EP3049741A2 - Verfahren und vorrichtung zur kryogenen trennung einer mischung mit mindestens kohlenstoffmonoxid, wasserstoff und stickstoff - Google Patents

Verfahren und vorrichtung zur kryogenen trennung einer mischung mit mindestens kohlenstoffmonoxid, wasserstoff und stickstoff

Info

Publication number
EP3049741A2
EP3049741A2 EP14796181.7A EP14796181A EP3049741A2 EP 3049741 A2 EP3049741 A2 EP 3049741A2 EP 14796181 A EP14796181 A EP 14796181A EP 3049741 A2 EP3049741 A2 EP 3049741A2
Authority
EP
European Patent Office
Prior art keywords
column
gas
enriched
hydrogen
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.)
Granted
Application number
EP14796181.7A
Other languages
English (en)
French (fr)
Other versions
EP3049741B1 (de
Inventor
Angela FERNANDEZ
Pascal Marty
Bhadri PRASAD
Marie-Pascal Victor
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
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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
Publication of EP3049741A2 publication Critical patent/EP3049741A2/de
Application granted granted Critical
Publication of EP3049741B1 publication Critical patent/EP3049741B1/de
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0655—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0204—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0257—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/0261—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
    • 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
    • F25J3/0295—Start-up or control of the process; Details of the apparatus used, e.g. sieve plates, packings
    • 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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0635—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation 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
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/066—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation 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
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/06—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation
    • F25J3/063—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream
    • F25J3/0665—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by partial condensation characterised by the separated product stream separation of carbon monoxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2235/60—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
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • 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 process and apparatus for cryogenic separation of a mixture containing at least carbon monoxide, hydrogen and nitrogen.
  • the nitrogen content is fluctuating
  • the condensers at the top of the columns CO / N 2 are of type "bath vaporizer”.
  • the condenser installed has de facto an excess of heat exchange surface leading to condense all of the mixture CO / N 2 bottom tank, which no longer allows to maintain the operating pressure of the column. It is no longer possible to maintain the purity of the CO to be produced and the risk of stopping the unit follows.
  • the mixture in liquid form is sent to the top of a depletion column where it separates to form a hydrogen-depleted liquid and a hydrogen-enriched gas and the hydrogen-depleted liquid or fluid derived from this liquid is sent to a denitrogenation column where it separates to form a carbon monoxide enriched liquid and a nitrogen enriched gas containing the majority of the nitrogen present in the mixture
  • a carbon monoxide-enriched gas is below a threshold, i) at least a portion of the gas is sent enriched with hydrogen from the exhaust column at an intermediate point of the denitrogenation column or
  • the fluid is derived from the hydrogen-depleted liquid by distillation in a separation column, at least a portion of the hydrogen-enriched gas from the exhaustion column is sent to an intermediate point of the column at the separation column the carbon monoxide enriched gas is discharged at the top of the separation column and a non-condensed gas is fed from a top condenser of the separation column to the denitrogenation column.
  • the mixture contains methane and the hydrogen-depleted liquid is sent to the separation column, the latter having a top condenser, a methane-enriched liquid being produced in the tank and a gas enriched with carbon monoxide. carbon being withdrawn at the top of the column. sending hydrogen-enriched gas to the separation column or the denitrogenation column is triggered by a nitrogen-enriched gas flow detector.
  • the sending of non-condensed gas in the condenser to the denitrogenation column is triggered by a nitrogen-enriched flow detector at the top of the denitrogenation column.
  • the separation column is decoupled in pressure from the denitrogenation column by a pressure detector on the carbon monoxide enriched gas at the top of the separation column.
  • the mixture is a bottom liquid of a methane wash column, the wash liquid from the bottom of the separation column.
  • the mixture is a liquid from a phase separator, according to variant i) the fluid derived from the hydrogen-depleted liquid is produced by relaxing the liquid in a valve.
  • an apparatus for the cryogenic separation of a mixture of carbon monoxide, hydrogen, and nitrogen and optionally methane comprising a depletion column, a denitrogenation column and optionally a separation column having an overhead condenser, a conduit for supplying the mixture, in liquid form at the top of the depletion column, a conduit for removing a hydrogen-depleted liquid connected to the depletion column, a conduit for removing a hydrogen-enriched gas from the depletion column, means for sending the depleted liquid to hydrogen or a fluid derived from this liquid at the denitrogenation column, a pipe for withdrawing a carbon monoxide enriched liquid from the denitrogenation column and a pipe for withdrawing a nitrogen-enriched gas from the head of the denitrogenation column, characterized in that it comprises means for sending at least a portion of the hydrogen enriched gas or fluid derived therefrom to the denitrogenation column.
