EP2158437A2 - Verfahren und vorrichtung zur kryogenen trennung eines methanreichen stroms - Google Patents

Verfahren und vorrichtung zur kryogenen trennung eines methanreichen stroms

Info

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Withdrawn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
English (en)
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/de
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • 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
    • F25J2205/40—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
    • 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
    • F25J2205/80—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
    • 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
    • F25J2210/40—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
    • 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
    • F25J2270/30—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
    • 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
    • F25J2270/908—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
    • 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
    • F25J2280/00—Control of the process or apparatus
    • F25J2280/02—Control in general, load changes, different modes ("runs"), measurements

Definitions

  • the present invention relates to a method and apparatus for cryogenic separation of a flow rich in methane.
  • the product contains less than 2% carbon dioxide and less than 2% for the total oxygen content of nitrogen.
  • 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.
  • the vaporized methane which has served as a regeneration gas is a product and preferably contains between 1 and 3 mol%. of carbon dioxide
  • 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.
  • the fluid withdrawn from the column is the flow enriched in methane
  • 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;
  • 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;
  • 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;
  • the maintenance in cold is provided at least partially by a refrigerant cycle
  • the enriched flow of methane is produced in gaseous and / or liquid form
  • the flow rate withdrawn from the column enriched in methane contains at least 98 or even 99% methane
  • the feed rate contains between 75 and 95% of methane
  • the feed rate contains between 3 and 25% in total of nitrogen and / or oxygen.
  • 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.
  • FIG. 1 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
  • FIG. 5 schematically represents an aspect of an apparatus according to the invention.
  • 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 exchanger 9 is a brazed plate heat exchanger made of aluminum or stainless steel.
  • 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.
  • 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.
  • 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.
  • the condenser 67 may be cooled by liquid nitrogen bubbling from an outside source.
  • the cold may otherwise be provided by a cold-producing machine, such as a Stirling engine, a Gifford-McMahon machine, a feed tube, etc.
  • 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.
  • FIG.4 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.
  • the liquid methane 27 containing ⁇ 2% nitrogen + oxygen and> 98% methane vaporizes by heat exchange in the exchanger 9.
  • 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.
  • 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.
  • 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.
  • This product contains a little more than> 96% methane, ⁇ 2% nitrogen + oxygen and ⁇ 2% CO2.
  • 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.
  • 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 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.
  • 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.
  • 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.
  • 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.
  • Liquid methane 27 is produced as the final product.
  • the nitrogen 21 1 may be replaced by a portion of the product 27.

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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)
EP08805953A 2007-06-14 2008-06-06 Verfahren und vorrichtung zur kryogenen trennung eines methanreichen stroms Withdrawn EP2158437A2 (de)

Applications Claiming Priority (2)

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FR0755758A FR2917489A1 (fr) 2007-06-14 2007-06-14 Procede et appareil de separation cryogenique d'un debit riche en methane
PCT/FR2008/051017 WO2009004207A2 (fr) 2007-06-14 2008-06-06 Procede et appareil de separation cryogenique d'un debit riche en methane

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FR3046086B1 (fr) 2015-12-24 2018-01-05 Waga Energy Procede de production de biomethane par epuration de biogaz issu d'installations de stockage de dechets non-dangereux (isdnd) et installation pour la mise en œuvre du procede
FR3051892B1 (fr) * 2016-05-27 2018-05-25 Waga Energy Procede de separation cryogenique d'un debit d'alimentation contenant du methane et des gaz de l'air, installation pour la production de bio methane par epuration de biogaz issus d'installations de stockage de dechets non-dangereux (isdnd) mettant en œuvre le procede
FR3066258A1 (fr) * 2017-05-11 2018-11-16 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Systeme et procede de traitement d’un flux de gaz naturel
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FR3075658B1 (fr) 2017-12-21 2022-01-28 Air Liquide Procede de limitation de la concentration d'oxygene contenu dans un courant de biomethane
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US8997519B2 (en) 2015-04-07
CN102099648A (zh) 2011-06-15
JP5259703B2 (ja) 2013-08-07
FR2917489A1 (fr) 2008-12-19
WO2009004207A3 (fr) 2013-07-18
WO2009004207A2 (fr) 2009-01-08
US20100192627A1 (en) 2010-08-05
JP2010538234A (ja) 2010-12-09

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