WO2013078606A1 - Process and apparatus for the purification of hydrogen by cryogenic nitrogen wash and co-production of liquid methane - Google Patents

Process and apparatus for the purification of hydrogen by cryogenic nitrogen wash and co-production of liquid methane Download PDF

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Publication number
WO2013078606A1
WO2013078606A1 PCT/CN2011/083108 CN2011083108W WO2013078606A1 WO 2013078606 A1 WO2013078606 A1 WO 2013078606A1 CN 2011083108 W CN2011083108 W CN 2011083108W WO 2013078606 A1 WO2013078606 A1 WO 2013078606A1
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Prior art keywords
liquid
gas
methane
column
sending
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PCT/CN2011/083108
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French (fr)
Inventor
Alain Briglia
Antoine Hernandez
Ping REN
Frédéric Staine
Marie-Pascal Victor
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L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude
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Priority to PCT/CN2011/083108 priority Critical patent/WO2013078606A1/en
Publication of WO2013078606A1 publication Critical patent/WO2013078606A1/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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/52—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with liquids; Regeneration of used liquids
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/08—Production of synthetic natural gas
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0233—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
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    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0261—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon monoxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0276—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of H2/N2 mixtures, i.e. of ammonia synthesis gas
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04—Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0415—Purification by absorption in liquids
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/06—Integration with other chemical processes
    • C01B2203/068—Ammonia synthesis
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/02—Mixing or blending of fluids to yield a certain product
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/90—Processes or apparatus involving steps for recycling of process streams the recycled stream being boil-off gas from storage
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J2270/14—External 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
    • F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/60—Closed external refrigeration cycle with single component refrigerant [SCR], e.g. C1-, C2- or C3-hydrocarbons
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    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
    • F25J2290/34—Details about subcooling of liquids

