EP2158437A2 - Method and device for the cryogenic separation of a methane-rich flow - Google Patents

Method and device for the cryogenic separation of a methane-rich flow

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Publication number
EP2158437A2
EP2158437A2 EP08805953A EP08805953A EP2158437A2 EP 2158437 A2 EP2158437 A2 EP 2158437A2 EP 08805953 A EP08805953 A EP 08805953A EP 08805953 A EP08805953 A EP 08805953A EP 2158437 A2 EP2158437 A2 EP 2158437A2
Authority
EP
European Patent Office
Prior art keywords
flow
methane
enriched
column
nitrogen
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP08805953A
Other languages
German (de)
French (fr)
Inventor
Pierre Briend
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
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
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP2158437A2 publication Critical patent/EP2158437A2/en
Withdrawn legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—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
    • F25J3/0257—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
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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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • 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
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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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/80—Processes or apparatus using other separation and/or other processing means using membrane, i.e. including a permeation step
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/40—Air or oxygen enriched air, i.e. generally less than 30mol% of O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/66—Landfill or fermentation off-gas, e.g. "Bio-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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/40—Air or oxygen enriched air, i.e. generally less than 30mol% of O2
    • 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
    • F25J2220/66—Separating acid gases, e.g. CO2, SO2, H2S or RSH
    • 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
    • F25J2270/14—External 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
    • F25J2270/14—External refrigeration with work-producing gas expansion loop
    • F25J2270/16—External refrigeration with work-producing gas expansion loop with mutliple gas expansion loops of the same refrigerant
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/30—Quasi-closed internal or closed external helium refrigeration 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/908—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by regenerative chillers, i.e. oscillating or dynamic systems, e.g. Stirling refrigerator, thermoelectric ("Peltier") or magnetic refrigeration
    • 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
    • F25J2280/00—Control of the process or apparatus
    • F25J2280/02—Control in general, load changes, different modes ("runs"), measurements

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a method for the cryogenic separation of a methane-rich feed flow (1) also containing carbon dioxide, nitrogen and oxygen, that comprises sending the flow to an adsorption purification unit (3, 29) for producing a flow lean in terms of carbon dioxide relative to the feed flow, cooling down a portion at least of the carbon dioxide lean flow for producing a cooled flow, sending a portion at least of the cooled flow to a distillation column (17), recovering from the distillation column a flow enriched in methane relative to the feed flow, and recovering from the distillation column a flow enriched in nitrogen and/or oxygen relative to the feed flow. The decarbonation tank is regenerated by a controlled flow of gaseous methane.

Description

Procédé et appareil de séparation cryogénique d'un débit riche en méthane Process and apparatus for cryogenic separation of a flow rich in methane
La présente invention concerne un procédé et un appareil de séparation cryogénique d'un débit riche en méthane.The present invention relates to a method and apparatus for cryogenic separation of a flow rich in methane.
Afin d'épurer un débit riche en méthane provenant d'une source organique, pour produire un produit épuré, il est nécessaire d'enlever les impuretés, telles que le dioxyde de carbone, l'oxygène et l'azote. Idéalement le produit contient moins de 2% de dioxyde de carbone et moins de 2% pour le contenu total en oxygène en azote.In order to purify a flow rich in methane from an organic source, to produce a purified product, it is necessary to remove impurities, such as carbon dioxide, oxygen and nitrogen. Ideally the product contains less than 2% carbon dioxide and less than 2% for the total oxygen content of nitrogen.
Tous les pourcentages de composition de ce document sont des pourcentages molaires.All percentages of composition of this document are molar percentages.
