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WO1997043207A1 - Purification de l'hydrogene - Google Patents

Purification de l'hydrogene Download PDF

Info

Publication number
WO1997043207A1
WO1997043207A1 PCT/GB1997/001267 GB9701267W WO9743207A1 WO 1997043207 A1 WO1997043207 A1 WO 1997043207A1 GB 9701267 W GB9701267 W GB 9701267W WO 9743207 A1 WO9743207 A1 WO 9743207A1
Authority
WO
WIPO (PCT)
Prior art keywords
accordance
catalyst
carbon monoxide
methanation
selective
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/GB1997/001267
Other languages
English (en)
Inventor
Robert Burch
Julia Margaret Evans
Michael Ian Petch
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Johnson Matthey PLC
Original Assignee
Johnson Matthey PLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Johnson Matthey PLC filed Critical Johnson Matthey PLC
Priority to AU27089/97A priority Critical patent/AU2708997A/en
Publication of WO1997043207A1 publication Critical patent/WO1997043207A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • C01B3/58—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction
    • C01B3/586—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction the reaction being a methanation reaction
    • 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
    • C01B3/56—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids
    • C01B3/58—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction
    • C01B3/583—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with solids; Regeneration of used solids including a catalytic reaction the reaction being the selective oxidation of carbon monoxide
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
    • H01M8/0662—Treatment of gaseous reactants or gaseous residues, e.g. cleaning
    • 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
    • C01B2203/0435—Catalytic purification
    • C01B2203/044—Selective oxidation of carbon monoxide
    • 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
    • C01B2203/0435—Catalytic purification
    • C01B2203/0445—Selective methanation
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • This invention relates to a method of and apparatus for the purification of gas streams containing hydrogen, carbon monoxide and carbon dioxide and more particularly but not exclusively relates to a method of and apparatus for the removal of carbon monoxide from reformate gas mixtures.
  • Fuel cell systems for vehicular application consist of either a tank of compressed gas that supplies a fuel cell with pure hydrogen, or an on-board hydrogen production unit followed by a hydrogen clean-up unit and a fuel cell.
  • a tank of compressed gas that supplies a fuel cell with pure hydrogen
  • a hydrogen clean-up unit for the hydrogen
  • the reformate gas mixture produced by such reforming of organic fuels contains hydrogen, carbon dioxide and
  • the concentration of carbon monoxide in the reformate gas mixture depends on such factors as the composition of the reactant feed, the temperature in the catalyst bed
  • anode catalyst of which can be poisoned by carbon monoxide levels as low as 40ppm.
  • the catalytic removal of carbon monoxide from a reformate is usually achieved in practice by a number of single step techniques. These include (i) the selective oxidation of the carbon monoxide to carbon dioxide; (ii) the reduction of the carbon monoxide with water vapour (water-gas shift) and (iii) the selective reduction of the carbon monoxide to methane (methanation).
  • Oxygen or air is added to the reformate and this must react with the carbon monoxide but not oxidise the hydrogen present, (eg see Oh and Sinkevitch,
  • 0533232 Al and 0650922 Al relate to processes for removing carbon monoxide from
  • the present invention relates to improvements in such processes.
  • the present invention provides a process for purifying a gas stream containing hydrogen, carbon monoxide and carbon dioxide comprising one or more oxidation stages wherein the carbon monoxide in the gas stream is oxidised to carbon dioxide in the presence of a selective oxidation catalyst so as to reduce the carbon monoxide concentration to no lower than lOOppm followed by selective methanation wherein the residual carbon monoxide in the gas stream is converted to
  • the methanation catalyst acts to selectively methanate carbon monoxide in preference to carbon dioxide.
  • the selective methanation may be carried out in one or more stages but
  • the concentration of carbon monoxide is lowered in the oxidation stage or stages of the process to between 4000 and lOOppm, preferably 500 and 400ppm and in the selective methanation to below lOppm.
  • the gas stream is a reformate gas mixture.
  • the oxidation is conducted by an oxygen-containing gas, eg air, the oxygen-containing gas being added to the gas stream prior to the oxidation stage or stages in an amount which gives an oxygen content in the gas stream between 2.5% to 3% by volume.
  • an oxygen-containing gas eg air
  • the oxygen-containing gas being added to the gas stream prior to the oxidation stage or stages in an amount which gives an oxygen content in the gas stream between 2.5% to 3% by volume.
  • the process of the invention is carried out in the presence of water vapour, the water vapour further preferably being added to the gas stream prior to the oxidation stage or stages in an amount which gives a water content in the gas stream of between 3% to 5% by volume.
