EP2856050A2 - Vorrichtung und verfahren zur kryogenen trennung einer mischung aus kohlenmonoxid und methan plus wasserstoff und/oder stickstoff - Google Patents

Vorrichtung und verfahren zur kryogenen trennung einer mischung aus kohlenmonoxid und methan plus wasserstoff und/oder stickstoff

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Publication number
EP2856050A2
EP2856050A2 EP13727260.5A EP13727260A EP2856050A2 EP 2856050 A2 EP2856050 A2 EP 2856050A2 EP 13727260 A EP13727260 A EP 13727260A EP 2856050 A2 EP2856050 A2 EP 2856050A2
Authority
EP
European Patent Office
Prior art keywords
column
methane
liquid
carbon monoxide
gas
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.)
Granted
Application number
EP13727260.5A
Other languages
English (en)
French (fr)
Other versions
EP2856050B1 (de
Inventor
Pascal Marty
Jean-Jacques Talbot
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
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 LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority to PL13727260T priority Critical patent/PL2856050T3/pl
Publication of EP2856050A2 publication Critical patent/EP2856050A2/de
Application granted granted Critical
Publication of EP2856050B1 publication Critical patent/EP2856050B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the feed stream
    • F25J3/0223—H2/CO mixtures, i.e. synthesis gas; Water gas or shifted synthesis gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0233—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of CnHm with 1 carbon atom or more
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • 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
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    • 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
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    • F25J3/0261—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon monoxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
    • 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
    • F25J3/0271—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 H2/CO mixtures, i.e. of synthesis gas
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    • 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
    • F25J3/0276—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 H2/N2 mixtures, i.e. of ammonia synthesis gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/30—Processes or apparatus using separation by rectification using a side column in a single pressure 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
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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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/76—Refluxing the column with condensed overhead gas being cycled in a quasi-closed loop 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
    • 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
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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
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
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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
    • F25J2210/06—Splitting of the feed stream, e.g. for treating or cooling in different ways
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/02—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams using a pump in general or hydrostatic pressure increase
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/60—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being (a mixture of) hydrocarbons
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
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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
    • F25J2260/00—Coupling of processes or apparatus to other units; Integrated schemes
    • F25J2260/02—Integration in an installation for exchanging heat, e.g. for waste heat recovery
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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
    • F25J2270/02—Internal refrigeration with liquid vaporising loop
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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
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
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    • F25J2270/00—Refrigeration techniques used
    • F25J2270/24—Quasi-closed internal or closed external carbon monoxide refrigeration cycle
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    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/40—Vertical layout or arrangement of cold equipments within in the cold box, e.g. columns, condensers, heat exchangers etc.
    • 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
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/42—Modularity, pre-fabrication of modules, assembling and erection, horizontal layout, i.e. plot plan, and vertical arrangement of parts of the cryogenic unit, e.g. of the cold box

Definitions

  • Apparatus and method for cryogenic separation of a mixture of carbon monoxide and methane and hydrogen and / or nitrogen The present invention relates to an apparatus and method for cryogenically separating a mixture of carbon monoxide, methane and hydrogen and possibly nitrogen.
  • the mixtures may consist of:
  • Nitrogen with hydrogen impurities, carbon monoxide and methane (cold box nitrogen wash).
  • An object of the invention is to make more compact a cryogenic separation apparatus of a mixture of carbon monoxide, hydrogen and methane when the methane must be produced under pressure.
  • Another object of the invention is, in certain cases, to reduce the maximum height of a cryogenic separation apparatus of a mixture of carbon monoxide, hydrogen and methane. This reduces the cost of the device as well as the transportation costs.
  • the liquid methane withdrawn from the tank of the CO / CH 4 column can be pressurized in a pump to be stored and / or sent to a customer or to be sent to the top of the methane wash column, if necessary.
