EP0081849B1 - Procédé et dispositif de séparation d'un gaz d'échappement de synthèse - Google Patents

Procédé et dispositif de séparation d'un gaz d'échappement de synthèse Download PDF

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Publication number
EP0081849B1
EP0081849B1 EP82111608A EP82111608A EP0081849B1 EP 0081849 B1 EP0081849 B1 EP 0081849B1 EP 82111608 A EP82111608 A EP 82111608A EP 82111608 A EP82111608 A EP 82111608A EP 0081849 B1 EP0081849 B1 EP 0081849B1
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Prior art keywords
nitrogen
compressor
pressure
separating
stage
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German (de)
English (en)
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EP0081849A3 (en
EP0081849A2 (fr
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Rainer Dipl.-Ing. Fabian
Wolfgang Dipl.-Ing. Schmid
Herwig Dipl.-Ing. Landes
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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
    • F25J3/0228—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
    • F25J3/028—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 noble gases
    • F25J3/0285—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 noble gases of argon
    • 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
    • F25J3/0219—Refinery gas, cracking gas, coke oven gas, gaseous mixtures containing aliphatic unsaturated CnHm or gaseous mixtures of undefined nature
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/30—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
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2210/20—H2/N2 mixture, i.e. synthesis gas for or purge gas from ammonia synthesis
    • 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
    • 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
    • F25J2270/04—Internal refrigeration with work-producing gas expansion loop
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S62/00—Refrigeration
    • Y10S62/931—Recovery of hydrogen
    • Y10S62/934—From nitrogen