  • the selective oxidation catalyst may be a supported noble metal catalyst in which the support material preferably is a substituted zeolite and the noble metal preferably is platinum or rhodium in an amount suitably between 1% to 5% by weight
  • Preferred selective oxidation catalysts for use in the process of the invention are 0.5% Pt/zeolite A - Na; 0.5% Pt/zeolite-H; 0.5% Pt/zeolite A - NaCa;
  • the selective methanation catalyst may be a supported noble metal catalyst in which the support material preferably is zirconia, silica, alumina or an alumino- silicate and the noble metal is preferably rhodium in an amount suitably between 0.1% to 5% by weight of the catalyst.
  • Preferred selective methanation catalysts for use in the process of the invention are 2% Rh/Al 2 O 3 , 2% Rh/SiO, and 2% Rh/ZrO 2 and 0.5% Rh/Al 2 O 3 .
  • the oxidation stage or stages preferably are carried out at a temperature between 180°C to 230°C, suitably 200°C to 220°C, and the methanation preferably is carried out at a temperature of between 200 °C to 240 °C.
  • the methanation is carried out at a temperature between 205 °C and 220 °C using 2%Rh/Al 2 O 3 as the selective methanation
  • the present invention also provides a multi-bed catalyst system for the purification of a gas stream containing hydrogen, carbon monoxide and carbon dioxide
  • Another aspect of the present invention is a fuel cell system for vehicular application comprising (a) an on-board hydrogen production unit; (b) a hydrogen clean ⁇ up unit and (c) a fuel cell wherein the hydrogen clean-up unit operates in accordance with the process of the invention as claimed herein.
  • Yet another aspect of the present invention is a fuel cell system for vehicular application comprising (a) an on-board hydrogen production unit; (b) a hydrogen clean-up unit and (c) a fuel cell wherein the hydrogen clean-up unit comprises a multi-bed catalyst system as described above.
  • the initial carbon monoxide concentrations in the gas stream are first decreased suitably to between 500ppm and 400ppm by selective oxidation to carbon dioxide.
  • the remaining carbon monoxide then is decreased suitably to below lOppm by selective catalytic
  • both the oxidation and reduction stages are run at their most efficient.
  • the oxidation stage can be run using a fixed amount of oxygen. Small fluctuations in the initial carbon monoxide concentration are not
  • the reduction stage will take care of a variable carbon monoxide input. Furthermore, the carbon monoxide input to the reduction stage is low enough for the hydrogen loss to be acceptable. As both the oxidation and reduction stages function at high gas space velocity, they contribute a relatively small extra volume. The total size of the multi-stage process needs to be no larger than 20% of the reformer volume.
  • a further advantage of the present invention is that both the oxidation and the reduction catalysts operate at similar temperatures which are compatible with the exit gas from a reformer. This negates the need for complex heat transfer systems.
  • the process and apparatus of the invention can be used for the purification of hydrogen in many other industrial applications, eg ammonia synthesis and methanol synthesis, chemical hydrogenations.
  • thermocouple inside each catalyst bed monitored its temperature, whilst each furnace
  • thermocouple connected to a Eurotherm programmable
  • a 20g batch of 0.5% Pt/zeoliteA-Na was prepared by dissolving a 0.2g
  • Zeolite powder sodium form of "4A"; 20g was added to the solution and left for 45 minutes.
  • the impregnated zeolite was dried at 120°C for 6 hours before being calcined in air at 500 °C for 2 hours.
  • the reactor containing 200mg of activated 2% Rh/Al 2 O 3 was connected downstream of a reactor containing 200mg of 0.5% Pt/zeoliteA-Na. In this arrangement
  • the product gas mixture from the bed of 0.5% Pt/zeoliteA-Na was made to pass through the bed of 2% Rh/Al 2 O 3 .
  • the outlet concentration of CO dropped to 8ppm at 205 °C to 220°C.
  • the 2%Rh/Al 2 O 3 catalyst can be used to attenuate up to 2400ppm of carbon monoxide down to 8ppm at an inlet temperature of 205 °C.
  • the nickel catalyst deactivated quickly. After 40 minutes, the exit CO concentration had risen from 30ppm to 240ppm.
  • a particulate form of 0.5% Pt/zeoliteA-Na was prepared by the method described in Example 1, except that pellets of zeolite "4A" (Na-form) were used.
  • Rh on extruded Al 2 O 3 was prepared by dissolving rhodium acetylacetonate (19.5mg per gram of catalyst) in dry toluene (1cm 3 per gram of catalyst). The particles of extrudate were then immersed in the solution and left for 5 days until they had become uniformly impregnated. After allowing the particles to dry at room temperature they were calcined in air at 400°C for 4 hours. Finally, the particles were activated in the same way as 2% Rh/Al 2 O 3 in Example 1.
  • Rhodium methanation catalysts are intrinsically more stable than conventional nickel methanation catalysts.
  • Rhodium catalysts have an optimum operational temperature window for achieving highly selective methanation of carbon monoxide.
  • Operational conditions can be determined for particular catalysts which allow an adiabatic methanation to be coupled with one or more selective oxidation stages to achieve carbon monoxide levels below lOppm.
  • Rh catalyst can be selected to match the output from the selective oxidation stage(s).
  • the gas stream emerging from the selected oxidation stage(s) can be cooled to match the required inlet temperature of the Rh-catalyst

