WO2008064762A2 - Procédé et dispositif d'obtention de produits provenant d'un gaz de synthèse - Google Patents

Procédé et dispositif d'obtention de produits provenant d'un gaz de synthèse Download PDF

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Publication number
WO2008064762A2
WO2008064762A2 PCT/EP2007/009607 EP2007009607W WO2008064762A2 WO 2008064762 A2 WO2008064762 A2 WO 2008064762A2 EP 2007009607 W EP2007009607 W EP 2007009607W WO 2008064762 A2 WO2008064762 A2 WO 2008064762A2
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Prior art keywords
carbon monoxide
gas
hydrogen
stage
condensation
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PCT/EP2007/009607
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German (de)
English (en)
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WO2008064762A3 (fr
Inventor
Martin Lang
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Linde Aktiengesellschaft
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Priority to EP07819626A priority Critical patent/EP2095047A2/fr
Publication of WO2008064762A2 publication Critical patent/WO2008064762A2/fr
Publication of WO2008064762A3 publication Critical patent/WO2008064762A3/fr

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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
    • C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/506—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification at low temperatures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0252—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of hydrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/0228—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream
    • F25J3/0261—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream characterised by the separated product stream separation of carbon monoxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • F25J3/04—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 for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04527—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general
    • F25J3/04539—Integration with an oxygen consuming unit, e.g. glass facility, waste incineration or oxygen based processes in general for the H2/CO synthesis by partial oxidation or oxygen consuming reforming processes of fuels
    • 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
    • F25J3/04—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 for air
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
    • F25J3/04563—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating
    • F25J3/04587—Integration with a nitrogen consuming unit, e.g. for purging, inerting, cooling or heating for the NH3 synthesis, e.g. for adjusting the H2/N2 ratio
    • 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
    • C01B2203/02—Processes for making hydrogen or synthesis gas
    • C01B2203/025—Processes for making hydrogen or synthesis gas containing a partial oxidation step
    • 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
    • C01B2203/046—Purification by cryogenic separation
    • 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
    • C01B2203/0465—Composition of the impurity
    • C01B2203/047—Composition of the impurity the impurity being carbon monoxide
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F25J2205/04—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum in the feed line, i.e. upstream of the fractionation step
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/02—Recycle of a stream in general, e.g. a by-pass stream
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • 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
    • 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
    • F25J2270/24—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
    • F25J2270/90—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration
    • F25J2270/904—External refrigeration, e.g. conventional closed-loop mechanical refrigeration unit using Freon or NH3, unspecified external refrigeration by liquid or gaseous cryogen in an open loop