Selon un objet de l'invention, il est prévu un procédé de séparation cryogénique d'un débit d'alimentation riche en méthane contenant également du dioxyde de carbone et soit de l'azote soit de l'oxygène soit les deux dans lequel : i) on envoie le débit à une unité d'épuration par adsorption pour produire un débit appauvri en dioxyde de carbone par rapport au débit d'alimentation ii) on refroidit au moins une partie du débit appauvri en dioxyde de carbone pour produire un débit refroidi iii) on envoie au moins une partie du débit refroidi à une colonne de distillation iv) on soutire de la colonne de distillation un débit enrichi en méthane par rapport au débit d'alimentation et v) on soutire de la colonne de distillation un débit enrichi en azote et/ou oxygène par rapport au débit d'alimentation vi) caractérisé en ce que l'unité d'épuration est régénérée par au moins une partie du liquide enrichi en méthane vaporisé.According to one object of the invention, there is provided a cryogenic separation method of a feed rate rich in methane also containing carbon dioxide and either nitrogen or oxygen or both in which: i the flow is sent to an adsorption purification unit to produce a depleted flow rate of carbon dioxide relative to the feed rate; ii) at least a portion of the depleted flow rate of carbon dioxide is cooled to produce a cooled flow rate iii at least a part of the cooled flow rate is sent to a distillation column; iv) a flow enriched in methane is withdrawn from the distillation column with respect to the feed rate; and v) a flow enriched in the distillation column is withdrawn from the distillation column. nitrogen and / or oxygen with respect to the feed rate vi), characterized in that the purification unit is regenerated by at least a part of the vaporized methane enriched liquid.
Selon d'autres aspects facultatifs - le méthane vaporisé ayant servi de gaz de régénération constitue un produit et contient de préférence entre 1 et 3 % mol. de dioxyde de carboneAccording to other optional aspects - the vaporized methane which has served as a regeneration gas is a product and preferably contains between 1 and 3 mol%. of carbon dioxide
- on refroidit le débit appauvri en dioxyde de carbone en amont de la colonne au moyen d'au moins un fluide soutiré de la colonne . - le fluide soutiré de la colonne est le débit enrichi en azote et/ou en oxygène .the carbon dioxide depleted flow rate is cooled upstream of the column by means of at least one fluid withdrawn from the column. the fluid withdrawn from the column is the flow rate enriched with nitrogen and / or oxygen.
- le fluide soutiré de la colonne est le débit enrichi en méthane ;the fluid withdrawn from the column is the flow enriched in methane;
- le débit enrichi en méthane est soutiré sous forme liquide ; - le liquide enrichi en méthane se vaporise par échange de chaleur avec le débit appauvri en dioxyde de carbone ;the flow enriched with methane is withdrawn in liquid form; the liquid enriched in methane vaporises by heat exchange with the flow rate depleted of carbon dioxide;
- le contenu en dioxyde de carbone du liquide vaporisé ayant servi à la régénération est maintenu substantiellement constant, en particulier en y mélangeant une partie de liquide enrichi en méthane vaporisé pris en amont de l'unité d'épuration ;- The carbon dioxide content of the vaporized liquid used for the regeneration is kept substantially constant, in particular by mixing a portion of vaporized methane enriched liquid taken upstream of the purification unit;
- le maintien en froid est assuré au moins partiellement par vaporisation d'un débit d'azote liquide provenant d'une source extérieure ;- Keeping cold is provided at least partially by vaporization of a flow of liquid nitrogen from an external source;
- l'azote liquide se vaporise par échange de chaleur avec le débit appauvri en dioxyde de carbone ; - l'azote liquide se vaporise dans un condenseur de tête de la colonne ;the liquid nitrogen is vaporized by heat exchange with the depleted flow rate of carbon dioxide; the liquid nitrogen is vaporized in a top condenser of the column;
- le maintien en froid est assuré au moins partiellement par un cycle frigorigène ;- The maintenance in cold is provided at least partially by a refrigerant cycle;
- on produit le débit enrichi en méthane sous forme gazeuse et/ou liquide ;the enriched flow of methane is produced in gaseous and / or liquid form;
- on chauffe un rebouilleur de cuve de la colonne, éventuellement avec au moins une partie du débit à séparer ;- Warming a reboiler tank of the column, optionally with at least a portion of the flow to be separated;
- le débit soutiré de la colonne enrichi en méthane contient au moins 98, voire 99% méthane ;the flow rate withdrawn from the column enriched in methane contains at least 98 or even 99% methane;
- le débit d'alimentation contient entre 75 et 95% de méthane ;the feed rate contains between 75 and 95% of methane;
- le débit d'alimentation contient entre 3 et 25% en total d'azote et/ou d'oxygène.- The feed rate contains between 3 and 25% in total of nitrogen and / or oxygen.