Definitions

  • the invention relates to a process for the decomposition of synthesis exhaust gas in two successive separation stages with a nitrogen refrigeration cycle, in which nitrogen is compressed to an end pressure, cooled, further cooled by heating the two separation stages, expanded and partially liquefied, gaseous and re-evaporated liquid nitrogen again is compressed, and a device for performing the method.
  • Nitrogen from the top of the second separation stage and from a storage tank is compressed to 150 to 200 bar, cooled and partly relieved of work and used for the bottom heating of the second separation stage, and partly further cooled by heat exchange with the non-compressed nitrogen and for the bottom heating of the first Separation stage used.
  • the two partial flows are then expanded into the storage container in partially liquefied form.
  • Liquid nitrogen is removed from the storage container as washing liquid for the second separation stage and for head cooling of the first separation stage.
  • a part of the gaseous nitrogen is heated together with nitrogen from the head of the second separation stage in heat exchange with synthesis exhaust gas, while another part of the gaseous nitrogen is warmed up again in heat exchange with nitrogen for the heating of the first separation stage.
  • a part of the liquefied nitrogen, after it has been re-evaporated, is compressed again together with a part of the gaseous nitrogen.
  • Excess nitrogen is withdrawn from the system after heat exchange with the synthesis exhaust gas to be separated.
  • the present invention is therefore based on the object of providing a method of the type mentioned at the outset in which the high-pressure cooling circuit can be replaced by a medium-pressure cooling circuit without any energy losses.
  • This object is achieved in that a part of the nitrogen is already removed at a medium pressure below the final pressure and cooled in parallel with the nitrogen at the final pressure, further cooled by heating the two separation stages, partially liquefied and after with the nitrogen at the final pressure whose relaxation is combined.
  • part of the nitrogen is removed from an intermediate stage of the compressor.
  • Both nitrogen flows - both those at medium pressure and those at final pressure - are cooled together and used to heat the bottom of the first and second separation stages.
  • the two nitrogen streams are then depressurized and combined together in a partially liquefied state, the liquid nitrogen, as in the previously known process, partly being fed as washing liquid to the second separation stage and being used in part to cool the head of the first separation stage.
  • a nitrogen stream according to the invention is applied to a large extent lower pressure has been compressed, used for the bottom heating of both separation stages and at the same time another nitrogen stream, which is at an even lower pressure level, is used in parallel with the first nitrogen stream for bottom heating of the two separation stages.
  • the subject of the invention surprisingly makes it possible to drastically lower the final pressure of the nitrogen and still provide the cooling capacity required for the process.
  • the mean pressure is between 6 and 20 bar.
  • the mean pressure is preferably between 10 and 16 bar, in particular about 13.5 bar.
  • the final pressure is between 30 and 50 bar, preferably between 35 and 45 bar and in particular about 40.5 bar.
  • the specified pressure ranges for the medium pressure and the final pressure a sufficient cooling capacity for the process is achieved.
  • the respective pressure values depend on external ones Process conditions such as gas composition and gas pressure.
  • the pressures in the method according to the invention are in a pressure range which is significantly below the high pressures previously required for the refrigeration cycle.
  • plate heat exchangers can now be used with advantage instead of the previously used wound heat exchangers, which can be manufactured much more economically.
  • the nitrogen at the final pressure is still above the critical point and is therefore not liquefied when it cools down in the first separation stage, it is still cooled down over the steep part of the enthalpy curve when the first separation stage is heated. In this area, relatively small amounts of nitrogen are sufficient for the required heating output.
  • part of the compressed, cooled nitrogen is expanded while performing work and is fed to the gaseous fraction of the partially liquefied nitrogen.
  • the outlet pressure is advantageously chosen to be equal to the pressure of the re-evaporated nitrogen. If final pressure nitrogen is expanded while performing work, a higher outlet pressure is expediently set so that an optimal pressure drop is achieved on the expansion machine.
  • the nitrogen which has been relieved of work, is expanded to a pressure above the inlet pressure of the compressor and fed to the compressor at an intermediate point.
  • the pressure at the intermediate point is advantageously below the mean pressure of the nitrogen partial stream withdrawn from the compressor.
  • part of the nitrogen remaining in gaseous form after the expansion is heated together with nitrogen from the head of the second separation stage in heat exchange with synthesis exhaust gas and then admixed with the nitrogen stream to be compressed.
  • Part of the recompressed nitrogen is fed, for example, to the synthesis in this process.
  • part of the nitrogen liquefied during the expansion evaporate by cooling the first separation stage and be admixed with the nitrogen stream to be heated in the heat exchange with synthesis exhaust gas.
  • the nitrogen used to heat the first separation stage provides an intermediate pressure of between 5 and 20% of the total heating power required in the first separation stage.
  • the medium pressure nitrogen flow provides about 10% heating power.
  • the nitrogen used to heat the second separation stage provides an intermediate pressure of between 60 and 90% of the total heating power required in the second separation stage.
  • this medium pressure nitrogen flow provides about 75% of the heating power required.
  • the remaining heating power is supplied by the nitrogen at the final pressure.
