WO2017144151A1 - Procédé et dispositif de décomposition cryogénique d'un gaz de synthèse - Google Patents

Procédé et dispositif de décomposition cryogénique d'un gaz de synthèse Download PDF

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Publication number
WO2017144151A1
WO2017144151A1 PCT/EP2017/000090 EP2017000090W WO2017144151A1 WO 2017144151 A1 WO2017144151 A1 WO 2017144151A1 EP 2017000090 W EP2017000090 W EP 2017000090W WO 2017144151 A1 WO2017144151 A1 WO 2017144151A1
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Prior art keywords
separation column
feed gas
carbon monoxide
reboiler
liquid phase
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PCT/EP2017/000090
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German (de)
English (en)
Inventor
Martin Lang
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Linde GmbH
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Linde GmbH
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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
    • 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
    • F25J3/0261—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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/40—Features relating to the provision of boil-up in the bottom of a column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—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
    • 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
    • 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
    • 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
    • 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
    • F25J2270/02—Internal 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
    • F25J2270/12—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
    • F25J2270/24—Quasi-closed internal or closed external carbon monoxide 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
    • F25J2270/88—Quasi-closed internal refrigeration or heat pump cycle, if not otherwise provided
    • 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

Definitions

  • the invention relates to a method for the cryogenic decomposition of a predominantly consisting of hydrogen and carbon monoxide, methane-containing feed gas, which is partially condensed by cooling to a largely from
  • Carbon monoxide product allowed, as well as a largely consisting of methane and carbon monoxide bottom product can be obtained, wherein a, in a guided by a cyclic compressor driven cooling circuit refrigerant heat withdrawn and used to heat the CO / CH 4 separation column. Furthermore, the invention relates to a device for carrying out the
  • Synthesis gases are used, which are obtained by partial oxidation and therefore have a high carbon monoxide and a low methane content.
  • the condensation process makes it possible to produce a carbon monoxide product with a yield of more than 85%, which has a methane content of less than 100 vppm and which can therefore be used, for example, to produce monoethylene glycol without a further purification step ,
  • a cooling circuit driven by a cycle compressor in which either externally supplied nitrogen or internally generated Carbon monoxide circulates as refrigerant.
  • a cycle compressor for the carbon monoxide cycle, part of the process streams obtained in the CO / CH separation column and heated against the process streams to be cooled are heated
  • a nitrogen cycle is also used in the prior art to provide the peak cooling for the process and a reflux for the CO / CH 4 -
  • the respective cooling circuit comprises a reboiler called heat exchanger, through which the CO / CH column heat is supplied.
  • heat exchanger a reboiler
  • liquid from the bottom space of the column is warmed in the heat exchanger against the circulating in the cooling circuit coolant and partially evaporated and then discharged back into the column.
  • the bottom product of the CO / CH 4 column consists largely of methane and
  • Carbon monoxide wherein the carbon monoxide content is between 50 and 70 vol%. It is therefore not suitable for recycling and is released after evaporation and warming against cooling process streams as fuel gas.
  • Object of the present invention is therefore to provide a method of the generic type and an apparatus for its implementation, which allow the To reduce carbon monoxide content in the bottom product with respect to the prior art significantly reduced energy input.
  • this object is achieved in that heat is removed from at least part of the feed gas and used to heat the CO / CH 4 separation column.
  • the feed gas is preferably cooled in indirect heat exchange with a liquid which accumulates in the CO / CH 4 separation column and which partially evaporates during this process. While the resulting liquid-vapor mixture is subsequently discharged into the CO / CH 4 separation column, the cooled, but preferably not condensed feed gas is partially condensed in a further cooling step.
  • the feed gas is cooled against bottom product of the C07CH separation column, which is recycled after partial evaporation together with the vapor phase formed back into the bottom space.
  • the cooling circuit is operated stationary in time, so that it can not be used to keep in particular the temperature conditions in the CO / CH 4 separation column constant under changing operating conditions. It is therefore proposed to control the temperature conditions in the CO / CH 4 separating column with the aid of the amount of starting gas which is used for heating the CO / CH separating column.
  • Heating the CO / CH separation column via the cooling circuit also to warm the bottom product of the CO / CH 4 separation column.
  • the already pre-cooled, gaseous Refrigerant is cooled in indirect heat exchange with the liquid, the liquid partially evaporated, the refrigerant but its
  • the resulting liquid-vapor mixture is subsequently discharged into the bottom space of the CO / CH 4 separation column.