Selon un autre aspect de l'invention, il est prévu un appareil de séparation cryogénique d'un débit d'alimentation riche en méthane contenant également du dioxyde de carbone et soit de l'azote soit de l'oxygène soit les deux comprenant : i) une unité d'épuration par adsorption et des moyens pour y envoyer le débit d'alimentation pour produire un débit appauvri en dioxyde de carbone par rapport au débit d'alimentation ii) des moyens de refroidissement d'au moins une partie du débit appauvri en dioxyde de carbone pour produire un débit refroidi iii) une colonne de distillation et des moyens pour envoyer au moins une partie du débit refroidi à la colonne de distillation iv) des moyens pour soutirer de la colonne de distillation un débit enrichi en méthane par rapport au débit d'alimentation et v) des moyens pour soutirer de la colonne de distillation un débit enrichi en azote et/ou oxygène par rapport au débit d'alimentation. L'invention sera décrite en plus de détail en se référant aux figures dont les figures 1 et 6 représentant schématiquement un appareil selon l'invention, la figure 2 est un graphique représentation un échange de chaleur ayant lieu dans un échangeur de l'appareil selon l'invention, les figures 3 et 4 illustrent des cycles de production de frigories exploitables pour la production du froid nécessaire au procédé selon l'invention et la figure 5 représente schématiquement un aspect d'un appareil selon l'invention.According to another aspect of the invention, there is provided an apparatus for cryogenic separation of a feed rate rich in methane also containing carbon dioxide and either nitrogen or oxygen or both comprising: ) an adsorption purification unit and means for sending the feed rate therein to produce a depleted flow rate of carbon dioxide with respect to the feed rate; ii) means for cooling at least a portion of the depleted flow rate in carbon dioxide to produce a cooled flow iii) a distillation column and means for sending at least a portion of the cooled flow to the distillation column; iv) means for extracting from the distillation column a flow enriched in methane with respect to the feed rate; and v) means for withdrawing from the distillation column a flow enriched in nitrogen and / or oxygen with respect to the feed rate. The invention will be described in more detail with reference to the figures of which Figures 1 and 6 schematically showing an apparatus according to the invention, Figure 2 is a graph showing a heat exchange taking place in a heat exchanger of the apparatus according to FIGS. 3 and 4 illustrate production cycles for exploitable frigories for producing the cold necessary for the process according to the invention, and FIG. 5 schematically represents an aspect of an apparatus according to the invention.
Dans la Figure 1 , un gaz d'alimentation 1 à température ambiante et moyenne pression ( 5 à 15 bars), ayant été épuré dans une unité de perméation ou d'adsorption, contient >75% de méthane, <2% de dioxyde de carbone et <25% au total d'oxygène et d'azote. De ces 25%, environ 20% sont constitués par de l'azote et le reste d'oxygène. Le contenu en oxygène et en azote dépasse largement celui souhaité pour le produit. Le gaz 1 est envoyé à une unité d'adsorption constitué par deux bouteilles d'adsorbants 3, 29 pour produire un débit appauvri en CO2 5. Ce débit 5 est envoyé à une boîte froide 7 contenant des échangeurs de chaleur 9, 13 et une colonne 17. Le débit 5, contenant entre 75 et 95% de méthane et de 3 à 25% au total d'azote et d'oxygène, se refroidit et se liquéfie partiellement dans l'échangeur de chaleur 9, selon le graphique que l'on voit à la figure 2.In Figure 1, a feed gas 1 at room temperature and medium pressure (5 to 15 bar), having been purified in a permeation or adsorption unit, contains> 75% methane, <2% carbon dioxide, and carbon and <25% total oxygen and nitrogen. Of these 25%, about 20% consist of nitrogen and the rest of oxygen. The oxygen and nitrogen content greatly exceeds that desired for the product. The gas 1 is sent to an adsorption unit constituted by two bottles of adsorbents 3, 29 to produce a depleted flow rate of CO 2 5. This flow 5 is sent to a cold box 7 containing heat exchangers 9, 13 and 17. The flow 5, containing between 75 and 95% methane and 3 to 25% total nitrogen and oxygen, cools and partially liquefies in the heat exchanger 9, according to the graph that we see in Figure 2.