  • an apparatus for the cryogenic separation of a mixture of methane, carbon monoxide and hydrogen and optionally nitrogen comprising a first separation unit comprising at least a first column and or a phase separator, the first separation unit being supplied with the mixture, a first pipe for removing a gas enriched in hydrogen and possibly nitrogen from the first unit, a second pipe for discharging a liquid containing methane and monoxide of carbon of the first column or phase separator, a second column connected to the second pipe, a third pipe connected to the tank of the second column to withdraw a liquid enriched in methane and a fourth pipe connected to the head of the second.
  • the second column for withdrawing a gas enriched in carbon monoxide or nitrogen, the first column and / or one or more separator (s) of being arranged below the second column, the two columns or the second column and the phase separator (s) having the same main axis, so that the methane-enriched liquid is produced at a higher pressure that the pressure of the tank of the second column, the second column comprising a tank reboiler characterized in that, where appropriate, when the apparatus comprises a first column, it does not include means for sending overhead gas from the first column to heat the bottom reboiler of the second column and in that the second conduit is a pipe connected to the tank of the first column.
  • the apparatus comprises:
  • a pump connected to the third pipe, disposed closer to the ground than the tank of the second column.
  • an auxiliary column whose head is optionally connected to the pump and whose tank is connected to the head of the first column by means for sending gas from the head of the first column to the tank of the auxiliary column and by means for sending liquid from the tank of the auxiliary column to the head of the first column, the auxiliary column being arranged next to the first column.
  • the auxiliary column is arranged so that its tank is farther from the ground than the head of the first column.
  • the auxiliary column is attached to the second column.
  • the first unit comprises a pre-treatment column, a line for feeding the mixture from the pre-treatment column to the first column, the auxiliary column being fixed to the pre-treatment column.
  • the apparatus comprises a post-treatment column downstream of the second column, the auxiliary column being fixed to the post-treatment column.
  • the first unit comprises a methane scrubbing column, which column is connected to the first column to feed it with the mixture which is a bottom liquid of the methane scrubbing column, the head of the methane scrubbing column being connected to the pump.
  • the first unit comprises a phase separator and means for supplying liquid phase separator as the mixture which feeds the first column.
  • the first unit comprises a washing column and the first column, the washing liquid being rich in carbon monoxide, as well as means for sending the tank liquid from the wash column to the first column.
  • the first unit comprises a washing column, the washing liquid being rich in nitrogen, the washing column constituting the first column.
  • the first unit comprises a nitrogen wash column
  • the second liquid contains methane and nitrogen
  • the second column produces a nitrogen enriched gas
  • a cryogenic separation process of a mixture of methane and carbon monoxide as well as hydrogen and optionally nitrogen in which a first separation of the mixture is carried out using at least a first column or a phase separator fed by the mixture, to produce a methane-enriched fluid containing carbon monoxide and / or nitrogen connected to the tank of the first column or phase separator, the fluid is separated in a second column to produce a gas enriched in carbon monoxide and optionally nitrogen and a methane-enriched liquid, the first column or the phase separator is arranged below the second column, the two columns or the second column and the phase separator having the same main axis, so that the liquid enriched in methane is pressurized at least in part by hydrostatic pressure, the second e column comprising a bottom reboiler characterized in that the bottom reboiler is heated by a gas other than a top gas of the first column and in that the methane-enriched fluid comes from the tank of
  • the bottom reboiler is heated by a cycle gas which is carbon monoxide.
  • a head gas of the first column is heated in an exchanger where the mixture cools.
  • the pump is on the ground.
  • a top gas of the first column is sent to the tank of an auxiliary column and of the methane-enriched liquid to the top of the column, the auxiliary column being arranged next to the first column.
  • the first unit comprises a pre-treatment column, a line for feeding the mixture from the pre-treatment column to the first column, the auxiliary column being fixed to the pre-treatment column.
  • the apparatus comprises a post-treatment column downstream of the second column, the auxiliary column being attached to the post-treatment column.
  • the first unit comprises a methane wash column, the wash tank liquid being fed to the first column as the mixture and pressurized methane enriched liquid being fed to the wash column.
  • the first unit comprises a washing column fed with a washing liquid being rich in carbon monoxide or nitrogen, the washing column liquid being sent to the first column.
  • the process produces liquid methane as final product from the vessel of the second column.
