DE3639779A1 - Process for extracting CO2 from a CO2-rich natural gas - Google Patents

Process for extracting CO2 from a CO2-rich natural gas

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Publication number
DE3639779A1
DE3639779A1 DE19863639779 DE3639779A DE3639779A1 DE 3639779 A1 DE3639779 A1 DE 3639779A1 DE 19863639779 DE19863639779 DE 19863639779 DE 3639779 A DE3639779 A DE 3639779A DE 3639779 A1 DE3639779 A1 DE 3639779A1
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Germany
Prior art keywords
natural gas
gas
rectification column
sump
liquid
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DE19863639779
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German (de)
Inventor
Rainer Dipl Ing Sapper
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Linde GmbH
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Linde GmbH
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Priority to DE19863639779 priority Critical patent/DE3639779A1/en
Publication of DE3639779A1 publication Critical patent/DE3639779A1/en
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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
    • F25J3/0266—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 dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/50—Carbon dioxide
    • 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
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the 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
    • 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
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • F25J2205/66—Regenerating the adsorption vessel, e.g. kind of reactivation 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
    • F25J2215/04—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
    • F25J2220/80—Separating impurities from carbon dioxide, e.g. H2O or water-soluble contaminants
    • F25J2220/82—Separating low boiling, i.e. more volatile components, e.g. He, H2, CO, Air gases, CH4
    • 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
    • F25J2270/06—Internal refrigeration with work-producing gas expansion loop with multiple gas expansion loops
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/12—External refrigeration with liquid vaporising loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-hydrocarbons
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A process is described for extracting CO2 from a CO2-rich natural gas, in which the CO2 content is, for example, between 60 and 80%. After cooling and partial condensation, a CO2-rich condensate is introduced into a rectifying column, in which the lighter companion substances are separated off and taken off overhead. In the bottom of the rectifying column, purified CO2 is extracted as the product. Cooling of the natural gas is first carried out against components separated off to be reheated and then with heating of the bottom product of the rectifying column. The liquid CO2 taken off from the bottom is supercooled in an intermediate heater for the rectifying column and then delivered as a liquid product stream.

Description

Die Erfindung betrifft ein Verfahren zur Gewinnung von CO2 aus einem CO2-reichen Erdgas, bei dem nach Abkühlung und partieller Kondensation des unter erhöhtem Druck stehenden Erdgases ein CO2-reiches Kondensat in eine Rektifiziersäule gegeben wird, in der leichtere Begleitstoffe des CO2 abgetrennt und über Kopf abgezogen werden und in der gereinigtes CO2 aus dem Sumpf als Produktstrom gewonnen wird.The invention relates to a process for the production of CO 2 from a CO 2 -rich natural gas, in which, after cooling and partial condensation of the pressurized natural gas, a CO 2 -rich condensate is placed in a rectification column in which lighter accompanying substances of the CO 2 are separated off and taken off overhead and in which purified CO 2 is obtained from the bottom as a product stream.

Bei CO2-reichen Erdgasen, die beispielsweise 60 bis 80% CO2 enthalten können, ist oftmals das CO2 ein gewünschtes Produkt, das unter anderem für die tertiäre Erdölgewinnung oder für eine Verwendung in der Lebensmittelindustrie benötigt wird. In derartigen Erdgasen sind Stickstoff oder leichte Kohlenwasserstoffe, insbesondere Methan, dagegen nur in so geringen Mengen enthalten, daß diese Komponenten oftmals für eine Produktgewinnung nicht interessant sind.When CO 2 -rich natural gases, which may contain, for example, 60 to 80% CO 2, the CO 2 is often a desired product, which is required, inter alia, for tertiary oil recovery or for use in the food industry. In contrast, such natural gases only contain nitrogen or light hydrocarbons, especially methane, in such small amounts that these components are often of no interest for product recovery.