L'échangeur 9 est un échangeur à plaques brasées en aluminium ou en acier inoxydable.The exchanger 9 is a brazed plate heat exchanger made of aluminum or stainless steel.
Le débit refroidi 5, qui est diphasique, assure le rebouillage d'un rebouilleur de cuve 11 de la colonne 17 et la chaleur produite 23 est transférée à la cuve de la colonne. Ensuite le débit 5 se liquéfie dans l'échangeur de chaleur 13, est détendu d'environ la moitié de sa pression dans une vanne 15 et envoyé à un point intermédiaire de la colonne 17.The cooled flow 5, which is two-phase, ensures the reboiling of a vessel reboiler 11 of the column 17 and the heat generated 23 is transferred to the column vessel. Then the flow 5 liquefies in the heat exchanger 13, is expanded by about half of its pressure in a valve 15 and sent to an intermediate point of the column 17.
Dans cette colonne 17, qui contient des garnissages structurés, la distillation du débit 5 liquéfié est effectuée pour produire en cuve un débit liquide 27 riche en méthane contenant moins de 2% au total d'azote et d'oxygène et un débit gazeux 19 en tête de colonne enrichi en azote et /ou en oxygène et contenant moins de 5% de méthane.In this column 17, which contains structured packings, the distillation of the liquefied flow is performed to produce a liquid flow in the vat. 27 a methane-rich stream containing less than 2% total of nitrogen and oxygen and a gas flow 19 at the top of the column enriched in nitrogen and / or oxygen and containing less than 5% methane.
Le refroidissement du condenseur de tête 67 (Figures 3 et 4) de la colonne 17 est assuré de diverses façons, pour enlever de la chaleur 21 de la colonne.Cooling of the overhead condenser 67 (FIGS. 3 and 4) of the column 17 is provided in various ways to remove heat from the column.
Par exemple, le condenseur 67 peut être refroidi par biberonnage d'azote liquide provenant d'une source extérieure.For example, the condenser 67 may be cooled by liquid nitrogen bubbling from an outside source.
Le froid peut autrement être fourni par une machine de production de froid, telle qu'une moteur Stirling, une machine Gifford-McMahon, un tube à puise... Alternativement les frigories pour le condenseur 67 peuvent être fournies par un cycle azote, tel qu'illustré dans la Figure 3. L'azote 66 est envoyé au condenseur 67 où il se vaporise pour former le gaz 67. Le gaz 67 est mélangé avec le gaz de tête 66 du séparateur de phases 65 et ensuite avec le débit 71 . Le débit 45 ainsi formé est envoyé à un mélangeur, refroidi dans les échangeurs 61 , 53 et ensuite comprimé dans le compresseur 44 alimenté en énergie 43. Le débit comprimé 47 est refroidi dans un échangeur 49 pour former le débit 51 , chauffé dans l'échangeur 53 pour former le gaz 55 et détendu dans une turbine 55. Le débit 55 est divisé en deux, une partie 59 étant envoyée à la turbine 69 pour former le débit 71 et le reste 57 étant envoyé à l'échangeur 61. Le débit 57 se détend dans la vanne 63 et est envoyé au séparateur de phases 65. Le débit liquide du séparateur 65 est envoyé au condenseur 67.The cold may otherwise be provided by a cold-producing machine, such as a Stirling engine, a Gifford-McMahon machine, a feed tube, etc. Alternatively, the frigories for the condenser 67 may be provided by a nitrogen cycle, such as As illustrated in FIG. 3. Nitrogen 66 is sent to condenser 67 where it vaporizes to form gas 67. Gas 67 is mixed with the overhead gas 66 of phase separator 65 and then flow 71. The flow 45 thus formed is sent to a mixer, cooled in the exchangers 61, 53 and then compressed in the compressor 44 supplied with energy 43. The compressed flow 47 is cooled in an exchanger 49 to form the flow 51, heated in the exchanger 53 for forming the gas 55 and expanded in a turbine 55. The flow 55 is divided in two, a portion 59 being sent to the turbine 69 to form the flow 71 and the remainder 57 being sent to the exchanger 61. The flow 57 expands in the valve 63 and is sent to the phase separator 65. The liquid flow of the separator 65 is sent to the condenser 67.