  • the first unit comprises a nitrogen wash column
  • the second liquid contains methane and nitrogen
  • the second column produces a nitrogen enriched gas
  • FIG. 1 represents a methane scrubbing process according to the prior art
  • FIGS. 2 and 3 represent methane scrubbing processes according to the invention
  • FIG. 4 represents a partial condensation process according to the prior art
  • FIG. 5 represents a partial condensation process according to the invention
  • FIG. 6 represents a carbon monoxide washing process according to the prior art
  • FIG. 7 represents a method of washing with carbon monoxide.
  • FIG. 8 represents a nitrogen washing process according to the prior art
  • FIG. 9 represents a nitrogen washing process according to the invention.
  • a mixture of hydrogen, carbon monoxide and methane 1 is purified in unit 3 to remove water and carbon dioxide.
  • the purified mixture cools in the main cryogenic exchanger 9 to be sent to a phase separator 7, where it is separated to form a hydrogen-enriched gas 11 and a methane-enriched liquid 13.
  • the gas 11 separates in a methane wash column 17 fed at the top by a washing liquid 41 rich in methane.
  • the bottom liquid of the column 17 is mixed with the liquid 13 to form the liquid 18 rich in CO and CH 4 and also containing the nitrogen sent to the top of a depletion column 19 (in English "flash column") having a tank reboiler 22.
  • the gas 21 withdrawn at the top of the column 19 is enriched in hydrogen and is heated in the exchanger 9 for recovery as a purge gas to a fuel system in general.
  • the bottom liquid 23 of the column 19 contains mainly carbon monoxide (and nitrogen) and methane and is expanded in the valve 25 and then sent for separation in the column CO / CH 4 27.
  • a gas 44 enriched in carbon monoxide is formed at the top of the column and a liquid enriched in methane 33 is formed in the bottom of the column.
  • the liquid 33 is divided in two, a part 37 being reheated (or not) in the main cryogenic exchanger 9 for recovery as a purge gas (or in liquid form bypassing the exchanger 9) at the pressure of the column CO / CH 4 (a few bars) and the other part being pressurized by a pump 36 to feed the head of the methane washing column 17 and for possible upgrading under pressure (fluid 38) in gaseous form via the main cryogenic exchanger 9 (or directly in liquid form by short-circuiting the exchanger 9).
  • a carbon monoxide cycle keeps the appliance cold. Carbon monoxide from the top of the column 27 is heated in the exchanger 9, sent as flow 45 to a compressor 51. Part of the Carbon monoxide is produced as pressurized gas 53 at the outlet of the compressor. Another part 57 cools in exchanger 9 and is divided in two. A portion 59 at an intermediate temperature of the exchanger 9 is expanded in a turbine 61 and sent via a valve 63 via line 65 to the compressor 51. Another part 67 continues to cool in the exchanger 9. A fraction 69 of the cooled carbon monoxide serves to heat the reboiler 22 of the depletion column 19 and is condensed.
  • Another fraction 71 serves to heat the bottom reboiler 31 of the CO / CH 4 column 27 and is mixed with the condensed fraction 69.
  • the entire flow rate 73 is expanded in a valve 75 and sent to the head condenser 29 of the CO column. / CH 4 where it vaporizes to form the flow of carbon monoxide 43 which mixes with the overhead gas of the CO / CH column.
  • phase separator 79 A part of the liquid 77 of the head condenser 29 is sent to a phase separator 79. From the phase separator 79 is withdrawn a liquid 81 which is sent to the exchanger 21 which cools the intermediate withdrawals of the methane washing column, the liquid 81 vaporizes and the gas is returned to the phase separator 79. The gas 83 of the phase separator 79 is sent to the inlet of the compressor 51 with the gas 43.
  • the three columns 17, 27, 19 are all placed on the ground, which increases the grip (the footprint) on the ground.
  • the column 27 is raised to a sufficient height.
  • the CO / CH 4 column 27 is placed above the depletion column 19, the two columns having the same main axis.