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)

Abstract

L'invention concerne un procédé et un dispositif permettant de purifier un flux gazeux contenant de l'hydrogène, du monoxyde de carbone et du dioxyde de carbone. Selon le procédé, on soumet le monoxyde de carbone contenu dans le flux gazeux à une oxydation catalytique sélective en une ou plusieurs étapes, suivie d'une méthanation catalytique sélective, afin d'abaisser la quantité de monoxyde de carbone contenue dans le flux gazeux en dessous de 10 ppm. La méthanation se fait à l'intérieur d'une plage de températures dans laquelle le catalyseur de méthanation agit de façon à méthaner sélectivement le monoxyde de carbone, de préférence au dioxyde de carbone.
PCT/GB1997/001267 1996-05-11 1997-05-09 Purification de l'hydrogene Ceased WO1997043207A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU27089/97A AU2708997A (en) 1996-05-11 1997-05-09 Hydrogen purification

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
GBGB9609918.9A GB9609918D0 (en) 1996-05-11 1996-05-11 Hydrogen purification
GB9609918.9 1996-05-11

Publications (1)

Publication Number Publication Date
WO1997043207A1 true WO1997043207A1 (fr) 1997-11-20

Family

ID=10793590

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/GB1997/001267 Ceased WO1997043207A1 (fr) 1996-05-11 1997-05-09 Purification de l'hydrogene

Country Status (3)

Country Link
AU (1) AU2708997A (fr)
GB (1) GB9609918D0 (fr)
WO (1) WO1997043207A1 (fr)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0941963A1 (fr) * 1998-03-09 1999-09-15 Toyota Jidosha Kabushiki Kaisha Appareil pour reduire la concentration du monoxide de carbone et son procédé de commande
KR100286414B1 (ko) * 1996-09-24 2001-04-16 와다 아끼히로 일산화탄소 농도저감장치 및 일산화탄소 농도 저감방법
US6329091B1 (en) 2000-04-14 2001-12-11 Ford Global Technologies, Inc. Fuel reformer system for a fuel cell
EP1059118A3 (fr) * 1999-06-08 2002-06-26 Mitsubishi Heavy Industries, Ltd. Catalyseur à base de métal précieux déposé sur un silicate; son utilisation dans l'oxydation sélective du monoxide de carbone et dans la purification de l'hydrogène
EP1174486A4 (fr) * 1999-03-05 2002-07-24 Osaka Gas Co Ltd Systeme et procede de suppression du monoxyde de carbone
WO2002011869A3 (fr) * 2000-08-07 2002-11-28 Noritake Co Ltd Membranes a base de zeolithe, destinees a une oxydation selective de monoxyde de carbone, dans une source melangee contenant de l'hydrogene gazeux
EP1252678A4 (fr) * 2000-01-03 2003-07-16 Idatech Llc Systeme et procede de detection precoce d'impuretes dans un dispositif de traitement de combustible
US7118717B2 (en) 2002-09-06 2006-10-10 Engelhard Corporation Simplified article for carbon monoxide removal
US7560496B2 (en) 2005-01-24 2009-07-14 Basf Aktiengesellschaft Catalytically active composition for the selective methanation of carbon monoxide and method for producing said composition
US8395009B2 (en) 2007-02-23 2013-03-12 Basf Se Catalyst for selective methanization of carbon monoxide
EP3072589A1 (fr) 2015-03-26 2016-09-28 Basf Se Catalyseur et procédé de méthanisation sélective de monoxyde de carbone
CN113501497A (zh) * 2021-07-06 2021-10-15 湖北力拓能源化工装备有限公司 一种净化氢气的方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB882536A (en) * 1958-09-10 1961-11-15 Engelhard Ind Inc Improvements in or relating to treatment of gases
US3615164A (en) * 1968-01-10 1971-10-26 Bernard S Baker Process for selective removal by methanation of carbon monoxide from a mixture of gases containing carbon dioxide
EP0533232A1 (fr) * 1991-09-20 1993-03-24 METALLGESELLSCHAFT Aktiengesellschaft Méthode de production d'hydrogène à partir de gaz brut, obtenu par gazéification de carburants solides, liquides ou gazeux
EP0650922A1 (fr) * 1993-10-14 1995-05-03 Daimler-Benz Aktiengesellschaft Procédé d'élimination catalytique de CO d'un gaz riche en H2