  • the apparatus may include a separation column having an overhead condenser and wherein the means for supplying fluid derived from the hydrogen-enriched gas to the denitrogenation column comprises a conduit for supplying at least a portion of the hydrogen-enriched gas to an hydrogen-depleted liquid separation column, the conduit being connected to an intermediate point of the separation column and a conduit for supplying gas from the overhead condenser which has not condensed thereon to the denitrogenation column.
  • the apparatus may include a separation column having an overhead condenser, the conduit for removing the hydrogen depleted liquid from the depletion column being connected to the separation column, the conduit for removing a hydrogen enriched gas being connected to the separation column and comprising a carbon monoxide enriched gas outlet line at the top of the separation column and a pipe for sending a non-condensed gas from the head condenser (6) of the separation column to the denitrogenation column .
  • the apparatus may include means for detecting the nitrogen content of the mixture and / or nitrogen enriched gas and / or carbon monoxide enriched gas and means for controlling the flow rate of the at least a portion of the enriched gas. hydrogen or fluid derived from this gas sent to the denitrogenation column.
  • the apparatus may comprise means for sending at least a portion of the hydrogen-enriched gas to the separation column at an intermediate point of the separation column or to the denitrogenation column by a detector of the nitrogen content of the mixture and / or gas enriched with carbon monoxide and / or nitrogen enriched gas and / or a flow detector of the mixture and / or carbon monoxide enriched gas and / or nitrogen enriched gas.
  • the innovation of the present invention is to compensate for nitrogen reduction by importing a portion of the overhead gas from the column from exhaustion upstream of the CO / N 2 column to the CO / N 2 column: the overhead gas of the depletion column contains hydrogen, which makes it possible to increase the flow rate of incondensables directed towards the CO / N column 2 .
  • flow control means (FIC)
  • a mixture of carbon monoxide, nitrogen and hydrogen is cooled in an exchanger 9 and sent to a distillation column 1 (or separator pot).
  • a hydrogen-enriched overhead gas 12 exits at the top of the column 1 and heats up in the exchanger 9.
  • the tank liquid 13 is expanded and then sent to the top of a depletion column 2 heated in the tank by a reboiler 8.
  • the hydrogen enriched overhead gas 14 is heated in the exchanger 9 and then burned.
  • the tank liquid containing mainly nitrogen and carbon monoxide is expanded and sent to the middle of a denitrogenation column 4.
  • the tank liquor enriched in carbon monoxide is sent to the exchanger 18 where it is used to condensing the overhead gas from the denitrogenation column.
  • a nitrogen-enriched gas exits the column head.
  • valve of the pipe 26 opens and hydrogen-enriched gas is sent from the top of the depletion column to the denitrogenation column 4, preferably by mixing it with the gas formed by expanding the liquid of line 16 in a valve.
  • the mixture to be separated comprises nitrogen, hydrogen, methane and carbon monoxide. It is known to separate such a mixture by cryogenic distillation, using a CO / CH 4 separation column followed by a CO / N 2 separation column.
  • the incondensables (H 2 -N 2 ) of the CO / CH 4 column are not recovered: they are sent directly to the flare or to a fuel network
  • the innovation consists in offsetting the reduction of nitrogen by an import of overhead gas (which contains hydrogen) from the exhaustion column upstream of the CO / CH 4 column, to the CO / CH 4 column. then an import of incondensables from the CO / CH 4 column to the CO / N 2 column.
  • the flows of each of the new lines are controlled by a FIC.
  • the impure CO flow rate is controlled by a PIC added to the CO / CH 4 column in order to decouple the two operating pressures of the columns.
  • the incondensables at the head of column CO / N 2 are then directed to the fuel network via the purge line N 2 which passes through the exchange line.
  • a mixture of carbon monoxide, nitrogen, hydrogen and methane is cooled in an exchanger 9 and sent to a methane washing column 1 fed at the top with liquid methane 11 or a separator pot.
  • a hydrogen-enriched overhead gas 12 leaves at the top of column 1 and heats up in exchanger 9.
  • the tank liquid 13 is expanded and sent to the top of a depletion column 2 heated in the tank by a reboiler 8.
  • the hydrogen enriched overhead gas 14 is heated in the exchanger 9 and then burned.
  • the vessel liquid containing mainly methane and carbon monoxide is expanded and sent to the middle of a distillation column 3 having a vessel reboiler 7 and a head condenser 6.
  • An incondensable gas flow 22 has come out of this condenser 6.
  • a carbon monoxide enriched overhead gas 16 exits the column 3 and is sent to the denitrogenation column 4.
  • the tank liquid enriched in methane is pumped by the pump 5, divided in two. Part 20 vaporizes in the exchanger 9 and the remainder feeds the washing column 1 as flow 1 1.
  • a nitrogen-enriched gas 21 leaves the head of the column and a liquid 22 exits the carbon monoxide enriched tank.
  • the carbon monoxide vaporizes in the head condenser 18 which is a bath vaporizer.
  • each of the new lines 24, 26 are controlled by a detector of minimum nitrogen purity of the nitrogen purge 21 coming from the head of the column CO / N 2 4 in general after passing through the exchange lines. . It is therefore necessary to slightly raise the pressure of the column CO / CH 4 3 to be certain that the flow of incondensables will be directed towards the column CO / N 2 4.
  • the impure CO flow 16 is controlled by a pressure controller added to the CO / CH 4 column in order to decouple the two operating pressures of the columns.
  • Incondensables, including hydrogen, at the top of column CO / N 2 are then directed to a fuel network via nitrogen purge pipe 21 which passes through the exchange line.