  • the methane enriched liquid 33 of the column vessel 27 passes through a height H to arrive at the pump 36 and is at a higher pressure due to the hydrostatic pressure. Some of the liquid at the elevated pressure can be taken to serve as a product downstream or upstream of the pump 36. The footprint of the columns of the cold box is thus reduced.
  • the sum of the heights of both columns 27 and 19 is less than height of the column 17, the length of the packet of the columns of the cold box is not modified.
  • the liquid phase 18 of the bottom of the washing column 17 is sent to the depletion column 19.
  • the function of this column is to eliminate the Residual hydrogen still dissolved in carbon monoxide.
  • the depletion column comprises a few additional trays at the top of the column, constituting an auxiliary column 20 with reduced diameter compared to column 19.
  • the gas phase is backwashed with liquid methane 39 to extract the carbon monoxide still dissolved.
  • the liquid / vapor traffic in this section 20 is quite low: all the other gas flows entering the exhaust column 19 are located below section 20.
  • it is therefore justified to reduce the diameter in the upper section 20 of the depletion column: it then takes the name of "auxiliary column" (minaret).
  • the auxiliary column 20 fits about one meter in the exhaust column 19.
  • An innovation of the present invention consists in relocating the auxiliary column 20 of exhaust head, for example by fixing it on the side of the washing column 17. This relocation can be carried out elsewhere in the cold box (on a another column, for example, such as the second column 27 or a post-treatment column such as a denitrogenation column) as long as the auxiliary column 20 remains positioned under load on the lower part of the depletion column 19. idea can reduce both:
  • a mixture of hydrogen, carbon monoxide and methane 1 is purified in unit 3 to remove water and carbon dioxide.
  • the purified mixture cools in a main cryogenic exchanger 9 to be sent to a phase separator 7, where it is separated to form a hydrogen-enriched gas 11 and a methane-enriched liquid 13.
  • the liquid 13 is sent to the top of a depletion column 19 having a bottom reboiler 22.
  • the gas 21 withdrawn at the top of the column 101 is enriched in hydrogen and is heated in the exchanger 9 for recovery as a gas purge to a fuel system in general ....
  • the bottom liquid 23 of column 19 contains mainly carbon monoxide and methane and is sent to separate in the column CO / CH 4 27.
  • a gas enriched in carbon monoxide is formed at the top of the column.
  • column and a methane enriched liquid 33 is formed in the bottom of the column. The liquid is heated in the exchanger to serve as fuel.
  • the liquid 33 is divided in two, a part 37 being reheated (or not) in the main cryogenic exchanger 9 for recovery as a purge gas (or in liquid form by short-circuiting the exchanger 9) at the pressure of the column CO / CH 4 (a few bars) and the other part 35 being pressurized by a pump 36 for possible upgrading under pressure (fluid 38) in gaseous form via the main cryogenic exchanger 9 (or directly in liquid form bypassing the exchanger 9).
  • a carbon monoxide cycle keeps the appliance cold.
  • Carbon monoxide from the top of the column 27 is heated in the exchanger 9, sent as flow 45 to a compressor 51. Part of the carbon monoxide is produced as pressurized gas at the outlet of the compressor. Another part 57 cools in exchanger 9 and is divided in two. A portion 59 at an intermediate temperature of the exchanger 9 is expanded in a turbine 61 and sent via a valve 63 via line 65 to the compressor 51. Another part 67 continues to cool in the exchanger 9. A fraction 69 of the cooled carbon monoxide serves to heat the reboiler 22 of the column 19 and is condensed. Another fraction 71 serves to heat the bottom reboiler 31 of the CO / CH 4 column 27 and is mixed with the condensed fraction 69. The entire flow rate 73 is expanded in a valve 75 and sent to the head condenser 29 of the CO column. / CH 4 where it vaporizes to form the flow of carbon monoxide 43 which will supply the compressor 51 after passing through the exchanger 9.
  • the column 27 is positioned above the column 19, which is itself positioned above the phase separator 7. it is also possible to place the phase separator 7 next to the two columns 101, 27.
  • a mixture of hydrogen, carbon monoxide, nitrogen and methane 1 is purified in unit 3 to remove water and dioxide of carbon.
