DE102010044646A1 - Process for separating nitrogen and hydrogen from natural gas - Google Patents

Process for separating nitrogen and hydrogen from natural gas Download PDF

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DE102010044646A1
DE102010044646A1 DE102010044646A DE102010044646A DE102010044646A1 DE 102010044646 A1 DE102010044646 A1 DE 102010044646A1 DE 102010044646 A DE102010044646 A DE 102010044646A DE 102010044646 A DE102010044646 A DE 102010044646A DE 102010044646 A1 DE102010044646 A1 DE 102010044646A1
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fraction
refrigerant
feed fraction
nitrogen
feed
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Dr. Schmidt Hans
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Linde GmbH
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Linde GmbH
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Priority to CN201110294067.7A priority patent/CN102564060B/en
Priority to US13/225,833 priority patent/US20120060554A1/en
Priority to AU2011221366A priority patent/AU2011221366B2/en
Publication of DE102010044646A1 publication Critical patent/DE102010044646A1/en
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10—Working-up natural gas or synthetic natural gas
    • C10L3/101—Removal of contaminants
    • C10L3/105—Removal of contaminants 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/0002—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the fluid to be liquefied
    • F25J1/0022—Hydrocarbons, e.g. natural 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0032—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration"
    • F25J1/004—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using the feed stream itself or separated fractions from it, i.e. "internal refrigeration" by flash gas recovery
    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/003—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production
    • F25J1/0047—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle
    • F25J1/0052—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures characterised by the kind of cold generation within the liquefaction unit for compensating heat leaks and liquid production using an "external" refrigerant stream in a closed vapor compression cycle by vaporising a liquid refrigerant stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
    • F25J1/00—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures
    • F25J1/02—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process
    • F25J1/0211—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle
    • F25J1/0212—Processes or apparatus for liquefying or solidifying gases or gaseous mixtures requiring the use of refrigeration, e.g. of helium or hydrogen ; Details and kind of the refrigeration system used; Integration with other units or processes; Controlling aspects of the process using a multi-component refrigerant [MCR] fluid in a closed vapor compression cycle as a single flow MCR cycle
    • 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
    • F25J3/0209—Natural gas or substitute natural 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/74—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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/06—Splitting of the feed stream, e.g. for treating or cooling in different ways
    • 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
    • F25J2215/04—Recovery of liquid products
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/60—Separating impurities from natural gas, e.g. mercury, cyclic hydrocarbons
    • F25J2220/64—Separating heavy hydrocarbons, e.g. NGL, LPG, C4+ hydrocarbons or heavy condensates in general
    • 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
    • F25J2245/90—Processes or apparatus involving steps for recycling of process streams the recycled stream being boil-off gas from storage
    • 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
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    • F25J2270/00—Refrigeration techniques used
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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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/66—Closed external refrigeration cycle with multi component refrigerant [MCR], e.g. mixture of hydrocarbons

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Abstract

Es wird ein Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten, insbesondere Wasserstoff, Kohlenmonoxid, Neon und Argon, aus einer zu Wasserstoff enthaltenden Einsatzfraktion, beschrieben, wobei die Abkühlung und Verflüssigung der Einsatzfraktion gegen das Kältemittel oder Kältemittelgemisch wenigstens eines Kältekreislaufes erfolgt. Erfindungsgemäß wird a) die Einsatzfraktion (1) partiell kondensiert (E1), b) in wenigstens einer Rektifizierkolonne (T) in eine Methan-reiche Fraktion (6) und eine Stickstoff und leichtere Komponenten enthaltende Fraktion (4) aufgetrennt, und c) die Methan-reiche Fraktion (6) unterkühlt, d) wobei die Kühlung des Kopfkondensators (E2) der Rektifizierkolonne (T) durch das Kältemittel oder Kältemittelgemisch oder einen Teilstrom des Kältemittels oder Kältemittelgemisches des oder wenigstens eines Kältekreislaufes (20–24) erfolgt.A process for the separation of nitrogen and lighter components, in particular hydrogen, carbon monoxide, neon and argon, from a feed fraction containing hydrogen is described, the cooling and liquefaction of the feed fraction taking place against the refrigerant or mixture of refrigerants of at least one refrigeration cycle. According to the invention, a) the feed fraction (1) is partially condensed (E1), b) in at least one rectification column (T) into a methane-rich fraction (6) and a fraction (4) containing nitrogen and lighter components, and c) the Methane-rich fraction (6) subcooled, d) wherein the cooling of the top condenser (E2) of the rectification column (T) is carried out by the refrigerant or refrigerant mixture or a partial flow of the refrigerant or refrigerant mixture of the or at least one refrigeration cycle (20-24).