Bei einem bekannten Verfahren zur Gewinnung von CO2 aus CO2-reichen Erdgasen wird das unter erhöhtem Druck stehende Erdgas nach einer Trocknung zunächst im Sumpf einer Rektifiziersäule abgekühlt und dann nach weiterer Kühlung gegen Fremdkälte partiell kondensiert. Die dabei anfallende CO2-reiche Flüssigkeit wird einer als Abtriebssäule betriebenen Rektifiziersäule aufgegeben, aus deren vom abzukühlenden Erdgas beheiztem Sumpf das reine CO2 in flüssiger Form abgezogen wird. Nicht kondensiertes Gas sowie das Kopfgas aus der Rektifiziersäule werden dabei als Restgas abgegeben.In a known process for the production of CO 2 from CO 2 -rich natural gases, the natural gas, which is under increased pressure, is first dried in the bottom of a rectification column after drying and then partially condensed against external cold after further cooling. The resulting CO 2 -rich liquid is fed to a rectification column operated as a stripping column, from the sump of which is heated by the natural gas to be cooled, the pure CO 2 is withdrawn in liquid form. Uncondensed gas and the top gas from the rectification column are released as residual gas.

Der Erfindung liegt die Aufgabe zugrunde, ein derartiges Verfahren zu verbessern, wobei der Energieverbrauch bei hoher Reinheit und Ausbeute des CO2 reduziert werden kann.The invention has for its object to improve such a method, wherein the energy consumption can be reduced with high purity and yield of CO 2 .

Diese Aufgabe wird dadurch gelöst, daß das Erdgas zunächst gegen wieder anzuwärmendes Gas und danach unter Beheizung des Sumpfes der Rektifiziersäule abgekühlt wird, daß das aus dem Sumpf abgezogene flüssige CO2 in einer oberhalb des Sumpfes gelegenen Zwischenkühlung für die Rektifiziersäule unterkühlt und danach als flüssiger Produktstrom abgegeben wird.This object is achieved in that the natural gas is first cooled against gas to be reheated and then with heating the sump of the rectification column, that the liquid CO 2 drawn off from the sump is subcooled in an intermediate cooling unit above the sump for the rectification column and then as a liquid product stream is delivered.

Beim bekannten Verfahren wird das getrocknete Erdgas, dessen Temperatur typischerweise zwischen 20 und 40°C liegt, direkt als Heizmedium für den Sumpf der Rektifiziersäule herangezogen. Bei typischen Rektifizierdrücken, d. h. bei Drücken zwischen etwa 20 und 45 bar, liegt die Sumpftemperatur im Bereich zwischen etwa -20 bis +10°C, so daß sich relativ große Temperaturdifferenzen zwischen dem Heizmedium und der Sumpftemperatur ergeben. Erfindungsgemäß wird die thermodynamisch ungünstige große Temperaturdifferenz verringert, indem das Erdgas zunächst gegen wieder anzuwärmendes Restgas vorgekühlt wird und erst danach zur Sumpfheizung herangezogen wird. Da durch die vorgeschaltete Abkühlung aber nicht mehr so viel Wärme durch das Erdgas in den Sumpf der Rektifiziersäule eingebracht wird, ist noch eine zusätzliche Heizung erforderlich. Dies wird erfindungsgemäß dadurch erreicht, daß das aus dem Sumpf abgezogene CO2-Produkt oberhalb der Sumpfheizung, d. h. an einer Stelle, an der die Temperatur in der Rektifiziersäule tiefer als im Sumpf ist, als Heizmedium für eine Zwischenheizung eingesetzt wird. Neben der Bereitstellung der zusätzlichen Heizenergie hat diese Verfahrensführung noch den Vorteil, daß das flüssige CO2 unterkühlt wird, bevor es als Produkt abgezogen wird. Vorteilhaft ist dies insbesondere, weil das CO2 meist unter niedrigerem Druck als dem Druck der Rektifiziersäule benötigt wird, denn bei der nötigen Entspannung fällt dadurch nur relativ wenig Entspannungsgas, aber ein größerer Anteil als gewünschtes flüssiges CO2-Produkt an. Typische Abgabedrucke für das flüssige CO2 liegen im Bereich zwischen etwa 1 und 20 bar, vorzugsweise zwischen 2 und 10 bar, beispielsweise bei etwa 5 bar.In the known method, the dried natural gas, the temperature of which is typically between 20 and 40 ° C., is used directly as a heating medium for the bottom of the rectification column. At typical rectification pressures, ie pressures between about 20 and 45 bar, the bottom temperature is in the range between about -20 to + 10 ° C, so that there are relatively large temperature differences between the heating medium and the bottom temperature. According to the invention, the thermodynamically unfavorable large temperature difference is reduced by first cooling the natural gas against residual gas to be reheated and only then using it for the sump heating. Since the upstream cooling does not bring as much heat through the natural gas into the sump of the rectification column, additional heating is required. This is achieved according to the invention in that the CO 2 product withdrawn from the sump is used as a heating medium for an intermediate heating above the sump heater, ie at a point at which the temperature in the rectification column is lower than in the sump. In addition to providing the additional heating energy, this procedure also has the advantage that the liquid CO 2 is subcooled before it is withdrawn as a product. This is particularly advantageous because the CO 2 is usually required at a lower pressure than the pressure of the rectification column, because when the pressure is released, only a relatively small amount of gas is released, but a larger proportion than the desired liquid CO 2 product. Typical discharge pressures for the liquid CO 2 are in the range between approximately 1 and 20 bar, preferably between 2 and 10 bar, for example approximately 5 bar.