  • the purified mixture cools in an exchanger 9 to be sent to a phase separator 7 where it is separated to form a hydrogen-enriched gas 11 and a methane-enriched liquid 13.
  • the gas 11 separates in a carbon monoxide washing column 601 fed at the top by a washing liquid 623 rich in carbon monoxide.
  • the bottom liquid of the column 601 is mixed with the liquid 13 to form the liquid 18 and the formed liquid is sent to the top of a depletion column 19 (in English "flash column") having a bottom reboiler 22.
  • the gas 21 withdrawn at the top of the column 19 is enriched in hydrogen and is heated in the exchanger 9 for recovery as a purge gas to a fuel system in general.
  • the vessel liquid 23 of the column 19 contains mainly carbon monoxide and methane and is sent to separate in the column CO / CH 4 27.
  • a gas enriched in carbon monoxide 43 is formed at the top of the column and a liquid enriched in methane 33 is formed in the bottom of the column.
  • the liquid 33 is divided in two, a part 37 being reheated (or not) in the main cryogenic exchanger 9 for recovery as a purge gas (or in liquid form by short-circuiting the exchanger 9) at the pressure of the column CO / CH 27 (a few bars) and the other part being pressurized by a pump 36 for possible upgrading under pressure (fluid 38), in gaseous form via the main cryogenic exchanger 9 (or directly in liquid form by short-circuiting the exchanger 9).
  • a carbon monoxide cycle keeps the appliance cold. Carbon monoxide from the top of the column 27 is heated in the exchanger 9, sent as flow 45 to a compressor 51. Part of the carbon monoxide is produced as pressurized gas at the outlet of the compressor. Another part 57 cools in exchanger 9 and is divided in two. A portion 59 is expanded in a valve 63 and then sent via line 65 to the compressor 51. Another part is divided into two fractions. A fraction 69 of the cooled carbon monoxide serves to heat the bottom reboiler 22 of the depletion column 19 and is condensed. Another fraction 71 serves to heating the bottom reboiler 31 of the column CO / CH 4 27 and is mixed with the condensed fraction 71.
  • the entire flow 73 is expanded in a valve and sent to the top condenser 619 of the column CO / CH 4 where it vaporizes to form the carbon monoxide fluid 43.
  • a carbon monoxide bath 29 at the top of the column 27 supplies the condenser 619 with gas to be condensed.
  • the overhead gas 635 of the column 27 is sent to the denitrogenation column 603 having a top condenser 615.
  • the tank liquid 613 of the denitrogenation column 603 is vaporizes in the head condenser 615 and is mixed with the fluid 43 to form the fluid 45 which is sent to the compressor 51 via the exchanger 9.
  • the nitrogen-enriched overhead gas 617 is heated in the exchanger 9 and directed to a network fuel.
  • the carbon monoxide necessary for washing in the column 603 is provided by the fluids 609 and 61 1 withdrawn at the discharge of the compressor 51. Part of these fluids is sent as flow 623 at the top of the washing column 601.
  • the establishment of a denitrogenation column may be applicable in all the cases mentioned above when the nitrogen must be partially or completely removed from the product gas.
  • the column CO / CH 4 27 is positioned above the exhaust column 19 so that the flow rich in liquid methane 35 is hydrostatically pressurized upstream of the pump 36.
  • Figure 8 shows a nitrogen washing process in which a mixture of hydrogen, carbon monoxide, nitrogen and methane 1 comes out of a Rectisol ® 804 type unit and is purified in a unit of purification 3 to remove water, methanol and CO 2 (adsorbing methanol or any other solvent used in an upstream washing may also be required in all the cases mentioned above).
  • the purified mixture 5 is cooled in the exchanger 9 and then sent to a phase separator 7.
  • the gas of the phase separator 7 is mixed with an uncooled portion 6 of the gas 5 to form the flow 1 1.
  • Part of the flow 1 1 is used to heat the bottom reboiler 851 of a column N 2 / CH 4 850, being partially condensed.
  • the partially condensed flow is sent to a phase separator 809.
  • the liquid 819 of the separator 809 is rich in methane and is sent to the pump 36.