Description

Die Erfindung betrifft ein Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten, insbesondere Wasserstoff, Kohlenmonoxid, Neon und Argon, aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion, wobei die Abkühlung und Verflüssigung der Einsatzfraktion gegen das Kältemittel oder Kältemittelgemisch wenigstens eines Kältekreislaufes erfolgt.The invention relates to a process for the separation of nitrogen and lighter components, in particular hydrogen, carbon monoxide, neon and argon, from a feed fraction to be liquefied, containing at least methane, nitrogen and hydrogen, wherein the cooling and liquefaction of the feed fraction against the refrigerant or refrigerant mixture at least one Refrigeration cycle takes place.

Für die Gewinnung von verflüssigtem Methan (LNG) werden in der jüngeren Vergangenheit neue ”Erdgasquellen” genutzt. Diese neuen Erdgasquellen stellen beispielsweise die Kohlevergasung oder Methanisierung dar. Die aus diesen Prozessen abgezogenen Gasgemische weisen neben der Hauptkomponente Methan Wasserstoff-Gehalte bis über 20 Vol-% sowie Stickstoff-Gehalte von mehr als 10 Vol-% auf. Darüber hinaus können diese Gasgemische Spuren von Kohlenmonoxid, Kohlendioxid, Neon und Argon enthalten. Neben dem Stickstoff muss auch der Wasserstoff aus dem zu verflüssigenden Methan abgetrennt werden, um die geforderten Spezifikationen für das LNG-Produkt einhalten zu können. Problematisch ist, dass der Wasserstoff zwar vergleichsweise tief siedet, jedoch im verflüssigten Methan sehr gut löslich ist.The extraction of liquefied methane (LNG) has recently exploited new sources of natural gas. These new natural gas sources represent, for example, coal gasification or methanation. The gas mixtures withdrawn from these processes have, in addition to the main component methane, hydrogen contents of more than 20% by volume and nitrogen contents of more than 10% by volume. In addition, these gas mixtures may contain traces of carbon monoxide, carbon dioxide, neon and argon. In addition to the nitrogen, the hydrogen must be separated from the methane to be liquefied in order to meet the required specifications for the LNG product. The problem is that although the hydrogen boils comparatively low, it is very soluble in liquefied methane.

Sofern das LNG-Produkt, wie dies üblicherweise der Fall ist, zwischengelagert wird, darf der Stickstoff-Gehalt einen Wert von 1 Vol-% nicht übersteigen, da es ansonsten im LNG-Speicherbehälter zu einem unerwünschten Roll-Over-Effekt kommen kann.If the LNG product is stored temporarily, as is usually the case, the nitrogen content must not exceed a value of 1% by volume, otherwise an undesirable roll-over effect may occur in the LNG storage tank.

Aufgabe der vorliegenden Erfindung ist es, ein gattungsgemäßes Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion anzugeben, das zum einen eine ausreichende Abtrennung des Stickstoffs ermöglicht und zum anderen die gleichzeitige Abtrennung von Wasserstoff, vorzugsweise bei einem vergleichsweise hohen Druck, ermöglicht.Object of the present invention is to provide a generic method for the separation of nitrogen and lighter components from a to be liquefied, at least methane, nitrogen and hydrogen containing feed fraction, which allows for a sufficient separation of the nitrogen and on the other hand, the simultaneous separation of hydrogen, preferably at a comparatively high pressure.