Une autre possibilité (fig.4) est d'utiliser un cycle Brayton avec de l'hélium comme fluide de cycle. Un gaz 81 , réchauffé dans le condenseur 67 est envoyé à un échangeur 83, comprimé dans un compresseur 85, alimenté par de l'énergie 87 pour former le débit 89. Ce débit est envoyé à l'échangeur 91 et ensuite à l'échangeur 83. Puis il est détendu dans une turbine 93 avant d'être envoyé au condenseur 67.Another possibility (fig.4) is to use a Brayton cycle with helium as cycle fluid. A gas 81, heated in the condenser 67 is sent to an exchanger 83, compressed in a compressor 85, powered by energy 87 to form the flow 89. This flow is sent to the exchanger 91 and then to the exchanger 83. Then it is expanded in a turbine 93 before being sent to the condenser 67.
Dans le cas où le méthane est produit uniquement sous forme gazeuse, le méthane liquide 27 contenant <2% d'azote+oxygèπe et >98% de méthane se vaporise par échange de chaleur dans l'échangeur 9.In the case where the methane is produced only in gaseous form, the liquid methane 27 containing <2% nitrogen + oxygen and> 98% methane vaporizes by heat exchange in the exchanger 9.
Le résiduaire enrichi en azote et/ou en oxygène 19 réchauffe le mélange à séparer dans l'échangeur 13, se réchauffe dans l'échangeur 9 et est envoyé à l'air. Il contient moins de 5% de méthane. Comme montré en détail dans la Figure 5, le méthane vaporisé à l'échangeur 9 est envoyé à l'autre bouteille d'adsorbants 29 afin de la régénérer et le gaz de régénération 32 ainsi produit sert de produit du procédé, étant enrichi en dioxyde de carbone par rapport au débit 27 pour contenir entre 1 et 3 % mol. de dioxyde de carbone, par exemple.The waste enriched in nitrogen and / or oxygen 19 warms the mixture to be separated in the exchanger 13, is heated in the exchanger 9 and is sent to air. It contains less than 5% methane. As shown in detail in FIG. 5, the methane vaporized at the exchanger 9 is sent to the other bottle of adsorbents 29 in order to regenerate it and the regeneration gas 32 thus produced serves as a product of the process, being enriched in dioxide. of carbon relative to the flow 27 to contain between 1 and 3 mol%. carbon dioxide, for example.
Le contenu en dioxyde de carbone du produit 32 est analysé par un analyseur AIC 105 et le contenu est maintenu substantiellement constant au moyen d'une vanne 103 commandée par I AIC qui ouvre une conduite de contournement 101 permettant de mélanger du gaz 101 plus riche en méthane au débit 32, au besoin. Comme l'opération des adsorbeurs est cyclique, cette disposition est nécessaire pour éviter une variation de pureté cyclique du produit 32.The carbon dioxide content of the product 32 is analyzed by an AIC analyzer 105 and the contents are kept substantially constant by means of a valve 103 controlled by I AIC which opens a bypass line 101 for mixing gas 101 which is richer in water. methane at flow 32, as needed. Since the operation of the adsorbers is cyclic, this arrangement is necessary to avoid a cyclic purity variation of the product 32.