  • the gas 827 of the separator 809 joins the gas 821 of the separator 7, is cooled in the exchanger 9, then separated in a phase separator 807 and the product gas 814 feeds the nitrogen washing column 81 1 to be separated.
  • the column 81 1 is fed at the top by a liquid flow 833 produced by the liquefaction of a flow rate 831 of nitrogen gas in the exchanger 9. Another portion 835 of the condensed nitrogen is mixed with the overhead gas 829 heated from column 81 1 containing hydrogen and sent to the extraction unit CO 2 / H 2 S (Rectisol ® for example) 804 for heat exchange; the formed gas 843 leaves the apparatus ..
  • the tank liquid 847 of the nitrogen wash column 81 1 is expanded and then sent to a phase separator 845.
  • the product gas 853 is heated in the exchanger 9 as a purge gas.
  • the liquid 849 feeds the N 2 / CH 4 850 column to form a gas flow 852 depleted of methane and enriched in nitrogen and a liquid flow enriched in methane.
  • the liquid flow enriched with methane 35 is sent to the pump 36, then feeds a phase separator 821.
  • the gas 825 is sent to the exchanger 9 to produce a gaseous phase rich in methane.
  • the liquid 823 can also be sent to the exchanger 9 to produce a phase rich in methane gas under pressure, or bypass the exchanger 9 to produce liquid methane under pressure as the final product. It is also possible to produce a phase rich in methane gas or liquid at low pressure by vaporizing liquid taken upstream of the pump 36.
  • the column N 2 / CH 4 850 is disposed above the scrubbing column with nitrogen 81 1.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Gas Separation By Absorption (AREA)
EP13727260.5A 2012-05-31 2013-05-06 Vorrichtung und verfahren zur kryogenen trennung einer mischung aus kohlenmonoxid und methan plus wasserstoff und gegebenenfalls stickstoff Active EP2856050B1 (de)

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PL13727260T PL2856050T3 (pl) 2012-05-31 2013-05-06 Urządzenie i sposób kriogenicznego rozdzielania mieszaniny tlenku węgla i metanu oraz wodoru i opcjonalnie azotu

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FR1255063A FR2991442B1 (fr) 2012-05-31 2012-05-31 Appareil et procede de separation cryogenique d'un melange de monoxyde de carbone et de methane ainsi que d'hydrogene et/ou d'azote
PCT/FR2013/051003 WO2013178901A2 (fr) 2012-05-31 2013-05-06 Appareil et procédé de séparation cryogénique d'un mélange de monoxyde de carbone et de méthane ainsi que d'hydrogène et/ou d'azote

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FR3052159B1 (fr) * 2016-06-06 2018-05-18 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et installation pour la production combinee d'un melange d'hydrogene et d'azote ainsi que de monoxyde de carbone par distillation et lavage cryogeniques
US11137204B2 (en) * 2016-08-25 2021-10-05 Praxair Technology, Inc. Process and apparatus for producing carbon monoxide
FR3057942B1 (fr) * 2016-10-21 2019-12-27 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation cryogenique d’un gaz de synthese par condensation partielle
SG11202008918SA (en) 2018-03-21 2020-10-29 Air Liquide Method and appliance for separating a synthesis gas by cryogenic distillation
FR3079288B1 (fr) * 2018-03-21 2020-05-22 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de separation d'un gaz de synthese par distillation cryogenique
CN108332510A (zh) * 2018-03-22 2018-07-27 上海华林工业气体有限公司 一种提高HyCO冷箱CO回收率的系统及方法
FR3089429B1 (fr) * 2018-12-11 2021-06-18 Air Liquide Procédé et appareil de purification d’un gaz riche en d’hydrogène

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CN104769376A (zh) 2015-07-08
CN104769376B (zh) 2016-08-31
WO2013178901A3 (fr) 2015-10-29
FR2991442A1 (fr) 2013-12-06
EP2856050B1 (de) 2021-04-14
FR2991442B1 (fr) 2018-12-07
PL2856050T3 (pl) 2021-10-25
WO2013178901A2 (fr) 2013-12-05

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