Zur Lösung dieser Aufgabe wird ein Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion vorgeschlagen, das dadurch gekennzeichnet ist, dass

  • a) die Einsatzfraktion partiell kondensiert wird,
  • b) in wenigstens einer Rektifizierkolonne in eine Methan-reiche Fraktion und eine Stickstoff und leichtere Komponenten enthaltende Fraktion aufgetrennt wird, und
  • c) die Methan-reiche Fraktion unterkühlt wird,
  • d) wobei die Kühlung des Kopfkondensators der Rektifizierkolonne durch das Kältemittel oder Kältemittelgemisch oder einen Teilstrom des Kältemittels oder Kältemittelgemisches des oder wenigstens eines Kältekreislaufes erfolgt.
To solve this problem, a method for the separation of nitrogen and lighter components from a to be liquefied, at least methane, nitrogen and hydrogen containing feed fraction is proposed, which is characterized in that
  • a) the feed fraction is partially condensed,
  • b) in at least one rectification column is separated into a methane-rich fraction and a fraction containing nitrogen and lighter components, and
  • c) the methane-rich fraction is undercooled,
  • d) wherein the cooling of the top condenser of the rectification carried by the refrigerant or refrigerant mixture or a partial flow of the refrigerant or refrigerant mixture of the or at least one refrigeration cycle.

Erfindungsgemäß werden nunmehr der in der Einsatzfraktion enthaltene Stickstoff sowie die ebenfalls enthaltenen leichteren Komponenten gemeinsam in einer Rektifizierkolonne aus der Einsatzfraktion abgetrennt. Da die Einsatzfraktion vor ihrer Verflüssigung üblicherweise auf einen Druck zwischen 40 und 90 bar verdichtet und vor ihrer Zuführung in die Rektifizierkolonne auf einen Druck zwischen 20 und 40 bar gedrosselt wird, können die abgetrennten Komponenten bei einem vergleichsweise hohen Druck gewonnen werden. Insbesondere im Falle der vergleichsweise wertvollen Komponente Wasserstoff ist eine Gewinnung bei hohem Druck erwünscht, da der Wasserstoff im Regelfall einer weiteren Verwendung zugeführt wird. Von Vorteil bei der erfindungsgemäßen Verfahrensweise ist ferner, dass durch die Integration der Abtrennung von leichteren Komponenten in den Stickstoff-Abtrennprozess die Investitionskosten, die ansonsten für eine separate Abtrennung der leichteren Komponenten erforderlich wären, eingespart werden können.According to the invention, the nitrogen present in the feed fraction and also the lighter components likewise present are separated off from the feed fraction together in a rectification column. Since the feed fraction before its liquefaction is usually compressed to a pressure between 40 and 90 bar and throttled before being fed into the rectification to a pressure between 20 and 40 bar, the separated components can be obtained at a relatively high pressure. Particularly in the case of the comparatively valuable component hydrogen, recovery at high pressure is desirable, since the hydrogen is generally supplied to a further use. An advantage of the method according to the invention is further that the integration costs of the separation of lighter components in the nitrogen removal process, the investment costs that would otherwise be required for a separate separation of the lighter components, can be saved.

Weitere vorteilhafte Ausgestaltungen des erfindungsgemäßen Verfahrens zur Abtrennung von Stickstoff und leichteren Komponenten aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion sind dadurch gekennzeichnet, dass