In einer günstigen Weiterbildung der Erfindung wird das Erdgas, nachdem es als Heizmedium für den Sumpf der Rektifiziersäule gedient hat, im Wärmetausch mit anzuwärmendem Restgas weiter abgekühlt. Um die Temperaturdifferenz über die Rektifiziersäule zu überbrücken, kann dabei gegebenenfalls eine zusätzliche Kühlung durch Fremdkälte erfolgen. In einer bevorzugten Ausgestaltung der Erfindung wird zusätzliche Abkühlung dadurch bewirkt, daß das Restgas nach seinem Wärmetausch gegen das weiter abzukühlende Erdgas entspannt und danach erneut in Wärmetausch mit dem abzukühlenden Erdgas gebracht wird. Die Entspannung kann dabei gegebenenfalls arbeitsleistend, unter Umständen auch mehrstufig, erfolgen. Das derart angewärmte Restgas kann dann anschließend noch für die Vorkühlung des Erdgases, bevor es zur Sumpfheizung der Rektifiziersäule eingesetzt wird, verwendet werden. In a favorable development of the invention Natural gas after being used as a heating medium for the swamp of the Rectification column has served in the heat exchange with residual gas to be heated cooled further. To the Bridging the temperature difference across the rectification column, can optionally by additional cooling External cold take place. In a preferred embodiment of the Invention additional cooling is effected in that the Residual gas after its heat exchange with the one to be cooled Natural gas relaxes and then again in heat exchange with the natural gas to be cooled is brought. The relaxation can doing work, possibly under certain circumstances multi-stage. The residual gas heated in this way can then then for the pre-cooling of the natural gas before it is used for the sump heating of the rectification column, be used.  