Definitions

  • the invention relates to a process for obtaining a carbon monoxide and a hydrogen product by cryogenic decomposition of a feed gas consisting predominantly of hydrogen (H 2 ) and carbon monoxide (CO) in a two-stage condensation process, wherein peak cooling for the second condensation stage by mixing an H 2 - rich fraction with liquid nitrogen (MN 2 ) is produced, and an apparatus for carrying out the method.
  • B. catalytic steam reforming or partial oxidation (POX) is produced from hydrocarbonaceous starting materials, such as natural gas, LPG, naphtha, heavy oil or coal, so-called synthesis gas, which for the most part consists of H 2 and CO, but also methane (CH 4 ) , Water (H 2 O), carbon dioxide (CO 2 ) and other components, such as. As nitrogen and argon contains. From the synthesis gas, CO and H 2 are obtained as products by purification and decomposition, which are widely used in industry.
  • Separation method is particularly useful for separation of synthesis gases produced by partial oxidation, since such gases are usually of high pressure and at the same time have high CO and low methane content.
  • the feed gas is cooled in indirect heat exchange against process streams to be heated so far that it comes to a partial condensation in which form a CO-rich, H 2 -containing liquid fraction and an H 2 -rich, CO-containing gas fraction, which subsequently in a Phase separator to be separated.
  • the CO-rich liquid fraction in the still H 2 and other substances are dissolved, is subsequently purified (H 2 -Strippung, methane separation) and delivered as a CO product.
  • the CO contained in the feed gas can only be obtained with a yield of about 90%.
  • an H 2 -containing stream is obtained, which has a purity of only about 90 mol%, and therefore can not be discharged as a product.
  • the condensation process either by one Membrane unit or extended by a condensation stage (two-stage condensation process).
  • the H 2 -rich, CO-containing gas fraction obtained by condensation is subjected to a wide treatment, wherein the carbon monoxide is largely separated and fed into the CO product; after separation of the carbon monoxide, the H 2 -rich gas fraction has the required purity of more than 95 mol%, which in some cases can be dispensed with a subsequent purification by pressure swing adsorption.
  • the H 2 -rich, CO-containing gas fraction obtained in the first condensation stage is further cooled against zuracemende process streams to form a second CO-rich, H 2 -containing liquid fraction and a second H 2 -rich, CO-containing gas fraction, the subsequently separated in a second phase separator.
  • the peak cold needed for the second condensation stage is generated in the prior art by the mixture of liquid nitrogen with a predominantly hydrogen gas fraction, including liquid nitrogen from the cryogenic process from the outside -. B. from a cryogenic air separation, in which the oxygen required for the POX is obtained - is supplied.
  • the invention is therefore based on the object to provide a method of the type mentioned and an apparatus for performing the method, which make it possible with lower operating costs than is possible in the prior art, from a synthesis gas, a hydrogen and a carbon monoxide product to create.
  • this object is achieved in that at least part (GN 2 ) of the MN 2 is produced from nitrogen supplied from the outside by cooling, condensation, and, preferably, subcooling against process streams to be heated within the two-stage condensation process, to the two-stage condensation process.
  • the invention is based on the experience that gaseous nitrogen can be produced much more cost-effectively compared to liquid nitrogen. By applying the method according to the invention thus corresponding reductions in operating, but also the investment costs in the air separator, achieved.
  • the two-stage condensation process is used to decompose synthesis gas produced by partial oxidation (POX) and the oxygen required for the POX is recovered in an air fractionator by the cryogenic separation of air, then the liquid nitrogen is conveniently obtained from that air fractionator ,
  • POX partial oxidation
  • an embodiment of the method according to the invention provides that the missing amount of nitrogen (LN 2 ) is liquid is supplied outside.
  • the quantitative ratio of GN 2 to LN 2 is expediently adjusted so that both the carbon monoxide product with the desired yield and the hydrogen product with the required purity, but without a cold excess, are produced.