  • – die Einsatzfraktion einen Methan-Gehalt zwischen 50 und 90 Vol-%, einen Stickstoff-Gehalt zwischen 1 und 30 Vol-% und einen Wasserstoff-Gehalt zwischen 1 und 30 Vol-% aufweist,
  • – die Stickstoff und leichtere Komponenten enthaltende. Fraktion gegen die abzukühlende Einsatzfraktion angewärmt wird, wobei diese Abkühlung vor und/oder nach einer ggf. vorzusehenden Trocknung der Einsatzfraktion erfolgt,
  • – die Kondensatortemperatur des Kopfkondensators der Rektifizierkolonne variiert werden kann,
  • – sofern die verflüssigte Methan-reiche Fraktion zwischengespeichert wird, bei der Zwischenspeicherung anfallendes Tankrückgas verdichtet und der zu verflüssigenden Einsatzfraktion zugeführt wird,
  • – ein Teilstrom der zu verflüssigenden Einsatzfraktion der Rektifizierkolonne als Strippgasstrom im Sumpf der Rektifizierkolonne und/oder im Aufkocher der Rektifizierkolonne gekühlt und der Rektifizierkolonne als weiterer Einsatzstrom zugeführt wird, und
  • – sofern die Abkühlung und Verflüssigung der Einsatzfraktion gegen Kältemittel und/oder Kältemittelgemische wenigstens zweier Kältekreisläufe erfolgt, die Kühlung des Kopfkondensators der Rektifizierkolonne mittels eines separaten Kältekreislaufes oder durch zumindest einen Teilstrom des Kältemittels oder Kältemittelgemisches des leichtesten Kältekreislaufes erfolgt, wobei diese vorteilhafte Ausgestaltung des erfindungsgemäßen Verfahrens insbesondere für LNG-Anlagen mit größerer Kapazität geeignet ist.
Further advantageous embodiments of the method according to the invention for the separation of nitrogen and lighter components from a feed fraction to be liquefied, containing at least methane, nitrogen and hydrogen are characterized in that
  • The feed fraction has a methane content of between 50 and 90% by volume, a nitrogen content of between 1 and 30% by volume and a hydrogen content of between 1 and 30% by volume,
  • - containing the nitrogen and lighter components. Fraction is heated against the feed fraction to be cooled, this cooling taking place before and / or after any drying of the feed fraction to be provided,
  • The condenser temperature of the top condenser of the rectification column can be varied,
  • - if the liquefied methane-rich fraction is intermediately stored, accumulated in the intermediate storage tank return gas is compressed and fed to the liquefied feed fraction,
  • A partial stream of the feed fraction of the rectification column to be liquefied is cooled as stripping gas stream in the bottom of the rectification column and / or in the reboiler of the rectification column and fed to the rectification column as a further feed stream, and
  • - If the cooling and liquefaction of the feed fraction against refrigerant and / or refrigerant mixtures of at least two refrigeration circuits, the cooling of the top condenser of the Rectification carried out by means of a separate refrigeration cycle or by at least a partial flow of the refrigerant or refrigerant mixture of the lightest refrigeration cycle, this advantageous embodiment of the method according to the invention is particularly suitable for LNG plants with larger capacity.

Das erfindungsgemäße Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion sowie weitere vorteilhafte Ausgestaltungen desselben seien nachfolgend anhand des in der Figur dargestellten Ausführungsbeispieles näher erläutert.The inventive method for the separation of nitrogen and lighter components from a to be liquefied, at least methane, nitrogen and hydrogen-containing feed fraction and further advantageous embodiments thereof will be explained in more detail with reference to the embodiment shown in the figure.

Über Leitung 1 wird die wenigstens Methan, Stickstoff und Wasserstoff enthaltende Einsatzfraktion einer ggf. vorzusehenden Vorreinigungs-Einheit R zugeführt. Diese umfasst bei niedrigen Drückender Einsatzfraktion eine Verdichtung auf einen Druck zwischen 40 und 90 bar sowie im Regelfall eine Kohlendioxid- und Quecksilber-Entfernung sowie Trocknung. Die derart vorbehandelte Einsatzfraktion wird anschließend über Leitung 2 dem Wärmetauscher E1 zugeführt und in diesem abgekühlt und partiell kondensiert. Der Wärmetauscher E1 ist üblicherweise als Plattenwärmetauscher oder als gewickelter Wärmetauscher ausgeführt. Bei entsprechend großen Kapazitäten werden ggf. mehrere, parallel zueinander und/oder hintereinander angeordnete Wärmetauscher vorgesehen.Via wire 1 the feed fraction containing at least methane, nitrogen and hydrogen is fed to a pre-cleaning unit R which may have to be provided. This comprises at low pressures of the feed fraction compression to a pressure between 40 and 90 bar and usually a carbon dioxide and mercury removal and drying. The feed fraction pretreated in this way is subsequently passed via line 2 fed to the heat exchanger E1 and cooled in this and partially condensed. The heat exchanger E1 is usually designed as a plate heat exchanger or as a wound heat exchanger. With correspondingly large capacities, a plurality of heat exchangers arranged parallel to one another and / or one behind the other are possibly provided.