Definitions

  • the present invention relates to a process and an apparatus for the purification of hydrogen by cryogenic nitrogen wash and co-production of liquid methane.
  • Ammonia synthesis units are fed with a stoichiometric mixture of hydrogen and nitrogen.
  • the hydrogen is produced from steam methane reforming, a partial oxidation reactor or coal gasification, for example.
  • the hydrogen may contain impurities, such an argon, carbon monoxide, carbon dioxide or oxygen, which may act as catalyst poisons for the ammonia.
  • a methane rich liquid contains at least 70% mol. methane. All the purities mentioned are molar purities.
  • the impure hydrogen produced in a steam methane reformer or a coal gasification is first treated to remove acid gases, then purified by adsorption to remove methanol, water or remaining carbon dioxide.
  • the hydrogen may then be treated by nitrogen washing in a cold box to produce the stochiometric mixture as described in GB-A-2192703.
  • the hydrogen contains between 1 % and 20% methane
  • the liquid phase can be separated to form a liquid rich in methane.
  • a process for co- production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising the steps of :
  • the feed gas may contain at least 70% hydrogen.
  • the feed gas may contain at most 99% hydrogen. It may contain at least 1 % methane. It may contain at most 20% methane. It may contain less than 4% carbon monoxide.
  • the hydrogen enriched gas is derived from the feed gas by carrying out a partial condensation of the feed gas by cooling the feed gas in a heat exchanger and sending the partially condensed fluid to a phase separator, removing the hydrogen enriched gas from the phase separator and removing a methane enriched liquid from the phase separator.
  • the methane enriched liquid is sent to an intermediate point of the stripping column.
  • the refrigeration for the process is provided by a closed refrigeration circuit.
  • an apparatus for co-production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising a liquid nitrogen wash column, a stripping column, a heat exchanger, an expansion valve, a conduit for sending feed gas or a hydrogen enriched gas derived therefrom to a liquid nitrogen wash column, a conduit for sending liquid nitrogen to the top of the liquid nitrogen wash column, a conduit for removing a mixture of nitrogen and hydrogen constituting an ammonia synthesis gas from the liquid nitrogen wash column, a conduit for sending a bottom liquid from the liquid nitrogen wash column to the top of the stripping column via the expansion valve and a conduit for removing methane rich liquid from the bottom of the stripping column as a final product.
  • the apparatus may comprise:
  • - a closed refrigeration circuit for supplying refrigeration to the heat exchanger and/or to the stripping column and/or a methane rich liquid subcooler.
  • the stripping column has a bottom reboiler, a conduit for sending a heating gas to the bottom reboiler, said heating gas being at least part of the feed gas or a gas circulating in the closed refrigeration circuit.
  • the means for liquefying gaseous nitrogen uses refrigeration provided by the closed refrigeration circuit.
  • the stripping column has a top condenser fed by the closed refrigeration circuit.
  • phase separator a phase separator, a conduit for sending the feed gas to the phase separator, a conduit for sending the hydrogen enriched gas from the phase separator to the liquid nitrogen wash column, a conduit for removing a methane enriched liquid from the phase separator and sending the methane enriched liquid from the phase separator to an expansion valve and a conduit for sending expanded liquid from the expansion valve to an intermediate point of the stripping column.
  • Figure 1 shows a cold box 33 contains heat exchangers 3, 59, columns 1 1 , 23 and closed cooling circuit 43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 77, 79.
  • a feed gas 1 containing from 70% to 99% of hydrogen, from 1 % to 20% of methane, less than 4% of CO is cooled in an exchanger 3 to form partially condensed feed gas 2 which is sent to a phase separator 5.
  • the gas 7 from the phase separator is sent to a liquid nitrogen wash column 1 1 and contains around 95% of H 2 , 3% of CO, 1 % of N 2 , 2% of CH 4 and less than 1 % of Ar.