  • GN 2 or / and LN 2 be obtained from an air fractionator in which oxygen is produced (for example in a POX) to produce the feed gas containing hydrogen and carbon monoxide.
  • medium or low pressure level GN 2 is withdrawn from the air separator to minimize the overall energy requirements of the process.
  • the invention further relates to an apparatus for carrying out a two-stage condensation process (gas decomposer) in which a feed gas consisting predominantly of hydrogen (H 2 ) and carbon monoxide (CO) can be decomposed into a carbon monoxide and a hydrogen product, wherein peak cooling for the second condensation stage of the gas decomposer by the mixture of an H 2 -rich fraction with liquid nitrogen (MN 2 ) is generated.
  • gas decomposer a feed gas consisting predominantly of hydrogen (H 2 ) and carbon monoxide (CO) can be decomposed into a carbon monoxide and a hydrogen product, wherein peak cooling for the second condensation stage of the gas decomposer by the mixture of an H 2 -rich fraction with liquid nitrogen (MN 2 ) is generated.
  • the gas decomposer comprises a device for producing at least part (GN 2 ) of the MN 2 , in which nitrogen which can be supplied in gaseous form from the outside by cooling against process streams to be heated is condensable and, preferably, subcoolable.
  • a gas separator usually has two series-connected heat exchangers, wherein the heat exchangers are plate heat exchangers and the cold side of the first heat exchanger is warmer than the warm side of the second heat exchanger.
  • the warm side of the first heat exchanger is connected via a line with a source of gaseous nitrogen, is supplied via the nitrogen gas in the first heat exchanger.
  • the heat exchangers is then carried out against heated process streams cooling, condensation and optionally a supercooling of the nitrogen.
  • the gas separator is equipped with a device on a subset of the MN 2 as liquid nitrogen (LN 2 ) from outside the gas separator can be fed.
  • a preferred embodiment of the device according to the invention provides that the gaseous nitrogen for generating G-N 2 or / and LN 2 are obtainable from an air separator, in which oxygen is produced for generating the feed gas containing hydrogen and carbon monoxide (for example in a POX) ,
  • this gaseous nitrogen from the air separator has a medium or low pressure level.
  • the process of the invention enables the cost of producing peak cold in the two-stage condensation process to be reduced and the economics of this separation process to be increased.
  • the embodiments are methods for producing a hydrogen and a carbon monoxide product from a hydrocarbon-containing feed.
  • the hydrocarbon-containing feed 1 is introduced into the POX reactor P together with the oxygen stream 2 obtained from the air fractionator LZ, where it is converted by partial oxidation into a synthesis gas 3 containing predominantly hydrogen (H 2 ) and carbon monoxide (CO).
  • a predominantly consisting of hydrogen and carbon monoxide feed gas 4 is obtained from the synthesis gas 3 by the substantial removal of undesirable substances such as water and carbon dioxide, which is then fed to the cryogenic separation unit Z.
  • a first two-phase mixture 5 is produced from the feed gas 4 by cooling and partial condensation against process streams to be heated in the two main heat exchangers E1 and E2, which in the phase separator D1 into a first H 2 -rich, CO-containing gas phase 6 and a first CO rich, H 2 -containing liquid phase 7 is separated.
  • the first H 2 -rich, CO-containing gas phase 6 is further cooled, wherein a part of the carbon monoxide contained in it condenses out and a second biphasic mixture 8 is formed, which in the phase separator D 2 in a second H 2 -rich, CO-containing gas phase 9 and a second CO-rich, H 2 -containing liquid phase 10 is separated.
  • the second CO-rich, H 2 -containing liquid phase 10 is continued after warming against cooling process streams in the heat exchanger E3 via line 11, via the throttle body a relaxed, together with the relaxed over the throttle body b first CO-rich, H 2 -containing liquid phase 7 via Passed line 12 to the H 2 -Strippkolonnen T1 and abandoned this at the head.
  • the H 2 -trip column T1 serves to remove the dissolved in the CO-rich stream 12 hydrogen.
  • a natural circulation evaporator (reboiler), which is integrated in the heat exchanger E2. From the bottom of the H 2 -trip column T1, a stream 13 is passed into the reboiler, partially evaporated there and returned via line 14.