Die Abkühlung und Verflüssigung der Einsatzfraktion erfolgt gegen wenigstens einen, beliebig ausgeführten Kältekreislauf, der in der Figur lediglich schematisch durch die Leitungsabschnitte 20 bis 24, auf die im Folgenden noch näher eingegangen werden wird, dargestellt ist. Dieser Kältekreislauf ist vorzugsweise als Expander- oder Gemischkreislauf ausgebildet.The cooling and liquefaction of the feed fraction takes place against at least one, arbitrarily executed refrigeration cycle, in the figure only schematically through the line sections 20 to 24 , which will be discussed in more detail below, is shown. This refrigeration cycle is preferably designed as expander or mixture cycle.

Die partiell kondensierte Einsatzfraktion wird über Leitung 3, in der ein Entspannungsventil a vorgesehen sein kann, der Rektifizierkolonne T zugeführt und in dieser in eine Flüssig- und eine Gasfraktion aufgetrennt. Am Kopf der Rektifizierkolonne T wird über Leitung 4 eine Stickstoff sowie die leichteren Komponenten, insbesondere Wasserstoff enthaltende Fraktion abgezogen. Diese wird im Wärmetauscher E1 gegen die abzukühlende Einsatzfraktion angewärmt und anschließend über Leitung 5 an der Anlagengrenze abgegeben. Alternativ oder ergänzend hierzu kann die über Leitung 4 abgezogene Fraktion auch für die Vorkühlung der Einsatzfraktion 1 vor deren Trocknung in R herangezogen werden, um den Wassergehalt der Einsatzfraktion 1 vor der Trocknung in R zu reduzieren.The partially condensed feed fraction is via line 3 in which an expansion valve a can be provided, the rectification column T is supplied and separated in this into a liquid and a gas fraction. At the top of the rectification column T is via line 4 a nitrogen and the lighter components, in particular hydrogen-containing fraction deducted. This is warmed in the heat exchanger E1 against the feed fraction to be cooled and then via line 5 delivered at the plant boundary. Alternatively or additionally, the over line 4 withdrawn fraction also for the pre-cooling of the feed fraction 1 before being dried in R, the water content of the feed fraction 1 to reduce in R before drying.

Sofern die zu verflüssigende Einsatzfraktion 1 schwere Kohlenwasserstoffe enthält, ist vorzugsweise vor der Rektifizierungskolonne T eine Abtrennung dieser schweren Kohlenwasserstoffe zu realisieren. Diese Abtrennung kann in einem SKW-Abscheider, einem Deethanizer, einem Depropanizer, etc. erfolgen.As far as the feed fraction to be liquefied 1 contains heavy hydrocarbons, is preferably before the rectification column T to realize a separation of these heavy hydrocarbons. This separation can take place in a SKW separator, a deethanizer, a depropanizer, etc.