  • a device for performing the method according to the invention comprises two series-connected separation columns and a nitrogen cooling circuit, which contains a compressor, a heat exchanger, reboiler in the sump of the two separation columns and a nitrogen storage container, the output of the compressor having the heat exchanger and its cold end is connected to the two reboilers, and the reboilers open on the outlet side into the storage container, and is characterized in that the compressor is designed at least in two stages, the outputs of the two compressor stages being separated from one another by the heat exchanger and the two reboilers and together in the Storage container open, and that the flow path for the nitrogen äus the first or second compressor stage is connected to an expansion machine.
  • the expansion machine is connected on the output side via a heat exchanger to a return line for gaseous nitrogen leading to the compressor.
  • a cooler in the head of the first separation column is connected on the inlet side to the nitrogen reservoir and on the outlet side to a further return line for gaseous nitrogen leading to the compressor.
  • a synthesis exhaust gas (purge gas) from ammonia synthesis has, for example, a composition of 31 mol% H 2 , 10 mol% N 2 , 19 mol% Ar and 40 mol% CH 4 . This gas mixture is to be broken down in order to To obtain synthesis gas and liquid argon.
  • the synthesis exhaust gas which is supplied at 1, has been freed of water and ammonia in a process step, not shown.
  • the synthesis exhaust gas is cooled to approximately 85 K in heat exchange with hydrogen product from the decomposition and a nitrogen refrigeration cycle, and is partially liquefied in the process.
  • the gaseous fraction which contains hydrogen with product purity (about 94.7 mol%), is withdrawn via the head of a downstream separator 3 and removed after heating in the heat exchanger 2.
  • the liquid fraction which contains almost all of the argon and methane and a large part of the nitrogen, is introduced via a line 4 into a first separation column 5 (methane column), from which a methane-free nitrogen-argon fraction (top side) and methane (bottom side) be removed.
  • the first separation column 5 is operated at a pressure of approximately 2.2 bar.
  • the methane (approx. 97 mol%) is removed via line 6 at a temperature of approximately 122 K.
  • the nitrogen-argon fraction is introduced via line 7 at about 89 K into a separation column 8 (argon column) operated at a pressure of about 2 bar, in which separation into nitrogen (top side) and argon product (bottom side) takes place.
  • the liquid argon runs through the second separation column 8 with approximately 94 K, the nitrogen with approximately 83.5 K.
  • the argon has a product purity of almost 100%, the nitrogen purity is approximately 94%.
  • a nitrogen refrigeration cycle is provided for performing the rectification in the separation columns 5, 8 and for generating refrigeration.
  • the nitrogen from the top of the second separation column 8 is partly passed (line 9) through the heat exchanger 2, in which it heats up with cooling of the synthesis exhaust gas, and is fed to the suction side of the first stage of a three-stage compressor 10.
  • the pressure at the compressor inlet is approximately 1.5 bar.
  • Another part of the nitrogen (line 11) is heated in heat exchangers 12, 13 in heat exchange with two nitrogen partial streams of the nitrogen cycle, which are still to be described, and then likewise fed to the first compressor stage.
  • a portion of the bottom liquid from the second separation column 8 is removed via a line 21, evaporated in the heat exchanger 12 and returned to the second separation column 8.
  • the nitrogen is compressed by a factor of 3 in each stage, i.e. to 4.5; 13.5 and finally to 40.5 bar.
  • the nitrogen compressed to the final pressure (line 15) is cooled in the heat exchanger 13 in heat exchange with the nitrogen stream 11 and with a further low-pressure nitrogen stream 19 to be described.
  • a refrigerant 14 provides additional cold.
  • Part of the nitrogen at the final pressure is cooled in a reboiler 16 in the bottom of the first separation column 5.
  • the nitrogen which is in the supercritical state, is guided over the steep part of the enthalpy curve (quasi-condensation). It then passes into the heat exchanger 12, in which it is subcooled, and is finally expanded into a nitrogen storage container 17, which is at a pressure of approximately 4.8 bar.
  • the remaining part of the nitrogen which is at the final pressure, is branched off from the heat exchanger 13 before the end of the heat exchange and expanded in a work-performing manner in a relaxation machine 18, its pressure rising from approx. 40 bar to approx. 5 bar and its temperature from approx. 132 K to approx 84 K lower. If required, part of the nitrogen at the final pressure is branched off via line 26 and used further, for example, as sealing gas for the compressor 10 or as synthesis gas.
  • the expanded in the expansion machine 18 nitrogen 19 is passed through part of the heat exchanger 12, in which it absorbs heat, further heated in the heat exchanger 13 and fed to the compressor 10 at an intermediate point, namely on the suction side of the second compressor stage.
  • a nitrogen stream is drawn from the compressor 10 at an intermediate point, which is at a mean pressure below the final pressure.
  • This medium-pressure nitrogen stream is withdrawn via line 20 at a pressure of 13.5 bar at the outlet of the second compressor stage and cooled in parallel with the nitrogen stream 15 under final pressure in the heat exchanger 13, further cooled in the reboiler 16, liquefied and supercooled in the heat exchanger 12 and finally also relaxed into the nitrogen reservoir 17.
  • the nitrogen streams 15 and 20 located at different pressure levels thus cover the heat requirement of the two separation columns 5, 8.
  • the majority of the heating power (approx. 90%) in the first separation column 5 is supplied by the nitrogen 15 at final pressure, while the larger one Share of the heating power in the second separation column 8 (approx. 75%) is supplied by the medium-pressure nitrogen 20.
  • Gaseous nitrogen 22 is removed from the storage container 17 and mixed with the work-relieved nitrogen 19 in front of the heat exchanger 12.
  • the liquid nitrogen 23 from the reservoir 17 is partially evaporated in a heat exchanger 27, for example in heat exchange with argon product (not shown), and fed to the gaseous nitrogen 9 in front of the heat exchanger 2.
  • the liquid nitrogen is fed on the one hand as a washing liquid to the second separation column 8 (line 24) and on the other hand through a cooler 25 in the head of the passed first separation column 5, in which it evaporates, and then also supplied in vapor form to the nitrogen stream 9.