  • the H 2 -rich, CO-containing overhead fraction 15 from the H 2 -trip column T1 is heated in the heat exchangers E2 and E1 and returned as so-called. Flash gas 16 via the gas purifier R in the process. If the gas purifier R is a Rectisol wash, the recycle compressor (not shown) installed there is preferably used for the recirculation.
  • the bottom fraction from the H 2 -Strippkolonnen T1 a predominantly carbon monoxide and nitrogen (N 2 ) containing mixture is withdrawn via line 17, expanded via the throttle body c and fed to the N 2 / CO separation column T2.
  • the N 2 / CO separation column T2 is heated directly via stream 18, which is carbon monoxide 19 having product purity, which is withdrawn from the CO compressor V after the medium-pressure section V2, cooled in the heat exchanger E1 against process streams to be heated, then via the Throttle d relaxed and fed directly into the column bottom.
  • the product purity having carbon monoxide fraction 27 from the bottom of the N 2 / CO separation column T2 is divided into two subsets 28 and 29, wherein the subset 28 relaxed via the throttle body g and the integrated into the N 2 / CO separation column T2 top condenser E5 its cooling is supplied while the subset 29, after a relaxation via the throttle body h, together with the vaporized in the head cooler E5 and withdrawn from the top of the N 2 / CO separation column T2 CO fraction 30 flows via the line 31 to the heat exchanger E2, from which it is warmed off withdrawn via line 32.
  • a small subset 33 branched off from the CO fraction 32 and passed in the bypass to the heat exchanger E1, wherein the size of the subset 33 is adjusted via the control element i.
  • the remaining portion 34 of the CO fraction 32 is heated in the heat exchanger E1, led on line 35 and after the union with the guided in the bypass subset 33 via line 36 as an intermediate feed to the CO compressor V abandoned.
  • a portion of the liquid carbon monoxide from the top of the N 2 / CO separation column T2 is withdrawn via line 20. After a relaxation to low pressure level via the throttle body e, it provides the peak cold at the heat exchanger E2, in which it is then evaporated. Via line 21, it is fed to the heat exchanger E1, there warmed and fed via line 22 to the suction side of the first section V1 of the CO compressor V.
  • the top fraction 23 from the N 2 / CO separation column T2, a N 2 / CO mixture, is expanded via the throttle body f and passed into the residual gas, which is passed via the lines 24 and 25 into the heat exchangers E1 and E2 and warmed there is before it is discharged via line 26 from the process.
  • the two product quality carbon monoxide fractions 22 and 36 are compressed in the compressor sections V1-V4 to product pressure and discharged at the plant boundary as CO product 37.
  • the gaseous nitrogen stream 39 which also serves for cooling recovery, is first cooled in the heat exchangers E1 and E2 and condensed and then subcooled in the heat exchanger E3, to which it is supplied via the line 41. Via line 42, the supercooled nitrogen is withdrawn from the heat exchanger E3 and, after relaxation to the pressure of the residual gas through the throttle member j, with a subset 43 of the H 2 fraction 9 from the separator D2 and via the throttle body k supplied liquid nitrogen stream 38th mixed.
  • the separator D2 can be operated at a temperature which makes it possible to deposit in the separator D2 a second H 2 -rich, CO-containing gas phase 9 with high purity (> 95 mol% H 2 ).
  • the main quantity 46 of the second H 2 -rich, CO-containing gas phase 9 is heated in the heat exchanger E 3 and then in the two heat exchangers E 2 and E 1, to which it is supplied via the lines 47 and 48, and delivered as hydrogen product 49 at the plant boundary.
  • the heated in the heat exchanger E3 N 2 / H 2 mixture 50 is performed together with the top fraction 23 from the N 2 / CO separation column T2 in the residual gas 26.
  • a second embodiment provides that a portion of the nitrogen stream 41 condensed in the heat exchangers E1 and E2 is used as reflux for the H 2 -tripping column T1 in order to reduce the CO content in the H 2 -rich top fraction.
  • this configuration can be dispensed with a return of the top fraction 16 from the H 2 - stripping T1. Instead, the top fraction 15 is discharged into the residual gas stream 24 or, if a particularly high H 2 yield is required, after subcooling in the heat exchanger E 3 instead of the partial stream 43 of the H 2 - rich fraction 9 from the separator D 2 with the two liquid nitrogen streams 38 and 42 mixed.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Separation By Low-Temperature Treatments (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