Aus dem Sumpf der Rektifizierkolonne T wird über Leitung 6 eine Methan-reiche Flüssigfraktion mit einem Stickstoff-Gehalt von typischerweise weniger als 3 Vol-% abgezogen und im Wärmetauscher E1 gegen das Kältemittel oder Kältemittelgemisch 23 des Kältekreislaufes unterkühlt. Über Leitung 7 wird das derart gewonnene LNG-Produkt nach Entspannung im Ventil b einem Speicherbehälter S zugeführt.From the bottom of the rectification T is via line 6 withdrawn a methane-rich liquid fraction having a nitrogen content of typically less than 3% by volume and in the heat exchanger E1 against the refrigerant or refrigerant mixture 23 the cooling circuit is undercooled. Via wire 7 the LNG product thus obtained is supplied to a storage tank S after relaxation in the valve b.

Innerhalb des Speicherbehälters S anfallendes Tankrückgas wird über die Leitung 8 aus dem Speicherbehälter S abgezogen, sofern erforderlich im Verdichter V ein- oder mehrstufig verdichtet und der Einsatzfraktion 1, vorzugsweise vor ihrer Abkühlung zugeführt. Alternativ kann das Tankrückgas auch einem Brenngassystem zugeführt oder an der Anlagengrenze abgegeben werden.Within the storage tank S accumulating tank return gas is via the line 8th withdrawn from the storage tank S, if necessary in the compressor V one or more stages compressed and the feed fraction 1 , preferably fed before its cooling. Alternatively, the tank return gas can also be supplied to a fuel gas system or discharged at the plant boundary.

Die Kühlung des Kopfkondensators E2 der Rektifizierkolonne T erfolgt erfindungsgemäß durch ein Kältemittel oder Kältemittelgemisch oder einen Teilstrom des Kältemittels bzw. Kältemittelgemisches. Bei der in der Figur dargestellten Ausführungsform wird ein Teil des Kältemittel(gemisch)stroms über Leitung 22 dem Kopfkondensator E2 zugeführt und nach Durchgang durch diesen über Leitung 23 durch den Wärmetauscher E1 geführt. Das in ihm gegen die abzukühlende Einsatzfraktion angewärmte Kältemittel(gemisch) wird anschließend über Leitung 24 aus dem Wärmetauscher E1 abgezogen. Der nicht dem Kopfkondensator E2 zugeführte Teilstrom des Kältemittels bzw. Kältemittelgemisches wird über Leitung 21, in der ein Regelventil d vorgesehen ist, geführt.The cooling of the top condenser E2 of the rectification T according to the invention is carried out by a refrigerant or refrigerant mixture or a partial flow of the refrigerant or refrigerant mixture. In the embodiment shown in the figure, a part of the refrigerant (mixture) flow is via line 22 fed to the top condenser E2 and after passing through this line 23 passed through the heat exchanger E1. The warmed in him against the cooled feed fraction refrigerant (mixture) is then via line 24 withdrawn from the heat exchanger E1. The non-top condenser E2 supplied partial flow of the refrigerant or refrigerant mixture is via line 21 in which a control valve d is provided guided.

Der Kopfkondensator E2 kann entweder als Plattentauscher, gewickelter Wärmetauscher oder TEMA-Tauscher ausgebildet und in oder oberhalb der Rektifizierkolonne T angeordnet sein, wobei eine Anordnung oberhalb der Rektifizierkolonne T eine Rücklaufpumpe obsolet macht. Durch Variation der Kolonnenhöhe und der Kondensatortemperatur kann der Methan-Gehalt in der über Leitung 4 abgezogenen Fraktion nahezu beliebig, nämlich zwischen ca. 10 ppm bis einige Vol-%, eingestellt werden.The top condenser E2 may be formed either as a plate exchanger, coiled heat exchanger or TEMA exchanger and be arranged in or above the rectification column T, wherein an arrangement above the rectification T makes a return pump obsolete. By varying the column height and the condenser temperature, the methane content in the over line 4 withdrawn fraction almost arbitrarily, namely between about 10 ppm to a few vol%, can be adjusted.