Optionnellement, le produit 32 est comprimé dans un ou plusieurs compresseurs 31 jusqu'à une haute pression (20 à 30 bars), voire une très haute pression (200 à 350 bars), comme illustré à la Figure 1.Optionally, the product 32 is compressed in one or more compressors 31 to a high pressure (20 to 30 bar), or even a very high pressure (200 to 350 bar), as shown in Figure 1.
Ce produit contient un peu plus que >96% méthane, < 2% d'azote+oxygène et < 2% de CO2.This product contains a little more than> 96% methane, <2% nitrogen + oxygen and <2% CO2.
Dans la Figure 6, un procédé selon l'invention est illustré qui permet de produire le méthane sous forme liquide. Un gaz d'alimentation 1 ayant été épuré dans une unité de perméation contient 76,5% de méthane, 1 ,6% de dioxyde de carbone et 22% au total d'oxygène et d'azote. Le contenu en oxygène et en azote dépasse largement celui souhaité pour le produit.In Figure 6, a method according to the invention is illustrated which allows to produce methane in liquid form. A feed gas 1 having been purified in a permeation unit contains 76.5% methane, 1.6% carbon dioxide and 22% total oxygen and nitrogen. The oxygen and nitrogen content greatly exceeds that desired for the product.
Le gaz 1 est envoyé à une unité d'adsorption constitué par deux bouteilles d'adsorbants 3, 29 pour produire un débit appauvri en CO2 5. Ce débit 5 est envoyé à une boîte froide 7 contenant des échangeurs de chaleur 9,13 et une colonne 17. Le débit 5, contenant entre 75 et 95% de méthane et de 3 à 25% au total d'azote et d'oxygène, se refroidit et se liquéfie partiellement dans l'échangeur de chaleur 9, selon le graphique que l'on voit à la figure 2.The gas 1 is sent to an adsorption unit consisting of two adsorbent bottles 3, 29 to produce a depleted flow rate of CO 2 5. This flow 5 is sent to a cold box 7 containing heat exchangers 9, 13 and 17. The flow 5, containing between 75 and 95% methane and 3 to 25% total nitrogen and oxygen, cools and partially liquefies in the heat exchanger 9, according to the graph that we see in Figure 2.
Le débit refroidi 5, qui est diphasique, assure le rebouillage d'un rebouilleur de cuve 11 de la colonne 17 et la chaleur produite 23 est transférée à la cuve de la colonne. Ensuite le débit 5 se liquéfie dans l'échangeur de chaleur 13, est détendu dans une vanne 15 et envoyé à un point intermédiaire de la colonne 17.The cooled flow 5, which is two-phase, ensures the reboiling of a vessel reboiler 11 of the column 17 and the heat generated 23 is transferred to the column vessel. Then the flow 5 liquefies in the heat exchanger 13, is expanded in a valve 15 and sent to an intermediate point of the column 17.
Dans cette colonne 17, qui contient des garnissages structurés, la distillation du débit 5 liquéfié est effectuée pour produire en cuve un débit liquide 27 riche en méthane contenant moins de 2% au total d'azote+oxygène et un débit gazeux 19 en tête de colonne enrichi en azote+oxygène et contenant moins de 5% de méthane.In this column 17, which contains structured packings, the distillation of the liquefied flow is performed to produce a liquid flow in the vat. 27 rich in methane containing less than 2% in total nitrogen + oxygen and a gas flow 19 at the top of column enriched in nitrogen + oxygen and containing less than 5% methane.
Le refroidissement du condenseur de tête 203 (Figures 3 et 4) de la colonne 17 est assuré par envoi d'azote liquide de biberonnage 201 provenant d'une source extérieure.The cooling of the overhead condenser 203 (FIGS. 3 and 4) of the column 17 is ensured by sending liquid feeding liquid nitrogen 201 from an external source.