In einer speziellen Ausgestaltung der Erfindung wird das Erdgas, das nach seiner Abkühlung partiell kondensiert ist, wobei im wesentlichen alle CO2-Bestandteile im Kondensat enthalten sind, in einen Abscheider eingespeist, in dem auch das vom Kopf der Rektifiziersäule abgezogene Gas geleitet wird. Die flüssige Phase wird dann in den oberen Bereich der Rektifiziersäule eingespeist, während die gasförmige Phase, die aus dem Kopfgas aus der Rektifiziersäule sowie aus den nicht kondensierten Anteilen des Erdgases besteht, als Restgas abgegeben wird.In a special embodiment of the invention, the natural gas, which is partially condensed after it has cooled, with essentially all of the CO 2 constituents being contained in the condensate, is fed into a separator in which the gas drawn off from the top of the rectification column is also passed. The liquid phase is then fed into the upper region of the rectification column, while the gaseous phase, which consists of the top gas from the rectification column and the uncondensed portions of the natural gas, is discharged as residual gas.

Weitere Einzelheiten der Erfindung werden nachfolgend anhand eines in der Figur schematisch dargestellten Ausführungsbeispiels erläutert.Further details of the invention are described below one shown schematically in the figure Exemplary embodiment explained.

Bei dem in der Figur dargestellten Ausführungsbeispiel wird über Leitung 1 ein Erdgas bei einen Druck von 40 bar und einer Temperatur von 30°C herangeführt, das 0,3% Helium, 22,6% Stickstoff, 71,5% CO2, 5,5% Methan und etwa 0,1% Wasserdampf enthält. Es wird zunächst über die Leitungen 2 bzw. 3 über einen der wechselweise in Adsorption und Regeneration betriebenen Adsorber 4 bzw. 5 geführt und gelangt danach über Leitung 6 zu einem Wärmetauscher 7, in dem eine erste Abkühlung des Erdgases gegen anzuwärmendes Restgas erfolgt. Anschließend gelangt das vorgekühlte Erdgas über Leitung 8 in einen Wärmetauscher 9, der im Sumpf der Rektifiziersäule 10 angeordnet ist. Nach Beheizung des Sumpfes gelangt das nunmehr auf eine Temperatur von etwa 0°C abgekühlte Erdgas über Leitung 11 zu einem weiteren Wärmetauscher 12, in dem es gegen anzuwärmendes Restgas sowie durch Leitung 13 angedeutete Fremdkälte, beispielsweise einen Propankreislauf, auf eine Temperatur von etwa -37°C abgekühlt wird. Das nunmehr partiell kondensierte Erdgas gelangt über Leitung 14 in einen Abscheider 15, aus dem die flüssige Phase über Leitung 16 auf den Kopf der Rektifiziersäule aufgegeben wird. In the embodiment shown in the figure, a natural gas is brought in via line 1 at a pressure of 40 bar and a temperature of 30 ° C., which contains 0.3% helium, 22.6% nitrogen, 71.5% CO 2 , 5, Contains 5% methane and about 0.1% water vapor. It is first led via lines 2 and 3 via one of the adsorbers 4 and 5 , which are operated alternately in adsorption and regeneration, and then passes via line 6 to a heat exchanger 7 , in which a first cooling of the natural gas takes place against residual gas to be heated. The pre-cooled natural gas then passes via line 8 into a heat exchanger 9 which is arranged in the bottom of the rectification column 10 . After the sump has been heated, the natural gas, which has now been cooled to a temperature of about 0 ° C., reaches another heat exchanger 12 via line 11 , in which it is heated to about -37 against residual gas to be heated and external cooling indicated by line 13 , for example a propane circuit ° C is cooled. The now partially condensed natural gas passes via line 14 into a separator 15 , from which the liquid phase is fed via line 16 to the top of the rectification column.