  • the gas from the top of the column after being mixed with stream nitrogen 93 contains one part of hydrogen for three parts of nitrogen and can be used as an ammonia synthesis gas 99.
  • the gas 99 warms in exchanger 3 and then in exchanger 59 as stream 101 , part of the warming for partial stream 103 being provided by exchanger 105 of a RectisolTM unit.
  • the two stream 99, 103 are then reunited to form stream 105.
  • the liquid nitrogen for the column 1 1 is supplied in gaseous form 89, cooled and liquefied in exchangers 59, 3 and part 91 of the liquid is sent via a valve 97 to the top of column 1 1 .
  • the rest 93 may be mixed directly with gas 13 to ensure the composition is correct.
  • the liquid 9 from phase separator 5, containing between 70% and 90% methane, is expanded in valve 21 to a lower pressure and sent to an intermediate point of stripping column 23.
  • the top of column 23 is fed by the bottom liquid 15 of the nitrogen wash column, after expansion in valve 17.
  • Gas 107 from the top of the stripping column is removed as fuel gas and warmed in exchangers 3, 59.
  • the gas contains preferably around 70% CO, 15%f N 2 ,
  • Liquid methane 29 is produced at the bottom of column 23 and sent to exchanger 31 to be subcooled.
  • the subcooled liquid methane is removed from the cold box 33 in liquid form and sent to storage tank 37 by pump 35.
  • Boil off 39 from the storage is liquefied in exchanger 41 and sent back to the tank.
  • the liquid in the tank may be used to feed a network of liquid methane conduits.
  • the liquid methane may contain at least 70% mol. methane, preferably at least 90% mol. methane and traces of nitrogen and carbon monoxide (for example less than 0.5% carbon monoxide and less than 100ppm nitrogen).
  • Reboil for the column 23 may either be provided by at least part of the feed stream 95 or, as shown, by a closed refrigeration circuit including a stream 77 which flows into exchanger 25 to warm bottom liquid stream 27.
  • the closed refrigeration circuit may contain nitrogen, carbon monoxide, methane or another industrial gas.
  • the closed refrigeration circuit preferably supplies refrigeration to the heat exchanger 3 and/or to the heat exchanger 59, preferably to liquefy gaseous nitrogen for the wash column and/or to the stripping column 23 and/or a methane rich liquid subcooler 31 and/or to a cooler 41 for boil off gas 39 from the methane rich liquid storage 37.
  • the closed refrigeration circuit uses three compressors in series 61 , 65, 71 .
  • Gas 57 warmed in exchangers 3, 59 is compressed in compressor 61 and cooled in cooler 63. It is then mixed with stream 87, also warmed in the two exchangers.
  • the combined stream is compressed in compressor 65, cooled in cooler 67 and divided in two.
  • One part 69 is sent to booster compressor 71 and the boosted stream 73 is cooled in exchanger 59, then partially in exchanger 3 and expanded in turbine 55, coupled to booster 71 .
  • the expanded stream 73 is mixed with stream 51 to form stream 57.
  • the other part 75 is cooled in exchanger 59 and divided in two.
  • One part 77 is used to cool bottom reboiler exchanger 25 and cooled in exchanger 3.
  • the other part 79 is cooled in exchanger 3, expanded in valve 83 and mixed with part 79 of stream 77 after expansion in valve 81 .
  • the combined stream 85 is cooled in exchanger 3 to form stream 87 sent back to the inlet of compressor 65, after cooling in exchanger 59.
  • stream 77 Part of stream 77 forms stream 47 which is used in part (stream 49) to subcool the liquid methane in exchanger 31 and in part (stream 45 after expansion in valve 43) in exchanger 41 to cool the boil off gas 39.
  • the streams 45, 49 are mixed to form stream 51 after the two cooling steps and stream 51 is added to expanded stream 73 to form stream 57.
  • Figure 2 differs from Figure 1 in that the feed for column 1 1 is sent directly to the column and there is no longer any phase separator 5. Thus all the feed for the column 23 is constituted by the bottom liquid from column 15 via valve 17.
  • column 23 has a top condenser 24 fed by part 76 of the circuit stream 77 in which the top gas of column 23 is condensed.
  • the vaporized stream 76 may then be mixed with stream 57 (not shown to simplify the figure).
  • the stripping column 23 of Figure 1 could also have a top condenser.

