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WO2009153079A1 - Procédé de fabrication d'un mélange gazeux contenant de l'hydrogène - Google Patents

Procédé de fabrication d'un mélange gazeux contenant de l'hydrogène Download PDF

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Publication number
WO2009153079A1
WO2009153079A1 PCT/EP2009/054520 EP2009054520W WO2009153079A1 WO 2009153079 A1 WO2009153079 A1 WO 2009153079A1 EP 2009054520 W EP2009054520 W EP 2009054520W WO 2009153079 A1 WO2009153079 A1 WO 2009153079A1
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WIPO (PCT)
Prior art keywords
zone
temperature
reactor according
catalyst
reactor
Prior art date
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Ceased
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PCT/EP2009/054520
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German (de)
English (en)
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WO2009153079A9 (fr
Inventor
Hans-Georg Anfang
Klaus Wanninger
Jürgen PAWLIK
Rainer Dippel
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.)
Sued Chemie AG
Viessmann Generations Group GmbH and Co KG
Original Assignee
Viessmann Werke GmbH and Co KG
Sued Chemie AG
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Application filed by Viessmann Werke GmbH and Co KG, Sued Chemie AG filed Critical Viessmann Werke GmbH and Co KG
Priority to EP09765659A priority Critical patent/EP2285738A1/fr
Publication of WO2009153079A1 publication Critical patent/WO2009153079A1/fr
Anticipated expiration legal-status Critical
Publication of WO2009153079A9 publication Critical patent/WO2009153079A9/fr
Ceased legal-status Critical Current