Le résiduaire enrichi en azote et/ou en oxygène 19 est détendu dans une vanne 25, mélangé avec le débit d'azote liquide de biberonnage vaporisé 204. Le débit mélangé 207 est mélangé dans un mélangeur, refroidit le mélange à séparer dans l'échangeur 13, se réchauffe dans l'échangeur 9 et est envoyé à l'air. Il contient moins de 5% de méthane.The waste enriched in nitrogen and / or oxygen 19 is expanded in a valve 25, mixed with the liquid nitrogen vaporization flow rate 204. The mixed flow 207 is mixed in a mixer, cools the mixture to be separated in the exchanger 13, warms up in the exchanger 9 and is sent to the air. It contains less than 5% methane.
Le méthane liquide 27 est produit comme produit final.Liquid methane 27 is produced as the final product.
Pour tenir en froid l'échangeur 9, un autre débit d'azote de biberonnage 21 1 est envoyé à l'échangeur 9 où il se vaporise pour former le débit 213. Ce débit d'azote 213 sert ensuite à régénérer la bouteille d'adsorbants 215 avant d'être rejeté à l'atmosphère comme débit 217.To keep the heat exchanger 9 cold, another flow of feeding nitrogen 21 1 is sent to the exchanger 9 where it vaporises to form the flow 213. This flow rate of nitrogen 213 is then used to regenerate the bottle. adsorbents 215 before being released to the atmosphere as flow 217.
Alternativement, comme pour la Figure 1 , l'azote 21 1 peut être remplacé par une partie du produit 27.Alternatively, as in FIG. 1, the nitrogen 21 1 may be replaced by a portion of the product 27.
Il sera compris que n'importe laquelle source de froid indiquée pour la Figure 1 peut être utilisée pour le procédé de la Figure 6. It will be understood that any cold source indicated for Figure 1 may be used for the process of Figure 6.

Claims

REVENDICATIONS
1. Procédé de séparation cryogénique d'un débit d'alimentation riche en méthane contenant également du dioxyde de carbone et soit de l'azote soit de l'oxygène soit les deux dans lequel : i) on envoie le débit à une unité d'épuration par adsorption (3, 29) pour produire un débit appauvri en dioxyde de carbone par rapport au débit d'alimentation ii) on refroidit au moins une partie du débit appauvri en dioxyde de carbone pour produire un débit refroidi iii) on envoie au moins une partie du débit refroidi à une colonne de distillation (17) iv) on soutire de la colonne de distillation un débit enrichi en méthane (27) par rapport au débit d'alimentation et v) on soutire de la colonne de distillation un débit (19) enrichi en azote et/ou oxygène par rapport au débit d'alimentation et caractérisé en ce que vi) l'unité d'épuration (3, 29) est régénérée par au moins une partie du liquide enrichi en méthane vaporisé.A method of cryogenically separating a feed flow rich in methane also containing carbon dioxide and either nitrogen or oxygen or both wherein: i) the flow is fed to a unit of adsorption purification (3, 29) to produce a depleted flow rate of carbon dioxide relative to the feed rate ii) at least a portion of the depleted flow rate of carbon dioxide is cooled to produce a cooled flow rate iii) at least one a part of the flow cooled to a distillation column (17) iv) is withdrawn from the distillation column a methane enriched flow (27) with respect to the feed rate and v) is withdrawn from the distillation column a flow ( 19) enriched in nitrogen and / or oxygen with respect to the feed rate and characterized in that vi) the purification unit (3, 29) is regenerated by at least a part of the vaporized methane enriched liquid.
2. Procédé selon la revendication 1 dans lequel on refroidit le débit appauvri en dioxyde de carbone en amont de la colonne (17) au moyen d'au moins un fluide soutiré de la colonne.2. Method according to claim 1 wherein the carbon dioxide depleted flow rate is cooled upstream of the column (17) by means of at least one fluid withdrawn from the column.
3. Procédé selon la revendication 2 dans lequel le fluide soutiré de la colonne (17) est le débit enrichi en azote et/ou en oxygène (19).3. The method of claim 2 wherein the fluid withdrawn from the column (17) is the flow enriched in nitrogen and / or oxygen (19).