Abstract

Process and apparatus are provided, which are used for co-production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70 mol% of hydrogen and at least 1 mol% of methane.

Description

PROCESS AND APPARATUS FOR THE PURIFICATION OF HYDROGEN BY CRYOGENIC NITROGEN WASH AND CO-PRODUCTION OF LIQUID METHANE
The present invention relates to a process and an apparatus for the purification of hydrogen by cryogenic nitrogen wash and co-production of liquid methane.
Ammonia synthesis units are fed with a stoichiometric mixture of hydrogen and nitrogen. The hydrogen is produced from steam methane reforming, a partial oxidation reactor or coal gasification, for example. The hydrogen may contain impurities, such an argon, carbon monoxide, carbon dioxide or oxygen, which may act as catalyst poisons for the ammonia.
In the context of this document, a methane rich liquid contains at least 70% mol. methane. All the purities mentioned are molar purities.
The impure hydrogen produced in a steam methane reformer or a coal gasification is first treated to remove acid gases, then purified by adsorption to remove methanol, water or remaining carbon dioxide.
The hydrogen may then be treated by nitrogen washing in a cold box to produce the stochiometric mixture as described in GB-A-2192703.
When the hydrogen contains between 1 % and 20% methane, it may be advantageous to separate a liquid phase from the hydrogen, as shown in Figure 1 , before sending it to the liquid nitrogen wash column. In this way, the liquid phase can be separated to form a liquid rich in methane.
According to an aspect of the invention, there is provided a process for co- production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising the steps of :
- sending the feed gas or a hydrogen enriched gas derived therefrom to a liquid nitrogen wash column,
- removing a mixture of nitrogen and hydrogen constituting an ammonia synthesis gas from the liquid nitrogen wash column,
- sending liquid from the bottom of the liquid nitrogen wash column to the top of a stripping column and,
- removing methane rich liquid from the bottom of the stripping column as a final product. The feed gas may contain at least 70% hydrogen. The feed gas may contain at most 99% hydrogen. It may contain at least 1 % methane. It may contain at most 20% methane. It may contain less than 4% carbon monoxide.
Other optional features include:
- the hydrogen enriched gas is derived from the feed gas by carrying out a partial condensation of the feed gas by cooling the feed gas in a heat exchanger and sending the partially condensed fluid to a phase separator, removing the hydrogen enriched gas from the phase separator and removing a methane enriched liquid from the phase separator.
- the methane enriched liquid is sent to an intermediate point of the stripping column.
- the refrigeration for the process is provided by a closed refrigeration circuit.
- gas from the top of the stripping column is removed as a fuel.
- liquefying gaseous nitrogen against at least one gas from the nitrogen wash column and/or the stripping column and/ or against a fluid of the closed refrigeration circuit.
- reboil for the stripping column is provided by the closed refrigeration circuit.
- gas at the top of the stripping column is cooled using a top condenser.
- cooling for the stripping column top condenser is provided by the closed refrigeration circuit.
- reboil for the stripping column is provided by the feed gas.
According to another aspect of the invention, there is provided an apparatus for co-production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising a liquid nitrogen wash column, a stripping column, a heat exchanger, an expansion valve, a conduit for sending feed gas or a hydrogen enriched gas derived therefrom to a liquid nitrogen wash column, a conduit for sending liquid nitrogen to the top of the liquid nitrogen wash column, a conduit for removing a mixture of nitrogen and hydrogen constituting an ammonia synthesis gas from the liquid nitrogen wash column, a conduit for sending a bottom liquid from the liquid nitrogen wash column to the top of the stripping column via the expansion valve and a conduit for removing methane rich liquid from the bottom of the stripping column as a final product. Optionally the apparatus may comprise:
- a closed refrigeration circuit for supplying refrigeration to the heat exchanger and/or to the stripping column and/or a methane rich liquid subcooler.
- where the stripping column has a bottom reboiler, a conduit for sending a heating gas to the bottom reboiler, said heating gas being at least part of the feed gas or a gas circulating in the closed refrigeration circuit.
- means for liquefying gaseous nitrogen and sending the liquefied gaseous nitrogen to the liquid nitrogen wash column.
- the means for liquefying gaseous nitrogen uses refrigeration provided by the closed refrigeration circuit.
- the stripping column has a top condenser fed by the closed refrigeration circuit.
- a phase separator, a conduit for sending the feed gas to the phase separator, a conduit for sending the hydrogen enriched gas from the phase separator to the liquid nitrogen wash column, a conduit for removing a methane enriched liquid from the phase separator and sending the methane enriched liquid from the phase separator to an expansion valve and a conduit for sending expanded liquid from the expansion valve to an intermediate point of the stripping column.