In vorteilhafter Weise wird über Leitung 9 ein Teilstrom der zu verflüssigenden Einsatzfraktion durch den Aufkocher E3 der Rektifizierkolonne T, durch den der Stickstoff-Gehalt des im Speicherbehälter S gelagerten LNG-Produkts unter 1 Vol-% gehalten werden kann, geführt, anschließend im Ventil c entspannt und über Leitung 9' der Rektifizierkolonne T als zusätzlicher Einsatzstrom zugeführt. Alternativ dazu kann auch ein Teilstrom der zu verflüssigenden Einsatzfraktion vor oder nach erfolgter Abkühlung im Wärmetauscher E1 als Strippgasstrom im Sumpf der Rektifizierkolonne T eingesetzt oder ein Teilstrom des Kältemittel(gemische)s als Wärmequelle für den Aufkocher E3 verwendet werden.Advantageously, via line 9 a partial stream of the feed fraction to be liquefied by the reboiler E3 of the rectification T, by which the nitrogen content of the stored in the storage tank S LNG product can be kept below 1% by volume, then discharged in the valve c and relaxed via line 9 ' the rectification column T supplied as an additional feed stream. Alternatively, a partial stream of the feed fraction to be liquefied before or after cooling in the heat exchanger E1 used as Strippgasstrom in the bottom of the rectification T or a partial flow of the refrigerant (mixtures) s used as a heat source for the reboiler E3.

Das erfindungsgemäße Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion ist in vorteilhafter Weise bei Stickstoff- und Wasserstoff-Gehalten bis jeweils 30 Vol-% einsetzbar. Dabei wirken sich auch vergleichsweise hohe Wasserstoff-Gehalte in der zu verflüssigenden Einsatzfraktion nur untergeordnet auf den Gesamtenergiebedarf des erfindungsgemäßen Verfahrens aus, da ein Teil der Kälte durch die Anwärmung der aus dem Kopf der Rektifizierkolonne T abgezogenen, Stickstoff sowie die leichteren Komponenten, insbesondere Wasserstoff enthaltenden Fraktion zurückgewonnen wird.The inventive method for the separation of nitrogen and lighter components from a to be liquefied, at least methane, nitrogen and hydrogen-containing feed fraction is advantageously used at nitrogen and hydrogen contents up to 30 vol%. In this case, comparatively high hydrogen contents in the feed fraction to be liquefied also have a subordinate effect on the total energy requirement of the process according to the invention, since part of the cold is due to the heating of the nitrogen withdrawn from the top of the rectification column T and the lighter components, in particular hydrogen Group is recovered.

Claims (7)