Im Sumpf der Rektifiziersäule 10 fällt flüssiges gereinigtes CO2 an, das über Leitung 17 abgezogen und einem Wärmetauscher 18 zugeführt wird. Der Wärmetauscher 18 ist als Zwischenheizung für die Rektifiziersäule 10 ausgebildet und oberhalb des Wärmetauschers 9 für die Sumpfheizung angeordnet. Das im Wärmetauscher 18 unterkühlte flüssige Kohlendioxid gelangt anschließend über Leitung 19 und ein Entspannungsventil 20, in dem es auf einen Druck von etwa 5 bar entspannt wird, in einen Produktabscheider 21. Aus dem Produktabscheider 21 wird über Leitung 22 flüssiges CO2 als Produkt abgezogen, während das bei der Entspannung im Ventil 20 gebildete Gas über Leitung 23 abgezogen wird. Das flüssige CO2 in Leitung 22 enthält neben 98,5% CO2 nur noch 1% Methan und 0,5% Stickstoff.In the bottom of the rectification column 10 , liquid purified CO 2 is obtained , which is drawn off via line 17 and fed to a heat exchanger 18 . The heat exchanger 18 is designed as an intermediate heater for the rectification column 10 and is arranged above the heat exchanger 9 for the sump heater. The liquid carbon dioxide, which is supercooled in the heat exchanger 18 , then reaches a product separator 21 via line 19 and an expansion valve 20 , in which it is expanded to a pressure of approximately 5 bar. Liquid CO 2 is withdrawn as product from the product separator 21 via line 22 , while the gas formed in the expansion in the valve 20 is withdrawn via line 23 . In addition to 98.5% CO 2, the liquid CO 2 in line 22 contains only 1% methane and 0.5% nitrogen.

In der Rektifiziersäule 10 fällt ein Kopfgas an, das über Leitung 24 abgezogen und in den Abscheider 15 eingespeist wird. Hier vermischt es sich mit dem über Leitung 14 herangeführten abgekühlten Erdgas. Es wird eine gemeinsame Gasphase aus dem Abscheider 15 über Leitung 25 abgezogen, die 35,5% CO2, 0,7% Helium, 52,8% Stickstoff und 11% Methan enthält. Nach einer ersten Anwärmung im Wärmetauscher 12 gegen abzukühlendes Erdgas wird diese unter einem Druck von 40 bar stehende Fraktion in einer Turbine 26 arbeitsleistend auf einen Zwischendruck entspannt. Die bei der Entspannung auftretende Abkühlung wird durch erneuten Wärmetausch gegen abzukühlendes Erdgas im Wärmetauscher 12 wieder ausgeglichen, danach erfolgt in einer weiteren Entspannungsturbine 27 eine weitere Entspannung auf den Abgabedruck des Restgases von etwa 5 bar. Das über Leitung 28 aus der Turbine 27 austretende kalte Gas wird zunächst wieder im Wärmetauscher 12 angewärmt und danach über Leitung 29 dem Wärmetauscher 7 zugeführt, in dem es weiter gegen aus den Trocknern 4 bzw. 5 kommendes Erdgas angewärmt wird. Ein Teil des Restgases wird über Leitung 30 abgezweigt, in einem Wärmetauscher 31 aufgeheizt und danach als Regeneriergas durch den gerade eine Regenerationsphase durchlaufenden Adsorber 5 bzw. 4 geleitet, bevor es über Leitung 32 abgezogen wird. Der Hauptteil des Restgases wird über Leitung 33 abgezogen.A head gas is obtained in the rectification column 10 , which is drawn off via line 24 and fed into the separator 15 . Here it mixes with the cooled natural gas supplied via line 14 . A common gas phase is withdrawn from the separator 15 via line 25 , which contains 35.5% CO 2 , 0.7% helium, 52.8% nitrogen and 11% methane. After a first heating in the heat exchanger 12 against natural gas to be cooled, this fraction, which is under a pressure of 40 bar, is expanded to an intermediate pressure in a turbine 26 while performing work. The cooling that occurs during the expansion is compensated for by renewed heat exchange against natural gas to be cooled in the heat exchanger 12 , after which a further expansion turbine 27 expands to the discharge pressure of the residual gas of approximately 5 bar. The cold gas emerging from the turbine 27 via line 28 is first heated again in the heat exchanger 12 and then fed via line 29 to the heat exchanger 7 , in which it is further heated against natural gas coming from the dryers 4 and 5 . A portion of the residual gas is branched off via line 30 , heated in a heat exchanger 31 and then passed as regeneration gas through the adsorber 5 or 4 which is currently undergoing a regeneration phase before it is drawn off via line 32 . The main part of the residual gas is withdrawn via line 33 .