L'invention a pour objet un procédé d'obtention d'un produit renfermant du monoxyde de carbone (37) et de l'hydrogène (16), par décomposition cryogénique d'un gaz d'alimentation (1) principalement composé d'hydrogène (H<SUB>2</SUB>) et de monoxyde de carbone (CO) dans un processus de condensation en deux étapes, le froid maximum pour la seconde étape de condensation étant produit par le mélange d'une fraction riche en H<SUB>2</SUB> (43) avec de l'azote liquide (M-N<SUB>2</SUB>) (38, 42). L'invention a également pour objet un dispositif pour la mise en oeuvre de ce procédé. Le procédé selon l'invention est caractérisé en ce qu'au moins une partie (G-N<SUB>2</SUB>) (42) de M-N<SUB>2</SUB> est produite à partir de l'azote (39) envoyé à l'état gazeux, de l'extérieur, au processus de condensation en deux étapes, par refroidissement, condensation et, de préférence, sous-refroidissement, à l'encontre de courants de procédé à réchauffer, au sein du processus de condensation en deux étapes.
PCT/EP2007/009607 2006-11-30 2007-11-06 Procédé et dispositif d'obtention de produits provenant d'un gaz de synthèse WO2008064762A2 (fr)

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EP07819626A EP2095047A2 (fr) 2006-11-30 2007-11-06 Procédé et dispositif d'obtention de produits provenant d'un gaz de synthèse

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DE102006056642A DE102006056642A1 (de) 2006-11-30 2006-11-30 Verfahren und Vorrichtung zur Gewinnung von Produkten aus Synthesegas
DE102006056642.4 2006-11-30

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FR3018599A1 (fr) * 2014-03-17 2015-09-18 Air Liquide Procede et appareil de separation cryogenique d’un gaz de synthese contenant du monoxyde de carbone, du methane et de l’hydrogene

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CN103438666B (zh) * 2013-08-21 2015-05-20 张周卫 低温液氮用多股流缠绕管式主回热换热装备
DE102014015160A1 (de) 2014-10-14 2016-04-14 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Gewinnung von Kohlenmonoxid und Wasserstoff aus Synthesegas
FR3075067B1 (fr) * 2017-12-14 2020-08-28 Air Liquide Procede et appareil de separation cryogenique d'un gaz de synthese contenant une etape de separation de l'azote
CN110044133B (zh) * 2019-05-17 2024-03-22 成都赛普瑞兴科技有限公司 分离提纯一氧化碳的设备与方法
AU2023209587A1 (en) * 2022-01-24 2024-05-16 Topsoe A/S Effective use of cryogenic separation section in syngas manufacture

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US20050076672A1 (en) * 2002-06-13 2005-04-14 William Davey Plant unit and method for decomposing and purifying synthesis gas
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DE102005046790A1 (de) * 2005-09-29 2007-04-05 Linde Ag Verfahren zur Reinigung eines Gasgemisches

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GB1183866A (en) * 1966-09-30 1970-03-11 Air Liquide A Process for the Production of Ammonia Synthesis Gas
US4544390A (en) * 1983-02-14 1985-10-01 Exxon Research & Engineering Co. Cryogenic production of ammonia synthesis gas
US4917716A (en) * 1988-01-28 1990-04-17 Linde Aktiengesellschaft Process for purifying a gaseous mixture
US6070430A (en) * 1998-02-02 2000-06-06 Air Products And Chemicals, Inc. Separation of carbon monoxide from nitrogen-contaminated gaseous mixtures also containing hydrogen
US20020116944A1 (en) * 2000-12-18 2002-08-29 Mcneil Brian Alfred Process and apparatus for the separation of carbon monoxide and hydrogen for a gaseous from a gaseous mixture thereof
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DE102005046790A1 (de) * 2005-09-29 2007-04-05 Linde Ag Verfahren zur Reinigung eines Gasgemisches

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Publication number Priority date Publication date Assignee Title
FR3018599A1 (fr) * 2014-03-17 2015-09-18 Air Liquide Procede et appareil de separation cryogenique d’un gaz de synthese contenant du monoxyde de carbone, du methane et de l’hydrogene
WO2015140460A3 (fr) * 2014-03-17 2015-12-17 L'air Liquide, Societe Anonyme Pour L'etude Et L'exploitation Des Procedes Georges Claude Procédé et appareil de séparation cryogénique d'un gaz de synthèse contenant du monoxyde de carbone, du méthane et de l'hydrogène

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EP2095047A2 (fr) 2009-09-02
WO2008064762A3 (fr) 2009-04-23
CN101627273A (zh) 2010-01-13
DE102006056642A1 (de) 2008-06-05

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