Verfahren zur Abtrennung von Stickstoff und leichteren Komponenten, insbesondere Wasserstoff, Kohlenmonoxid, Neon und Argon, aus einer zu verflüssigenden, wenigstens Methan, Stickstoff und Wasserstoff enthaltenden Einsatzfraktion, wobei die Abkühlung und Verflüssigung der Einsatzfraktion gegen das Kältemittel oder Kältemittelgemisch wenigstens eines Kältekreislaufes erfolgt, dadurch gekennzeichnet, dass a) die Einsatzfraktion (1) partiell kondensiert wird (E1), b) in wenigstens einer Rektifizierkolonne (T) in eine Methan-reiche Fraktion (6) und eine Stickstoff und leichtere Komponenten enthaltende Fraktion (4) aufgetrennt wird, und c) die Methan-reiche Fraktion (6) unterkühlt wird, d) wobei die Kühlung des Kopfkondensators (E2) der Rektifizierkolonne (T) durch das Kältemittel oder Kältemittelgemisch oder einen Teilstrom des Kältemittels oder Kältemittelgemisches des oder wenigstens eines Kältekreislaufes (20–24) erfolgt.A process for the separation of nitrogen and lighter components, in particular hydrogen, carbon monoxide, neon and argon, from a feed fraction to be liquefied, containing at least methane, nitrogen and hydrogen, wherein the cooling and liquefaction of the feed fraction against the refrigerant or refrigerant mixture of at least one refrigeration cycle, characterized characterized in that a) the feed fraction ( 1 ) is partially condensed (E1), b) in at least one rectification column (T) in a methane-rich fraction ( 6 ) and a fraction containing nitrogen and lighter components ( 4 ) and c) the methane-rich fraction ( 6 ), wherein the cooling of the top condenser (E2) of the rectification column (T) by the refrigerant or refrigerant mixture or a partial flow of the refrigerant or refrigerant mixture of the or at least one refrigeration cycle ( 20 - 24 ) he follows. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass die Einsatzfraktion (1) einen Methan-Gehalt zwischen 50 und 90 Vol-%, einen Stickstoff-Gehalt zwischen 1 und 30 Vol-% und einen Wasserstoff-Gehalt zwischen 1 und 30 Vol-% aufweist.Process according to claim 1, characterized in that the feed fraction ( 1 ) has a methane content between 50 and 90% by volume, a nitrogen content between 1 and 30% by volume and a hydrogen content between 1 and 30% by volume. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, dass die Stickstoff und leichtere Komponenten enthaltende Fraktion (4) gegen die abzukühlende Einsatzfraktion (1, 2) angewärmt wird (E1), wobei die Abkühlung der Einsatzfraktion (1) vor und/oder nach einer ggf. vorzusehenden Trocknung (R) der Einsatzfraktion (1) erfolgt.A method according to claim 1 or 2, characterized in that the fraction containing nitrogen and lighter components ( 4 ) against the feed fraction to be cooled ( 1 . 2 ) is warmed (E1), wherein the cooling of the feed fraction (E1) 1 ) before and / or after any drying (R) of the feed fraction ( 1 ) he follows. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die Kondensatortemperatur des Kopfkondensators (E2) der. Rektifizierkolonne (T) variiert werden kann.Method according to one of the preceding claims 1 to 3, characterized in that the condenser temperature of the top condenser (E2) of the. Rectification column (T) can be varied. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 4, wobei die verflüssigte Methan-reiche Fraktion zwischengespeichert wird, dadurch gekennzeichnet, dass bei der Zwischenspeicherung (S) anfallendes Tankrückgas (8) verdichtet (V) und der zu verflüssigenden Einsatzfraktion (1) zugeführt wird.Method according to one of the preceding claims 1 to 4, wherein the liquefied methane-rich fraction is intermediately stored, characterized in that in the intermediate storage (S) accumulating tank back gas ( 8th ) (V) and the feed fraction to be liquefied ( 1 ) is supplied. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 5, dadurch gekennzeichnet, dass ein Teilstrom der zu verflüssigenden Einsatzfraktion (1) der Rektifizierkolonne (T) als Strippgasstrom im Sumpf der Rektifizierkolonne (T) und/oder im Aufkocher (E3) der Rektifizierkolonne (T) gekühlt und der Rektifizierkolonne (T) als weiterer Einsatzstrom zugeführt wird.Method according to one of the preceding claims 1 to 5, characterized in that a partial stream of the feed fraction to be liquefied ( 1 ) of the rectification column (T) is cooled as a stripping gas stream in the bottom of the rectification column (T) and / or in the reboiler (E3) of the rectification (T) and the rectification (T) is fed as a further feed stream. Verfahren nach einem der vorhergehenden Ansprüche 1 bis 6, wobei die Abkühlung und Verflüssigung der Einsatzfraktion gegen Kältemittel und/oder Kältemittelgemische wenigstens zweier Kältekreisläufe erfolgt, dadurch gekennzeichnet, dass die Kühlung des Kopfkondensators (E2) der Rektifizierkolonne (T) mittels eines separaten Kältekreislaufes oder durch zumindest einen Teilstrom des Kältemittels oder Kältemittelgemisches des leichtesten Kältekreislaufes erfolgt.Method according to one of the preceding claims 1 to 6, wherein the cooling and liquefaction of the feed fraction against the refrigerant and / or refrigerant mixtures of at least two refrigeration cycles, characterized in that the cooling of the top condenser (E2) of the rectification (T) by means of a separate refrigeration cycle or by at least a partial flow of the refrigerant or refrigerant mixture of the lightest refrigeration cycle takes place.
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