US20210055047A1 - Method and appliance for separating a synthesis gas by cryogenic distillation - Google Patents

Method and appliance for separating a synthesis gas by cryogenic distillation Download PDF

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US20210055047A1
US20210055047A1 US16/982,846 US201916982846A US2021055047A1 US 20210055047 A1 US20210055047 A1 US 20210055047A1 US 201916982846 A US201916982846 A US 201916982846A US 2021055047 A1 US2021055047 A1 US 2021055047A1
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column
gas
liquid
withdrawn
carbon monoxide
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Bertrand Demolliens
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Priority claimed from FR1852439A external-priority patent/FR3079288B1/fr
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Publication of US20210055047A1 publication Critical patent/US20210055047A1/en
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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
    • F25J3/0257—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
    • 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
    • F25J2200/74—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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
    • 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
    • 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
    • F25J2270/24—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
    • F25J2270/88—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
    • F25J2270/902—Details about the refrigeration cycle used, e.g. composition of refrigerant, arrangement of compressors or cascade, make up sources, use of reflux exchangers etc.

Definitions

  • the present invention relates to a process and to a device for the separation of a synthesis gas by cryogenic distillation.
  • Synthesis gas contains, as major components, hydrogen, methane and carbon monoxide. It can also contain nitrogen.
  • the first column carries out a methane scrubbing in order to recover, at the bottom, a fraction rich in CO and in methane and, at the top, a fraction rich in hydrogen.
  • the second column or stripping column (flash column) is used to discharge the few percent of hydrogen contained in the liquid fraction of the first column.
  • Processes according to the preamble of claim 1 are known from WO2013/178901 and EP 317 851. According to these processes of the prior art, the overhead gas from the stripping column is cooled by means of a dedicated exchanger present in the column or of an auxiliary column associated with the methane scrubbing column.
  • the present invention makes it possible to improve the performance qualities, by using existing scrubbing column equipment with intermediate gas cooling.
  • the idea of the invention is to cool and to at least partially condense a gas withdrawn in an upper part of the stripping column in an exchanger where at least one intermediate gas of the methane scrubbing column is cooled and to return at least a part of the at least partially condensed gas therefrom to the upper part of the stripping column.
  • the stripping column comprises an upper part and a lower part, below the upper part.
  • the CO yield can be increased by approximately 0.5% to 1% compared to the case with the minaret.
  • This overhead gas from the stripping column can, for example, be cooled countercurrentwise with another fluid from the cold box, such as, for example, liquid CO.
  • the cooled synthesis gas is separated by a first means in order to produce a liquid depleted in hydrogen; the separation carried out by the first means consists of a stage of scrubbing in a scrubbing column with at least a part of the liquid enriched in methane withdrawn from a column for the separation of carbon monoxide and methane having an overhead condenser, the condenser being cooled by a carbon monoxide cycle, and
  • the liquid depleted in hydrogen is introduced into the upper part of a stripping column which also comprises a lower part,
  • a liquid is withdrawn at the bottom of the stripping column and sent to the separation column, a gas enriched in carbon monoxide and depleted in methane is withdrawn at the top of the separation column, a liquid depleted in carbon monoxide and enriched in methane is withdrawn at the bottom of the separation column and the gas enriched in carbon monoxide is heated by heat exchange with the synthesis gas from stage i) in order to form a product,
  • a gas withdrawn in the upper part of the stripping column is at least partially condensed and returned at least in part to the upper part of the stripping column, characterized in that the gas withdrawn in the upper part of the stripping column is at least partially condensed in a heat exchanger which also serves to cool at least one gas withdrawn from the scrubbing column, the heat exchanger also serving to heat a refrigerant.
  • an apparatus for the separation of a synthesis gas comprising hydrogen, carbon monoxide, methane and optionally nitrogen by cryogenic distillation comprising a heat exchanger, a first separation means which is a methane scrubbing column, a stripping column and optionally a column for the separation of carbon monoxide and methane, means for purifying the synthesis gas, means for sending the purified gas to be cooled in the heat exchanger to a cryogenic temperature, means for sending the cooled synthesis gas to the first means for producing a liquid depleted in hydrogen, means for introducing the liquid depleted in hydrogen into the upper part of the stripping column which also comprises a lower part, means for withdrawing a gas enriched in hydrogen at the top of the stripping column, means for withdrawing a liquid at the bottom of the stripping column, a second heat exchanger, means for sending there a gas withdrawn in the upper part of the stripping column and means for sending at least a part of the gas at least partially
  • the apparatus can also comprise:
  • FIG. 1 schematically illustrates a process using a phase separator, a methane scrubbing column, a stripping column and a column for the separation of carbon monoxide and methane.
  • FIG. 2 schematically illustrates a stripping column with a methane scrubbing section, a part of the liquid pressurized and sent to the top of the stripping column and another part being sent to the top of the scrubbing column.
  • FIG. 3 schematically illustrates a process that does not use a methane scrubbing column.
  • FIG. 1 shows a process using a phase separator 9 , a methane scrubbing column 15 , a stripping column 25 and a column for the separation of carbon monoxide and methane 45 , for example containing structured packings for the columns, and capable of operating at cryogenic temperatures.