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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)

Claims (12)

1. Procédé de séparation d'un gaz de synthèse dans deux étapes de séparation successives, utilisant un circuit d'azote de réfrigération, procédé dans lequel l'azote est comprimé à une finale, refroidi, puis refroidi à nouveau en assurant l'échauffement des deux étapes de séparation, détendu et partiellement liquéfié, cependant que l'on comprime à nouveau de l'azote gazeux et de l'azote qui a été vaporisé à partir de l'azote liquéfié, caractérisé en ce qu'une partie de l'azote (20) est retirée dès que celui-ci atteint une pression intermédiaire inférieure à la pression finale, en ce que cette partie d'azote est canalisée en parallèle avec l'azote (15) soumis à la pression finale, pour être refroidie, en ce qu'elle est refroidie davantage en assurant l'échauffement des deux étapes de séparation (5, 8), et en ce qu'elle est liquéfiée partiellement et réunie à l'azote (15) soumis à la pression finale, après une détente de ce dernier.
2. Procédé selon la revendication 1, caractérisé en ce que ladite pression intermédiaire est comprise entre 6 et 20 bars.
3. Procédé selon la revendication 1 ou 2, caractèrisè en ce que ladite pression finale est comprise entre 30 et 50 bars.
4.- Procédé selon une des revendications 1 à 3, caractérisé en ce qu'on détend, avec fourniture de travail, une partie de l'azote comprimé et refroidi et on l'ajoute à la phase gazeuse (22) de l'azote partiellement liquéfié.
5. Procédé selon la revendication 4, caractérisé en ce qu'on porte la pression de l'azote soumis à détente avec fourniture de travail, à une valeur supérieure à celle de la pression d'entrée du compresseur (10) et on l'introduit dans ce dernier en un point intermédiaire.
6. Procédé selon une des revendications 1 à 4, caractérisé en ce qu'une partie de l'azote resté en phase gazeuse (22) après la détente est réchauffée avec l'azote provenant de la tête, dans la deuxième étape de séparation (8), par échange de chaleur avec le gaz de synthèse (1), et est ensuite ajoutée au courant d'azote (9) à comprimer.
7. Procédé selon une des revendications 1 à 6, caractérisé en ce qu'une partie de l'azote (23) liquéfié lors de la détente est vaporisée par refroidissement dans la première étape de séparation (5) et ajoutée au courant d'azote (9) à réchauffer par échange de chaleur avec le gaz de synthèse (1).
8. Procédé selon une des revendications 1 à 7, caractérisé en ce que l'azote (20) soumis à la pression intermédiaire et l'azote utilisé pour l'échauffement, dans la première étape de séparation (5), fournit 5 à 20 % de la puissance calorifique totale requise pour l'échauffement dans la première étape de séparation.
9. Procédé selon une des revendications 1 à 8, caractérisé en ce que l'azote utilisé, sous pression intermédiaire, pour l'échauffement dans la deuxième étape de séparation (8), fournit 60 à 90 % de la puissance calorifique requise totale requise dans cette deuxième étape de séparation (8).
10. Dispositif pour la mise en oeuvre du procédé selon la revendication 1, comportant deux colonnes de séparation montées en série, ainsi qu'un circuit de refroidissement à azote comprenant un compresseur, un échangeur de chaleur, des bouilleurs dans la cuve des deux colonnes de séparation et un réservoir d'azote, cependant que la sortie du compresseur est reliée à l'échangeur de chaleur dont le côté froid est relié aux deux bouilleurs et que les sorties respectives desdits bouilleurs débouchent dans ledit réservoir, caractérisé en ce que ledit compresseur (10) comprend au moins deux étages, les sorties des deux étages de compresseur étant reliées séparément audit échangeur de chaleur (13) et aux deux bouilleurs, tout en débouchant ensemble dans ledit réservoir (17), et en ce que le trajet d'écoulement de l'azote sortant du premier ou du deuxième étage du compresseur est relié à une machine de détente (18).
11. Dispositif selon la revendication 10, caractérisé en ce que la machine de détente (18) est reliée, par sa sortie et par l'intermédiaire d'un échangeur de chaleur (12) à une conduite de recyclage (11, 19) d'azote gazeux qui débouche dans le compresseur (10).
12. Dispositif selon la revendication 10 ou 11, caractérisé en ce qu'un refroidisseur (25) disposé dans la tête de la première colonne de séparation (5) est reliée, par son entrée, audit réservoir d'azote (17) et, par sa sortie, à une autre conduite de recyclage (9) d'azote gazeux qui débouche dans ledit compresseur (10).
EP82111608A 1981-12-16 1982-12-14 Procédé et dispositif de séparation d'un gaz d'échappement de synthèse Expired EP0081849B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE19813149846 DE3149846A1 (de) 1981-12-16 1981-12-16 "verfahren und vorrichtung zur zerlegung von syntheseabgas"
DE3149846 1981-12-16

