Entspannen des CO-Kreislaufstroms auf dem höchsten Druck des Kreislaufs umfasst, deren Auslass an die Entstickungskolonne (C4) angeschlossen ist.
  19. Anlage nach einem der Ansprüche 14 bis 18, die eine Austauschleitung (17) und Mittel umfasst, um den CO-Kreislaufstrom zur Austauschleitung stromaufwärts der Entstickungskolonne (C4) zu leiten.
  20. Anlage nach einem der Ansprüche 14 bis 19, wobei das erste Trennmittel eine Methanwaschkolonne ist, und Mittel umfassend, um eine methanangereicherte Flüssigkeit aus der CO/CH4-Trennkolonne (C3) zur Waschkolonne (C1) zu leiten.
  21. Anlage nach Anspruch 20, wobei der Kohlenmonoxidkreislauf mit einem Tauscher zum Kühlen des für die Methanwaschkolonne (C1) vorgesehenen Methans verbunden ist.
  22. Anlage nach einem der Ansprüche 14 bis 19, wobei das erste Trennmittel ein Phasentrenner (C1) ist.
EP07871946.5A 2006-12-21 2007-12-14 Verfahren und vorrichtung zur trennung einer mischung aus kohlenmonoxid, methan, wasserstoff und stickstoff durch kryogene destillation Active EP2122282B1 (de)

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FR0655775A FR2910603B1 (fr) 2006-12-21 2006-12-21 Procede de separation d'un melange de monoxyde de carbone, de methane, d'hydrogene et eventuellement d'azote par distillation cryogenetique
FR0755103A FR2916264A1 (fr) 2006-12-21 2007-05-16 Procede de separation d'un melange de monoxyde de carbone, de methane, d'hydrogene et eventuellement d'azote par distillation cryogenique
PCT/FR2007/052530 WO2008087318A2 (fr) 2006-12-21 2007-12-14 Procédé de séparation d'un mélange de monoxyde de carbone, de méthane, d'hydrogène et éventuellement d'azote par distillation cryogénique

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WO2008087318A3 (fr) 2009-11-26
FR2916264A1 (fr) 2008-11-21
ES2683145T3 (es) 2018-09-25
WO2008087318A2 (fr) 2008-07-24
CN101680713B (zh) 2013-08-14
CN101680713A (zh) 2010-03-24
US8959952B2 (en) 2015-02-24
US20100043489A1 (en) 2010-02-25
PL2122282T3 (pl) 2018-12-31

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