  • the refrigerant which is preferably nitrogen introduced from the outside or internally generated carbon monoxide, may either be cooled together with the feed gas therewith and / or independently of the feed gas to another liquid arising in the CO / CH 4 separation column. For example, it is possible to cool the feed gas to bottom product of the CO / CH 4 separation column, while for the cooling of the refrigerant one above the
  • the liquid to be withdrawn is collected in a chimney tray above the bottom space of the CO / CH 4 separation column.
  • a preferred embodiment of the method according to the invention further cools the refrigerant against at least a first part of the second liquid phase accumulating in the H 2 -stripping column is liquefied, wherein the evaporation of the liquid phase from the H 2 -Strippkolonne a first vapor phase is formed.
  • the liquefied refrigerant is subsequently used expediently for generating a reflux at the top of the CO / CH 4 separation column. At least a portion of the refrigerant is then further expanded to provide the peak cooling for the process.
  • Liquid phase which typically makes up about 5-10% of the total amount, relaxed and the CO / CH 4 separation column are abandoned as an intermediate reflux.
  • the inventive method allows a significantly lower temperature level of
  • the invention relates to a device for the cryogenic disassembly of a predominantly consisting of hydrogen and carbon monoxide, methane-containing feed gas with at least one heat exchanger for cooling and partial condensation of the feed gas, a separator in which a first liquid phase can be separated from the partially condensed feed gas, a H 2 stripping column in which a second liquid phase can be produced from the first liquid phase by separating off hydrogen, and a CO / CH separating column in which a carbon monoxide-rich gas phase with a purity permitting its release as carbon monoxide product from the second liquid phase and a bottom product largely consisting of methane and carbon monoxide are obtainable, wherein the CO / CH separation column is in communication with a reboiler, which is part of a driven by a cycle compressor cooling circuit and the one guided in the cooling circuit cold deprived of heat and the CO / CH 4 separation column
  • arranged reboiler is connected via which at least a portion of the feed gas can be performed to provide heat for heating the CO / CH 4 separation column.
  • the reboiler arranged in the flow path of the feed gas is preferably connected to the bottom space of the CO / CH 4 separation column, so that bottom product in the reboiler at least partially evaporates against the feed gas to be cooled and can subsequently be discharged into the bottom space from the CO / CH 4 separation column ,
  • a flow divider is arranged in the flow path of the feed gas upstream of the reboiler, via which the feed gas stream can be divided into a first and a second partial flow to lead the first via the reboiler and the second in the bypass to the reboiler.
  • the flow divider is made adjustable and incorporated into a control loop, via which the temperature conditions in the CO / CH separation column can be controlled by changing the size of the first partial flow.
  • the reboiler arranged in the path of the feed gas is also part of the cooling circuit, so that heat can be withdrawn via it to heat both the refrigerant and the feed gas for heating the CO / CH separating column.
  • the device according to the invention preferably comprises a condenser arranged downstream of the reboiler and connected to the H 2 -stripping column, in which the reboiler cooled but not liquefied refrigerant in indirect heat exchange against at least a portion of the second liquid phase from the H 2 -Strippkolonne can be condensed, wherein the inserted part of the second liquid phase completely evaporated.
  • the H 2 -tripping column is additionally connected directly to the heat exchanger used for the partial condensation of the feed gas and the CO / CH 4 separation column, so that a first part of the second liquid phase in the condenser and a second part in the partial condensation of the feed gas used heat exchanger evaporated and a third of the CG7CH 4 - separation column can be fed as intermediate reflux.
  • Heat exchangers usefully connected to the CO / CH 4 separation column so that they can be fed as the intermediate gas in the gas streams obtained in the evaporation of the second liquid phases.
  • the CG7CH separation column is connected to a first and a second reboiler, of which only the first is arranged in the flow path of the feed gas. It should not be excluded that the first reboiler is also part of the cooling circuit;
  • the CO / CH 4 separation column is designed in its lower region with a chimney tray arranged above the sump space and connected to the second reboiler such that liquid is withdrawn from the chimney tray and after at least partial evaporation against cooling and condensing refrigerant in the second reboiler above the Chimney tray can be returned to the CO / CH 4 - separating column.
  • the sections of the CO / CH 4 separation column above and below the chimney tray are interconnected by an overflow, so that liquid collecting in the chimney tray floor can be passed on to the lower section for further separation of carbon monoxide. It makes sense, the column section below the chimney tray due to the lower conversion met there with a smaller diameter than the section above the chimney tray.
  • a reboiler is designed as a plate heat exchanger or coiled heat exchanger and arranged either outside or inside the CO / CH 4 separation column.
  • the reboiler arranged in the flow path of the feed gas is designed as a coiled heat exchanger and arranged in the bottom space of the CO / CH 4 separation column.
  • FIG. 1 shows a variant of the invention in which the CO / CH 4 separating column is connected to only one reboiler.
  • Figure 2 shows another variant of the invention in which the CO / CH 4 separation column is connected to two reboilers.