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EP0081849A2 EP0081849A2 (fr) 1983-06-22
EP0081849A3 EP0081849A3 (en) 1986-03-12
EP0081849B1 true EP0081849B1 (fr) 1987-07-01

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EP82111608A Expired EP0081849B1 (fr) 1981-12-16 1982-12-14 Procédé et dispositif de séparation d'un gaz d'échappement de synthèse

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US (1) US4473385A (fr)
EP (1) EP0081849B1 (fr)
DE (2) DE3149846A1 (fr)
IN (1) IN158298B (fr)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4689062A (en) * 1986-02-24 1987-08-25 The Boc Group, Inc. Argon recovery from ammonia plant purge gas utilizing a combination of cryogenic and non-cryogenic separating means
US4805414A (en) * 1987-12-15 1989-02-21 Union Carbide Corporation Process to recover hydrogen-free higher boiling synthesis gas component
US5289688A (en) * 1991-11-15 1994-03-01 Air Products And Chemicals, Inc. Inter-column heat integration for multi-column distillation system
US5685170A (en) * 1995-11-03 1997-11-11 Mcdermott Engineers & Constructors (Canada) Ltd. Propane recovery process
US5775128A (en) * 1997-05-02 1998-07-07 Praxair Technology, Inc. Process for producing ammonia and recovering argon using low purity oxygen

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1467202A1 (de) * 1963-03-21 1969-03-13 Linde Eismasch Ag Verfahren und Vorrichtung zur Regelung des Kaeltehaushaltes beim Herstellen von NH3-Synthesegas
GB1351598A (en) * 1970-03-26 1974-05-01 Air Prod & Chem Separation of gas mixtures
DE2814660A1 (de) * 1978-04-05 1979-10-11 Linde Ag Verfahren zur gewinnung von kohlenmonoxid und wasserstoff

Also Published As

Publication number Publication date
DE3276671D1 (en) 1987-08-06
DE3149846A1 (de) 1983-07-21
IN158298B (fr) 1986-10-11
EP0081849A3 (en) 1986-03-12
EP0081849A2 (fr) 1983-06-22
US4473385A (en) 1984-09-25

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