Landscapes

  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
EP14796181.7A 2013-09-24 2014-09-23 Verfahren und vorrichtung zur kryogenen trennung einer mischung mit mindestens kohlenstoffmonoxid, wasserstoff und stickstoff Active EP3049741B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1359155A FR3011069B1 (fr) 2013-09-24 2013-09-24 Procede et appareil de separation cryogenique d'un melange contenant au moins du monoxyde de carbone, de l'hydrogene et de l'azote
PCT/FR2014/052368 WO2015044575A2 (fr) 2013-09-24 2014-09-23 Procede et appareil de separation cryogenique d'un melange contenant au moins du monoxyde de carbone, de l'hydrogene et de l'azote

Publications (2)

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DE102015016771A1 (de) * 2015-12-23 2017-06-29 Linde Aktiengesellschaft Verfahren und Vorrichtung zur kryogenen Zerlegung von Synthesegas
CN116518647B (zh) * 2023-04-11 2024-06-28 英德市西洲气体有限公司 一种一氧化氮气体中脱除氧化亚氮的装置及脱除方法

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IN160585B (de) * 1983-02-14 1987-07-18 Exxon Research Engineering Co
US4805414A (en) * 1987-12-15 1989-02-21 Union Carbide Corporation Process to recover hydrogen-free higher boiling synthesis gas component
FR2754541B1 (fr) * 1996-10-15 1998-12-24 Air Liquide Procede et installation pour la separation d'un melange d'hydrogene et/ou d'au moins un hydrocarbure et/ou d'azote et/ou d'oxyde de carbone
GB9800693D0 (en) * 1998-01-13 1998-03-11 Air Prod & Chem Separation of carbon monoxide from nitrogen-contaminated gaseous mixtures
FR2775276B1 (fr) * 1998-02-20 2002-05-24 Air Liquide Procede et installation de production de monoxyde de carbone et d'hydrogene
DE10226210A1 (de) * 2002-06-13 2004-01-08 Lurgi Ag Anlagenteil zur Zerlegung und Reinigung von Synthesegas
FR2916264A1 (fr) * 2006-12-21 2008-11-21 Air Liquide Procede de separation d'un melange de monoxyde de carbone, de methane, d'hydrogene et eventuellement d'azote par distillation cryogenique
FR2895067A1 (fr) 2007-01-09 2007-06-22 Air Liquide Procede integre de deux separations cryogeniques et appareil integre pour la mise en oeuvre du procede
FR2912207B1 (fr) 2007-02-01 2012-10-26 Air Liquide Procede et appareil de production de monoxyde de carbone par distillation cryogenique
FR2912206B1 (fr) * 2007-02-01 2015-05-29 Air Liquide Procede et appareil de production de monoxyde de carbone par distillation cryogenique
FR2930332A1 (fr) * 2008-04-18 2009-10-23 Air Liquide Procede et appareil de separation cryogenique d'un melange d'hydrogene et de monoxyde de carbone
US8640495B2 (en) * 2009-03-03 2014-02-04 Ait Products and Chemicals, Inc. Separation of carbon monoxide from gaseous mixtures containing carbon monoxide
US20100251765A1 (en) * 2009-04-01 2010-10-07 Air Products And Chemicals, Inc. Cryogenic Separation of Synthesis Gas
FR2953004B1 (fr) * 2009-11-24 2013-12-20 Air Liquide Procede de separation cryogenique d'un melange d'azote et de monoxyde de carbone

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WO2015044575A3 (fr) 2015-09-17
US20160245583A1 (en) 2016-08-25
EP3049741B1 (de) 2017-09-06
FR3011069B1 (fr) 2015-09-11
CN105745506B (zh) 2019-07-02
US10539365B2 (en) 2020-01-21
FR3011069A1 (fr) 2015-03-27
CN105745506A (zh) 2016-07-06
WO2015044575A2 (fr) 2015-04-02

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