  • a methane-containing feed gas 1 to be separated consisting predominantly of hydrogen and carbon monoxide and having a pressure between 30 and 60 bar (a) is cooled in a first heat exchanger E1 against process streams to be heated without condenser and subsequently into a first 2 and a second partial stream 3, of which the one 2 for heating the CO / CH 4 distillation column T2 in the reboiler R heat is withdrawn, wherein a further cooled, completely gaseous first partial stream 4 is formed, with the second, in the bypass to Reboiler R guided partial stream 3 to the feed stream 5 is combined.
  • the quantitative ratio of the two partial streams 2 and 3 can be varied.
  • the feed stream 5 is cooled to such an extent that a two-phase mixture 6 is formed by the condensation of components, which is separated in the separator D in a largely consisting of carbon monoxide and methane, hydrogen-containing liquid and a hydrogen-rich gas phase.
  • the gas phase is withdrawn via line 7 from the separator D and after heating in the heat exchangers E2 and E1 as raw hydrogen 8 at the
  • the liquid phase 9 is fed to the H 2 separation column T1.
  • it is split into two partial streams, of which the first 10 is relaxed as reflux to the top of the H 2 separation column T1, while the second partial stream 11 after a relaxation and subsequent partial evaporation in the
  • Heat exchanger E2 the center part of the H 2 separation column T1 is given as an intermediate heater.
  • the H 2 separation column T1 which is operated at a pressure which is between one fifth and one third of the pressure of the feed gas 1, is used for removal of the dissolved in the liquid phase 9 hydrogen. It is heated by a circulating heater 12, which is integrated in the heat exchanger E2.
  • the hydrogen-rich overhead fraction 13 from the H 2 separation column T1 is after
  • Carbon monoxide and methane existing bottoms fraction 15 is split into three partial streams 16, 17 and 18 and in the at a pressure between 5 and 9bar (a) operated CO / CH 4 separation column T2 is expanded.
  • the CG7CH 4 separation column T2 is heated via the reboiler R, in which bottom product 9 is at least partially vaporized.
  • the peak cooling required for the process is obtained via a refrigeration cycle driven by the cycle compressor V, which is designed with three stages C1, C2 and C3, in which carbon monoxide circulates as refrigerant.
  • Carbon monoxide 20 leaves the third compressor stage C3 with a pressure which is typically between 8 and 12 bar (a) is subsequently cooled in heat exchanger E1 and in the reboiler R, together with the first partial flow 2 of feed gas 1 to be warming the bottom product 19 of the CO / CH 4 Separation column T2 further cooled, without condensing.
  • the condenser E3 the cooled in the reboiler R Kohlemonoxid 21 against the partial flow 16, which is typically more than 45% of the amount
  • the condensed in the condenser E3 carbon monoxide 25 is divided into two partial streams 26 and 27, which are expanded to the top of the CO / CH 4 separation column T2. While the one part 26 serves as reflux, the liquid phase of the second part 27 is withdrawn in two carbon monoxide streams 28 and 29 again from the chimney tray K1 acting as a separator: While a liquid phase 28 with the gas phase 30 from the top of the CO / CH 4 separation column T2 to the carbon monoxide stream 31 is combined and supplied after evaporation and heating in the heat exchangers E2 and E1 of the third compressor stage C3, the second liquid phase 29 is further relaxed to provide the peak cooling for the process.
  • the resulting during the relaxation two-phase carbon monoxide stream 33 is subsequently also evaporated in the heat exchangers E2 and E1 and warmed before it is abandoned on the suction side of the cycle compressor V.
  • the compressed carbon monoxide on the exit side of the third compressor stage C3 is divided. Part is called
  • a methane-rich, carbon monoxide-containing liquid phase 34 collects, which can be discharged as fuel gas 35 after evaporation and heating in the heat exchangers E2 and E1.
  • the peak cooling required for the process is obtained via a refrigeration cycle driven by the cycle compressor V designed with two stages C ' and C2 ' in which nitrogen circulates as refrigerant.
  • Nitrogen 40 leaves the second compressor stage C2 ' with a pressure that
  • Separation column T2 ' is withdrawn nitrogen at medium pressure level in gaseous form via line 45 and liquid via lines 46 and 47.
  • the two nitrogen streams 45 and 46 are combined to nitrogen stream 48, which without further
  • nitrogen can be supplied to the closed nitrogen cycle via the low-pressure passage 49 from the outside, gaseous nitrogen 50 being introduced on the warm side of the heat exchanger E1 and liquid nitrogen 51 on the cold side of the heat exchanger E2. Excess nitrogen 52 is discharged on the pressure side of the cycle compressor V.
  • the chimney tray K is designed with an overflow U, passes through the liquid in the column below section and the bottom space S 'of the CO / CH - separation column T2 ' .
  • the sump space S ' is connected to a second reboiler R2, via which the first part stream 2 of the pre-cooled in the heat exchanger E1 feed gas 1 against liquid 53 from the sump space S ' heat for the heating of the CO / CH 4 -Trennkolonne T2 'is withdrawn, wherein the further cooled partial flow 4 is formed and the liquid 53 partially evaporated before it is returned to the sump space S ' .
  • This variant of the method makes it possible to lower the
  • Carbon monoxide content of the liquid phase 34 to values of less than 30Vol-% and thus also a significant increase in efficiency due to the lower amount of fuel gas 35.
  • Bottom fraction 15 from the H 2 separation column T1 is split into two partial streams 16 ' and 18 ' , of which the first 16 'is expanded, evaporated in the heat exchanger E 2 and subsequently passed as intermediate heating 24 ' into the CO / CH 4 separation column T2 ' ,
  • the partial stream 18 ' is also expanded into the CO / CH 4 separation column T2', where it serves as an intermediate reflux.