The invention will now be described in greater detail with reference to the figures which show processes according to the invention.
Figure 1 shows a cold box 33 contains heat exchangers 3, 59, columns 1 1 , 23 and closed cooling circuit 43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 77, 79.
A feed gas 1 containing from 70% to 99% of hydrogen, from 1 % to 20% of methane, less than 4% of CO is cooled in an exchanger 3 to form partially condensed feed gas 2 which is sent to a phase separator 5. The gas 7 from the phase separator is sent to a liquid nitrogen wash column 1 1 and contains around 95% of H2, 3% of CO, 1 % of N2, 2% of CH4 and less than 1 % of Ar. The gas from the top of the column after being mixed with stream nitrogen 93 contains one part of hydrogen for three parts of nitrogen and can be used as an ammonia synthesis gas 99. The gas 99 warms in exchanger 3 and then in exchanger 59 as stream 101 , part of the warming for partial stream 103 being provided by exchanger 105 of a Rectisol™ unit. The two stream 99, 103 are then reunited to form stream 105.
The liquid nitrogen for the column 1 1 is supplied in gaseous form 89, cooled and liquefied in exchangers 59, 3 and part 91 of the liquid is sent via a valve 97 to the top of column 1 1 . The rest 93 may be mixed directly with gas 13 to ensure the composition is correct.
The liquid 9 from phase separator 5, containing between 70% and 90% methane, is expanded in valve 21 to a lower pressure and sent to an intermediate point of stripping column 23. The top of column 23 is fed by the bottom liquid 15 of the nitrogen wash column, after expansion in valve 17.
Gas 107 from the top of the stripping column is removed as fuel gas and warmed in exchangers 3, 59. The gas contains preferably around 70% CO, 15%f N2,
8% H2, 2% CH4 and less than 1 % Ar.
Liquid methane 29 is produced at the bottom of column 23 and sent to exchanger 31 to be subcooled. The subcooled liquid methane is removed from the cold box 33 in liquid form and sent to storage tank 37 by pump 35. Boil off 39 from the storage is liquefied in exchanger 41 and sent back to the tank. The liquid in the tank may be used to feed a network of liquid methane conduits. The liquid methane may contain at least 70% mol. methane, preferably at least 90% mol. methane and traces of nitrogen and carbon monoxide (for example less than 0.5% carbon monoxide and less than 100ppm nitrogen).
Reboil for the column 23 may either be provided by at least part of the feed stream 95 or, as shown, by a closed refrigeration circuit including a stream 77 which flows into exchanger 25 to warm bottom liquid stream 27. The closed refrigeration circuit may contain nitrogen, carbon monoxide, methane or another industrial gas.
There is no mass transfer between the closed refrigeration circuit and the rest of the process.
The closed refrigeration circuit preferably supplies refrigeration to the heat exchanger 3 and/or to the heat exchanger 59, preferably to liquefy gaseous nitrogen for the wash column and/or to the stripping column 23 and/or a methane rich liquid subcooler 31 and/or to a cooler 41 for boil off gas 39 from the methane rich liquid storage 37.
The closed refrigeration circuit uses three compressors in series 61 , 65, 71 . Gas 57 warmed in exchangers 3, 59 is compressed in compressor 61 and cooled in cooler 63. It is then mixed with stream 87, also warmed in the two exchangers. The combined stream is compressed in compressor 65, cooled in cooler 67 and divided in two. One part 69 is sent to booster compressor 71 and the boosted stream 73 is cooled in exchanger 59, then partially in exchanger 3 and expanded in turbine 55, coupled to booster 71 . The expanded stream 73 is mixed with stream 51 to form stream 57.
The other part 75 is cooled in exchanger 59 and divided in two. One part 77 is used to cool bottom reboiler exchanger 25 and cooled in exchanger 3. The other part 79 is cooled in exchanger 3, expanded in valve 83 and mixed with part 79 of stream 77 after expansion in valve 81 . The combined stream 85 is cooled in exchanger 3 to form stream 87 sent back to the inlet of compressor 65, after cooling in exchanger 59.
Part of stream 77 forms stream 47 which is used in part (stream 49) to subcool the liquid methane in exchanger 31 and in part (stream 45 after expansion in valve 43) in exchanger 41 to cool the boil off gas 39. The streams 45, 49 are mixed to form stream 51 after the two cooling steps and stream 51 is added to expanded stream 73 to form stream 57.
Figure 2 differs from Figure 1 in that the feed for column 1 1 is sent directly to the column and there is no longer any phase separator 5. Thus all the feed for the column 23 is constituted by the bottom liquid from column 15 via valve 17.
To improve the methane purity, column 23 has a top condenser 24 fed by part 76 of the circuit stream 77 in which the top gas of column 23 is condensed. The vaporized stream 76 may then be mixed with stream 57 (not shown to simplify the figure). The stripping column 23 of Figure 1 could also have a top condenser.