4. Procédé selon la revendication 2 ou3 dans lequel le fluide soutiré de la colonne (17) est le débit enrichi en méthane (27).4. The method of claim 2 or 3 wherein the fluid withdrawn from the column (17) is the flow enriched in methane (27).
5. Procédé selon la revendication 4 dans lequel le débit enrichi en méthane (27) est soutiré sous forme liquide. 5. The method of claim 4 wherein the flow enriched methane (27) is withdrawn in liquid form.
6. Procédé selon la revendication 5 dans lequel le liquide enrichi en méthane (27) se vaporise par échange de chaleur avec le débit (5) appauvri en dioxyde de carbone.6. The method of claim 5 wherein the methane enriched liquid (27) vaporizes by heat exchange with the flow (5) depleted carbon dioxide.
7. Procédé selon l'une des revendications précédentes dans lequel le contenu en dioxyde de carbone du liquide vaporisé ayant servi à la régénération est maintenu substantiellement constant, en particulier en y mélangeant une partie de liquide enrichi en méthane vaporisé (101 ) pris en amont de l'unité d'épuration.7. Method according to one of the preceding claims wherein the carbon dioxide content of the vaporized liquid used for the regeneration is kept substantially constant, in particular by mixing a portion of vaporized methane enriched liquid (101) taken upstream. of the purification unit.
8. Procédé selon l'une des revendications précédentes dans lequel le maintien en froid est assuré au moins partiellement par vaporisation d'un débit d'azote liquide (201 , 21 1) provenant d'une source extérieure.8. Method according to one of the preceding claims wherein the maintaining cold is provided at least partially by vaporization of a liquid nitrogen flow (201, 21 1) from an external source.
9. Procédé selon la revendication 9 dans lequel l'azote liquide se vaporise par échange de chaleur avec le débit appauvri en dioxyde de carbone.The process of claim 9 wherein the liquid nitrogen vaporizes by heat exchange with the depleted flow rate of carbon dioxide.
10. Procédé selon la revendication 8 ou 9 dans lequel l'azote liquide se vaporise dans un condenseur de tête (67) de la colonne (17).The method of claim 8 or 9 wherein the liquid nitrogen vaporizes in a head condenser (67) of the column (17).
11 . Procédé selon l'une des revendications précédentes dans lequel le maintien en froid est assuré au moins partiellement par un cycle frigorigène.11. Method according to one of the preceding claims wherein the maintenance in cold is provided at least partially by a refrigerant cycle.
12. Procédé selon l'une des revendications précédentes dans lequel on produit le débit enrichi en méthane (27) sous forme gazeuse et/ou liquide.12. Method according to one of the preceding claims wherein the flow enriched methane (27) in gaseous and / or liquid form is produced.
13. Procédé selon l'une des revendications précédentes dans lequel on chauffe un rebouilleur de cuve (11 ) de la colonne (17), éventuellement avec au moins une partie du débit à séparer.13. Method according to one of the preceding claims wherein a tank reboiler (11) of the column (17) is heated, optionally with at least a portion of the flow to be separated.
14. Procédé selon l'une des revendications précédentes dans lequel le débit soutiré de la colonne enrichi en méthane (27) contient au moins 98, voire 99% méthane. 14. Method according to one of the preceding claims wherein the flow rate withdrawn from the enriched methane column (27) contains at least 98 or 99% methane.
15. Procédé selon l'une des revendications précédentes dans lequel le débit d'alimentation (1) contient entre 75 et 95% de méthane.15. Method according to one of the preceding claims wherein the feed rate (1) contains between 75 and 95% methane.
16. Procédé selon la revendication 17 dans lequel le débit d'alimentation (1) contient entre 3 et 25% en total d'azote et/ou d'oxygène. 16. The method of claim 17 wherein the feed rate (1) contains between 3 and 25% in total of nitrogen and / or oxygen.
EP08805953A 2007-06-14 2008-06-06 Method and device for the cryogenic separation of a methane-rich flow Withdrawn EP2158437A2 (en)

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WO2009004207A2 (en) 2009-01-08
WO2009004207A3 (en) 2013-07-18

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