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB882536A (en) * 1958-09-10 1961-11-15 Engelhard Ind Inc Improvements in or relating to treatment of gases
US3615164A (en) * 1968-01-10 1971-10-26 Bernard S Baker Process for selective removal by methanation of carbon monoxide from a mixture of gases containing carbon dioxide
EP0533232A1 (fr) * 1991-09-20 1993-03-24 METALLGESELLSCHAFT Aktiengesellschaft Méthode de production d'hydrogène à partir de gaz brut, obtenu par gazéification de carburants solides, liquides ou gazeux
EP0650922A1 (fr) * 1993-10-14 1995-05-03 Daimler-Benz Aktiengesellschaft Procédé d'élimination catalytique de CO d'un gaz riche en H2

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100286414B1 (ko) * 1996-09-24 2001-04-16 와다 아끼히로 일산화탄소 농도저감장치 및 일산화탄소 농도 저감방법
US6495113B2 (en) 1998-03-09 2002-12-17 Toyota Jidosha Kabushiki Kaisha Carbon monoxide concentration reducing apparatus and method for driving the same
EP0941963A1 (fr) * 1998-03-09 1999-09-15 Toyota Jidosha Kabushiki Kaisha Appareil pour reduire la concentration du monoxide de carbone et son procédé de commande
EP1174486A4 (fr) * 1999-03-05 2002-07-24 Osaka Gas Co Ltd Systeme et procede de suppression du monoxyde de carbone
EP1059118A3 (fr) * 1999-06-08 2002-06-26 Mitsubishi Heavy Industries, Ltd. Catalyseur à base de métal précieux déposé sur un silicate; son utilisation dans l'oxydation sélective du monoxide de carbone et dans la purification de l'hydrogène
US6482378B1 (en) 1999-06-08 2002-11-19 Mitsubishi Heavy Industries Selective removing method of carbon monoxide and hydrogen refining method
US7008708B2 (en) 2000-01-03 2006-03-07 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
US7368195B2 (en) 2000-01-03 2008-05-06 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
EP1252678A4 (fr) * 2000-01-03 2003-07-16 Idatech Llc Systeme et procede de detection precoce d'impuretes dans un dispositif de traitement de combustible
US6818335B2 (en) 2000-01-03 2004-11-16 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
US6329091B1 (en) 2000-04-14 2001-12-11 Ford Global Technologies, Inc. Fuel reformer system for a fuel cell
US7390347B2 (en) 2000-08-07 2008-06-24 Noritake Co., Ltd. Zeolite membranes for selective oxidation of carbon monoxide in mixed hydrogen gas source
WO2002011869A3 (fr) * 2000-08-07 2002-11-28 Noritake Co Ltd Membranes a base de zeolithe, destinees a une oxydation selective de monoxyde de carbone, dans une source melangee contenant de l'hydrogene gazeux
US7118717B2 (en) 2002-09-06 2006-10-10 Engelhard Corporation Simplified article for carbon monoxide removal
US7837953B2 (en) 2002-09-06 2010-11-23 Basf Corporation Simplified article for carbon monoxide removal
US7560496B2 (en) 2005-01-24 2009-07-14 Basf Aktiengesellschaft Catalytically active composition for the selective methanation of carbon monoxide and method for producing said composition
US8395009B2 (en) 2007-02-23 2013-03-12 Basf Se Catalyst for selective methanization of carbon monoxide
US8796169B2 (en) 2007-02-23 2014-08-05 Basf Se Catalyst for selective methanization of carbon monoxide
EP3072589A1 (fr) 2015-03-26 2016-09-28 Basf Se Catalyseur et procédé de méthanisation sélective de monoxyde de carbone
WO2016151031A1 (fr) 2015-03-26 2016-09-29 Basf Se Catalyseur à base de ruthénium-rhénium et procédé de méthanisation sélective de monoxyde de carbone
US10780422B2 (en) 2015-03-26 2020-09-22 Basf Se Rhenium-doped catalyst and a method for the selective methanation of carbon monoxide
CN113501497A (zh) * 2021-07-06 2021-10-15 湖北力拓能源化工装备有限公司 一种净化氢气的方法

Also Published As

Publication number Publication date
AU2708997A (en) 1997-12-05
GB9609918D0 (en) 1996-07-17

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