  • the synthesis gas 1 containing carbon monoxide, methane and carbon monoxide is purified of water and/or of carbon dioxide in the purification unit 3 before arriving at the heat exchanger 7 , where it cools to a cryogenic temperature and partially condenses.
  • the two phases are separated in a phase separator 9 , in order to form a gas 11 enriched in hydrogen and a liquid depleted in hydrogen 13 .
  • the gas 11 is sent to the bottom of the methane scrubbing column 15 , which produces a gas 19 enriched in hydrogen which is heated in the exchanger. A part of this gas 19 serves to regenerate the purification unit 3 .
  • At least one intermediate gas 21 A, 21 B, 21 C withdrawn from the column 15 is cooled in a heat exchanger 23 by indirect heat exchange with a fluid of the process, in this instance the liquid 51 .
  • the bottom liquid 17 from the column 15 joins the liquid 13 from the separator 9 and the mixture 91 , containing between 1 mol % and 3 mol % of hydrogen, is sent to the top of a stripping column 25 .
  • An overhead gas 27 from the stripping column condenses at least partially in the heat exchanger 23 .
  • a part 31 at least of the at least partially condensed gas is returned at the top of stripping column 25 in order to provide reflux liquid.
  • the remainder 29 can heat up in the heat exchanger 7 against the synthesis gas 5 .
  • the refrigerant gas 27 which leaves to be cooled in the heat exchanger 23 will undergo an at least partial condensation therein.
  • partial condensations liquid and gas are created. It is possible that a part of the liquid created passes through another pipe 31 or else falls back via the pipe 27 from which the refrigerant gas to be cooled originates, to join the column 25 . In this second case, the pipe 31 is not necessary.
  • a liquid 33 taken at the bottom of the stripping column 25 cools in the exchanger 7 and is sent to the separation column 45 .
  • Another part of the same liquid 35 vaporizes in a bottom reboiler 37 and is returned at the bottom of the stripping column.
  • the separation column comprises several sections for separation by distillation and optionally a capacity 99 . It has a bottom reboiler 73 which serves to heat the bottom liquid 75 , the gas formed being returned to the bottom.
  • the bottom liquid 77 enriched in methane is divided into two.
  • a part 83 vaporizes in the exchanger 7 in order to form fuel.
  • the remainder 85 is pressurized by a pump 87 and is sent to the top of the scrubbing column 15 .
  • the overhead gas from the column 43 enriched in carbon monoxide is sent to a product compressor 57 , which produces a gas enriched in carbon monoxide 57 .
  • a part of the gas enriched in carbon monoxide 61 is cooled and is divided into two.
  • a part 65 is expanded in a turbine 67 in order to provide cold.
  • the expanded gas 89 is returned to the inlet of the compressor 57 .
  • the remainder of the gas 69 continues to cool in the exchanger 7 and serves to heat the reboilers 73 and 37 (flows 93 and 73 ).
  • the gas which has served for the reboiling is thus partially condensed and feeds, as flow 97 , the capacity 99 at the top of the separation column 45 .
  • the gas 41 from the capacity 99 feeds the compressor 57 .
  • the liquid 47 from the capacity 99 is sent to a phase separator 49 , the liquid 51 from the separator serves as refrigerant in the heat exchanger 23 in order to cool the intermediate gases 21 A, 21 B, 21 C as well as the overhead gas 27 from the stripping column.
  • the liquid 51 is thus vaporized and returned to the phase separator 49 , the gas 53 from which feeds the compressor 57 .
  • a liquid withdrawn from the separation section of the separation column can replace the liquid 47 or another liquid of the process.
  • the stripping column comprising a methane scrubbing section, a part of the liquid 85 pressurized by the pump 87 being sent to the top of the stripping column 25 and another part being sent, as for FIG. 1 , to the top of the scrubbing column 15 .
  • the gas 27 withdrawn from the stripping column 25 is taken at least one theoretical plateau below the top of the column.
  • the gas at least partially condensed in the exchanger 23 returns to the stripping column next to the withdrawal point and the gas rising in the upper part of the stripping column (scrubbing section 25 A) becomes more enriched in hydrogen, making it possible to reduce the number of theoretical plates required.
  • the invention also applies to the case where the process does not use a methane scrubbing column.
  • the first separation is carried out simply by partial condensation in the separator 9 .
  • the gas 11 is heated and the liquid depleted in hydrogen 13 is sent to the stripping column 25 .
  • the latter may or may not comprise a methane scrubbing section, as for FIG. 2 , according to requirements.
  • the methane scrubbing section 25 A is present and thus the gas 27 withdrawn from the stripping column is taken at an intermediate level, as for FIG. 2 .
  • the heat exchanger 23 is simplified and makes possible a heat exchange between two fluids alone, the gas to be cooled 27 and the liquid to be heated 51 .
  • the gas 27 is taken at the top of the column 25 .

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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)
US16/982,846 2018-03-21 2019-03-20 Method and appliance for separating a synthesis gas by cryogenic distillation Abandoned US20210055047A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR1852439 2018-03-21
FR1852439A FR3079288B1 (fr) 2018-03-21 2018-03-21 Procede et appareil de separation d'un gaz de synthese par distillation cryogenique
PCT/FR2019/050624 WO2019180374A1 (fr) 2018-03-21 2019-03-20 Procede et appareil de separation d'un gaz de synthese par distillation cryogenique

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US20210055047A1 true US20210055047A1 (en) 2021-02-25

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US16/982,846 Abandoned US20210055047A1 (en) 2018-03-21 2019-03-20 Method and appliance for separating a synthesis gas by cryogenic distillation

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US (1) US20210055047A1 (de)
EP (1) EP3769022A1 (de)
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CN (1) CN111886465B (de)
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KR20200135805A (ko) 2020-12-03
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CN111886465B (zh) 2022-06-24
WO2019180374A1 (fr) 2019-09-26
SG11202008918SA (en) 2020-10-29

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