Claims (7)

1. Verfahren zur Gewinnung von CO2 aus einem CO2-reichen Erdgas, bei dem nach Abkühlung und partieller Kondensation das unter erhöhtem Druck stehenden Erdgases ein CO2-reiches Kondensat in eine Rektifiziersäule gegeben wird, in der leichtere Begleitstoffe des CO2 abgetrennt und über Kopf abgezogen werden und in der gereinigtes CO2 aus dem Sumpf als Produktstrom gewonnen wird, dadurch gekennzeichnet, daß das Erdgas zunächst gegen wieder anzuwärmendes Gas und danach unter Beheizung des Sumpfes der Rektifiziersäule abgekühlt wird, daß das aus dem Sumpf abgezogene flüssige CO2 in einer oberhalb des Sumpfes gelegenen Zwischenheizung für die Rektifiziersäule unterkühlt und danach als flüssiger Produktstrom abgegeben wird.1. A process for the production of CO 2 from a CO 2 -rich natural gas, in which, after cooling and partial condensation, the natural gas under increased pressure, a CO 2 -rich condensate is placed in a rectification column, in which lighter accompanying substances of the CO 2 are separated and are withdrawn overhead and recovered in the purified CO 2 from the sump as a product stream, characterized in that the natural gas is first cooled against gas to be reheated and then with heating the sump of the rectification column, that the liquid CO 2 withdrawn from the sump in an intermediate heater for the rectification column located above the sump and then released as a liquid product stream. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die Rektifikation bei einem Druck zwischen 20 und 45 bar durchgeführt wird.2. The method according to claim 1, characterized in that rectification at a pressure between 20 and 45 bar is carried out. 3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das unterkühlte CO2 auf einen tieferen Druck entspannt wird.3. The method according to claim 1 or 2, characterized in that the supercooled CO 2 is expanded to a lower pressure. 4. Verfahren nach Anspruch 3, dadurch gekennzeichnet, daß das flüssige CO-Produkt auf einen Druck zwischen 1 und 20 bar, vorzugsweise zwischen 2 und 10 bar entspannt wird. 4. The method according to claim 3, characterized in that the liquid CO product at a pressure between 1 and 20 bar, preferably between 2 and 10 bar is relaxed.   5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß das Erdgas nach Wärmeabgabe zur Sumpfheizung der Rektifiziersäule im Wärmetausch mit anzuwärmendem Gas weiter abgekühlt wird.5. The method according to any one of claims 1 to 4, characterized characterized in that the natural gas after heat emission for Sump heating of the rectification column in the heat exchange with gas to be heated is cooled further. 6. Verfahren nach Anspruch 4, dadurch gekennzeichnet, daß das anzuwärmende Gas kälteleistend entspannt wird.6. The method according to claim 4, characterized in that the gas to be warmed up is relieved of cold. 7. Verfahren nach einem der Ansprüche 1 bis 6, dadurch gekennzeichnet, daß das partiell kondensierte Erdgas einem Abscheider zugeführt wird, in den auch das vom Kopf der Rektifiziersäule abgezogene Gas geleitet wird, daß die flüssige Phase aus dem Abscheider in den oberen Bereich der Rektifiziersäule eingespeist wird und die gasförmige Phase aus dem Abscheider das wieder anzuwärmende Gas bildet.7. The method according to any one of claims 1 to 6, characterized characterized in that the partially condensed natural gas a separator is fed, in which also from the head the rectified column withdrawn gas is passed that the liquid phase from the separator in the upper area the rectification column is fed and the gaseous Phase from the separator the gas to be reheated forms.
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