Claims

1 . Process for co-production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising the steps of :
- sending the feed gas (1 , 95) or a hydrogen enriched gas (7) derived therefrom to a liquid nitrogen wash column (1 1 )
- removing a mixture of nitrogen and hydrogen constituting an ammonia synthesis gas from the liquid nitrogen wash column
- sending liquid (15) from the bottom of the liquid nitrogen wash column to the top of a stripping column (23) and,
- removing methane rich liquid (29) from the bottom of the stripping column as a final product.
2. Process according to Claim 1 wherein the hydrogen enriched gas (7) is derived from the feed gas (1 , 95) by carrying out a partial condensation of the feed gas by cooling the feed gas in a heat exchanger (3) and sending the partially condensed fluid to a phase separator (5), removing the hydrogen enriched gas from the phase separator (7) and removing a methane enriched liquid (9) from the phase separator.
3. Process according to Claim 2 wherein the methane enriched liquid (9) is sent to an intermediate point of the stripping column (23).
4. Process according to any preceding claim wherein the refrigeration for the process is provided by a closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 76, 77, 79).
5. Process according to any preceding claim wherein gas (107) from the top of the stripping column (23) is removed as a fuel.
6. Process according to any preceding claim comprising liquefying gaseous nitrogen against at least one gas from the nitrogen wash column (1 1 ) and/or the stripping column (23) and/or against a fluid of the closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 77, 79).
7. Process according to any preceding claim wherein reboil for the stripping column (23) is provided by the closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 76, 77, 79).
8. Process according to any preceding claim wherein reboil for the stripping column (23) is provided by the feed gas.
9. Apparatus for co-production of liquid methane and ammonia synthesis gas from a feed gas containing at least 70% mol. hydrogen and at least 1 % mol. methane comprising a liquid nitrogen wash column (1 1 ), a stripping column (23), a heat exchanger (3), an expansion valve (17), a conduit for sending feed gas (1 , 95) or a hydrogen enriched gas (7) derived therefrom to the liquid nitrogen wash column, a conduit for sending liquid nitrogen to the top of the liquid nitrogen wash column, a conduit for removing a mixture of nitrogen and hydrogen constituting an ammonia synthesis gas (99) from the liquid nitrogen wash column, a conduit for sending a bottom liquid (15) from the liquid nitrogen wash column to the top of the stripping column via the expansion valve and a conduit for removing methane rich liquid (29) from the bottom of the stripping column as a final product.
10. Apparatus according to Claim 9 comprising a closed refrigeration circuit (43,
45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 76, 77, 79) for supplying refrigeration to the heat exchanger (3) and/or to the stripping column (23) and/or a methane rich liquid subcooler (31 ).
1 1 . Apparatus according to any of Claims 9 to 10 wherein the stripping column has a bottom reboiler (25) and comprising a conduit for sending a heating gas to the bottom reboiler, said heating gas being at least part of the feed gas or a gas circulating in the closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 76, 77, 79).
12. Apparatus according to any of Claims 9 to 1 1 comprising means for liquefying gaseous nitrogen (89) and sending the liquefied gaseous nitrogen to the liquid nitrogen wash column (1 1 ).
13. Apparatus according to Claim 12 wherein the means for liquefying gaseous nitrogen (89) uses refrigeration provided by the closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75, 76,77, 79).
14. Apparatus according to any of Claims 9 to 13 wherein the stripping column
(23) has a top condenser (24) fed by the closed refrigeration circuit (43, 45, 49, 51 , 57, 55, 61 , 63, 65, 67, 69, 71 , 73, 75,76, 77, 79).
15. Apparatus according to any of Claims 9 to 14 including a phase separator (5), a conduit for sending the feed gas (1 , 95) to the phase separator, a conduit for sending the hydrogen enriched gas (7) from the phase separator to the liquid nitrogen wash column (1 1 ), a conduit for removing a methane enriched liquid (9) from the phase separator and sending the methane enriched liquid from the phase separator to an expansion valve (21 ) and a conduit for sending expanded liquid from the expansion valve to an intermediate point of the stripping column (23).
PCT/CN2011/083108 2011-11-29 2011-11-29 Process and apparatus for the purification of hydrogen by cryogenic nitrogen wash and co-production of liquid methane WO2013078606A1 (en)

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CN105157348A (en) * 2015-08-17 2015-12-16 杭州中泰深冷技术股份有限公司 Liquid nitrogen washing device for recycling LNG and method for liquid nitrogen washing device
CN109884218A (en) * 2019-04-12 2019-06-14 山东非金属材料研究所 The preparation facilities and method of arsine gas standard substance in a kind of nitrogen
CN114276846A (en) * 2021-12-16 2022-04-05 陕西黑猫焦化股份有限公司 Method and system for preparing LNG (liquefied Natural gas) and coproducing synthetic ammonia by using coke oven gas

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN105157348A (en) * 2015-08-17 2015-12-16 杭州中泰深冷技术股份有限公司 Liquid nitrogen washing device for recycling LNG and method for liquid nitrogen washing device
CN109884218A (en) * 2019-04-12 2019-06-14 山东非金属材料研究所 The preparation facilities and method of arsine gas standard substance in a kind of nitrogen
CN114276846A (en) * 2021-12-16 2022-04-05 陕西黑猫焦化股份有限公司 Method and system for preparing LNG (liquefied Natural gas) and coproducing synthetic ammonia by using coke oven gas
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