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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)

Abstract

L'invention concerne un procédé ainsi qu'un dispositif de décomposition cryogénique d'un gaz d'alimentation (1) constitué principalement d'hydrogène et de monoxyde de carbone et contenant du méthane, lequel gaz d'alimentation est condensé partiellement par refroidissement, afin d'obtenir une première phase liquide (9) constituée en grande partie de monoxyde de carbone et de méthane et contenant de l'hydrogène, première phase liquide à partir de laquelle une deuxième phase liquide (15) est produite dans une colonne de fractionnement H2 (T1) par séparation de l'oxygène, première phase liquide à partir de laquelle sont produits une phase gazeuse riche en monoxyde de carbone (31) présentant une pureté qui permet sa distribution en tant que produit de monoxyde de carbone (32), ainsi qu'un produit de fond (34) constitué en grande partie de méthane et de monoxyde de carbone, dans une colonne de séparation CO/CH4 (T2). De la chaleur est extraite d'un réfrigérant (20) guidé dans un circuit de refroidissement et entraîné par un compresseur de circuit (V), et utilisée pour chauffer la colonne de séparation CO/CH4 (T2). L'invention est caractérisée en ce que de la chaleur est extraite d'au moins une partie (2) du gaz d'alimentation (1) et est utilisée pour chauffer la colonne de séparation CO/CH4 (T2).
PCT/EP2017/000090 2016-02-25 2017-01-26 Procédé et dispositif de décomposition cryogénique d'un gaz de synthèse Ceased WO2017144151A1 (fr)

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DE102016002225.6A DE102016002225A1 (de) 2016-02-25 2016-02-25 Verfahren und Vorrichtung zur kryogenen Synthesegaszerlegung
DE102016002225.6 2016-02-25

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CN108332509A (zh) * 2018-03-22 2018-07-27 上海华林工业气体有限公司 一种开车时节省氮气用量的HyCO冷箱系统
WO2018151954A1 (fr) 2017-02-15 2018-08-23 Butts Properties, Ltd. Système et procédé de séparation de liquides de gaz naturel et d'azote de courants de gaz naturel
US20190368810A1 (en) * 2016-11-18 2019-12-05 L'air Liquide, Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Method and installation for cryogenic separation of a gaseous mixture by methane scrubbing
EP3783292A1 (fr) * 2019-08-20 2021-02-24 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de production de monoxyde de carbone par condensation partielle

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20190368810A1 (en) * 2016-11-18 2019-12-05 L'air Liquide, Societe Anonyme Pour I'etude Et I'exploitation Des Procedes Georges Claude Method and installation for cryogenic separation of a gaseous mixture by methane scrubbing
US11680747B2 (en) * 2016-11-18 2023-06-20 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Method and installation for cryogenic separation of a gaseous mixture by methane scrubbing
WO2018151954A1 (fr) 2017-02-15 2018-08-23 Butts Properties, Ltd. Système et procédé de séparation de liquides de gaz naturel et d'azote de courants de gaz naturel
EP3583368A4 (fr) * 2017-02-15 2020-06-10 Butts Properties Ltd. Système et procédé de séparation de liquides de gaz naturel et d'azote de courants de gaz naturel
US11125497B2 (en) 2017-02-15 2021-09-21 Bcck Holding Company System and method for separating natural gas liquid and nitrogen from natural gas streams
CN108332509A (zh) * 2018-03-22 2018-07-27 上海华林工业气体有限公司 一种开车时节省氮气用量的HyCO冷箱系统
EP3783292A1 (fr) * 2019-08-20 2021-02-24 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procede et appareil de production de monoxyde de carbone par condensation partielle
CN112410081A (zh) * 2019-08-20 2021-02-26 乔治洛德方法研究和开发液化空气有限公司 通过部分冷凝生产一氧化碳的方法和装置

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