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    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a method and a reactor for producing a hydrogen-containing gas mixture, in particular for use in fuel cells.
  • Today's fuel cells are operated with hydrogen, wherein at the anode, a reaction of hydrogen to protons and electrons and at the cathode takes place a reduction reaction of oxygen by means of protons and electrons to water.
  • the protons pass through a polymer electrolyte membrane (PEM).
  • PEM polymer electrolyte membrane
  • PEM fuel cells are very sensitive to carbon monoxide. Their sensitivity is based on the adsorption of CO at the active sites of the anode catalyst (platinum). This adsorption has the consequence that the rate of conversion of the hydrogen and consequently the cell voltage and, as a result, the electrical efficiency of the fuel cells decrease.
  • the hydrogen-containing fuel for fuel cells can be obtained by reforming natural gas or other hydrocarbons such as methane, LPG (liquefied petroleum gas), gasoline, diesel, alcohols or similar hydrocarbons.
  • LPG liquefied petroleum gas
  • gasoline diesel
  • alcohols alcohols or similar hydrocarbons.
  • the two reactions which are generally (and also within the scope of the present invention) used for the conversion of hydrocarbons into hydrogen can be described, for example, by means of methane by the following reaction equations:
  • ATR autothermal reforming reaction
  • CO fine purification stages such as the so-called CO methanation reaction (Selmeth) or CO oxidation (Selectox) are used, which can be described by the following reaction equation:
  • reformer concepts for producing fuel for PEM fuel cells typically consist of the following components:
  • WO 2003/080505 A1 describes a device for generating hydrogen with a steam reforming stage, at least one downstream catalytic conversion stage and a subsequent fine purification stage.
  • DE 100 57 537 A1 describes an apparatus for generating hydrogen for operating fuel cells, which has a reformer, two WGS stages and a selective oxidation stage with a graduated temperature profile. Overall, therefore, four catalyst stages are used. All stages are connected to each other in terms of plant stages in terms of reaction stages, ie each represents individual units.
  • NT-PEM fuel cells low-temperature (NT) and high-temperature (HT) PEM fuel cells.
  • HT-PEM fuel cells the CO contained in the reformate must be largely removed as described above, whereas the HT-PEM fuel cells are less sensitive to CO because of the CO adsorption / desorption equilibrium shifted to CO adsorption at higher temperatures .
  • synthesis gases having a concentration of CO of up to 3% by volume can also be used (see, for example, EP 1 523 053 A2), as a result of which the abovementioned CO fine purification stage can be dispensed with. No.
  • 6,753,102 B2 describes in this context a fuel cell system based on an HT-PEM with a three-stage process concept. After desulphurisation (first stage), an autothermal reactor for reforming follows (second stage), followed by a shift reactor to reduce the CO content (third stage).
  • the object of the present invention is therefore to provide a method and an apparatus for producing a hydrogen-containing gas mixture with the lowest possible CO concentration with as little equipment as possible.
  • a catalyst which has a reforming reaction and a Catalyze water gas shift reaction.
  • the control in which areas of the catalyst-loaded catalyst support one or the other reaction prevails, is carried out with a two-step axial temperature profile. This has i) a first zone, in which predominantly undergoes a reforming reaction, with a minimum temperature above the temperature of the second zone ii), and ii) a second zone, in which predominantly runs a Wassergasshiftresure, with a maximum temperature below the temperature of the first zone i).
  • the same catalyst or mixtures of several (two, three, four) different catalysts can be used.
  • the same catalyst which catalyzes both the reforming reaction and the shift reaction can be used in both zones, such as a Pt / Rh-containing catalyst, a Pt / Re-containing catalyst, a Ni catalyst or a Fe catalyst. Cr-shift catalyst.
  • This embodiment also includes the use of the same mixture of two or more catalysts in both zones.
  • a catalyst is used which catalyses both the reforming reaction and the shift reaction, and in the second zone another catalyst other than the first catalyst which also catalyzes both the reforming reaction and the shift reaction.
  • the second catalyst in the lower zone is better for the shift reaction
  • the first catalyst in the upper zone is better for reforming, but both catalysts catalyze both reactions.
  • a Pt / Rh-containing catalyst can be used; at the bottom in zone ii) a Pt / Re-containing catalyst is used.
  • an upper charge can also be made from a different catalyst than the lower one, but both catalyze both reactions - depending on the temperature. Examples include, for example, above a Ni catalyst and below an Fe-Cr shift catalyst. It is also conceivable to use different mixtures of two or more different catalysts in each of the zones i) and ii).
  • catalysts which contain finely dispersed platinum in particular so-called shift catalysts, as are generally known. It is also possible to use catalysts of other metals, such as Co, Ni, Cu / Zn, Fe / Cr, Ru, Rh, Pd, Ag, Re, Os, Ir, Au and / or mixtures thereof (also in combination with Pt) , Preference is given to using, for example, Pt / Rh-containing catalysts, Pt / Re-containing catalysts, Ni catalysts or Fe-Cr-shift catalysts. Suitable catalysts are, for example, as described in EP 1 161 991 A1 and in particular in the examples there.
  • the disclosure of EP 1 161 991 A1 is hereby incorporated by reference into the present application.
  • the catalysts to be used according to the invention generally catalyze both the reforming reaction and the shift reaction, with a strong preference for one or the other reaction depending on the temperature.
  • the same catalyst can be used in both zones, or even a different catalyst. Particularly preferably, the same catalyst is used in both zones.
  • the catalysts are applied to the catalyst support, according to methods known in the art.
  • the catalyst is applied to the catalyst support by coating or by impregnation of the catalyst support.
  • the active catalyst components can be applied directly to bulk material, for. B. on simple ⁇ Al 2 O 3 carrier or Y-Al 2 O 3 carrier or similar ceramic carrier systems - carriers, for example, previously shaped into spheres, tablets, extrudates, Triholes or other forms.
  • Al 2 O 3 and other oxides such as Ce oxides, Zr oxides, Ti oxides, La oxides and mixtures of the oxides and optionally additional promoters are conceivable.
  • concentration and temperature of the impregnation solution, the porosity of the support and the impregnation process itself can be used to control the penetration depth and the concentration of the catalytically active catalyst materials on the support.
  • the catalyst of the invention can be prepared by impregnation of a catalyst support such. As tablets, spheres, extrudates or granules are prepared with an aqueous solution of salts of the desired metal. The impregnated Catalyst is then dried and calcined, optionally these steps are repeated one or more times.
  • so-called supported catalysts can be prepared in which the catalytically active components are applied in highly dispersed form on support materials.
  • support materials are used which have a large specific surface area for receiving the catalytically active components.
  • washcoat It is finely divided, that is powdery, temperature-stable metal oxides - hereinafter referred to as washcoat.
  • Typical washcoat main constituents are aluminum oxides, cerium oxides, zirconium oxides and other metal oxides. Additional promoters to stabilize the high surface areas or to suppress or promote side reactions may also be present.
  • mixed oxides with BET surface areas of about 50 to about 250 m 2 / g are used.
  • honeycomb bodies made of ceramic (eg cordierite) or metal.
  • honeycomb bodies are also called monoliths below.
  • monolith as used in the context of the present invention, is described, for example, in "Monoliths in multiphase catalytic processes - aspects and prospects" by F. Kapteijn, JJ Heiszwolf, TA Nijhuis and JA Moulijn, Cattech 3, 1999, p. 24 Are defined. According to this, monoliths are understood to mean not only the “classical” carrier bodies with parallel, radially non-interconnected channels. It also includes foams, sponges o. The like.
  • the carrier materials are dispersed, for example, in water and homogenized, for example, by a grinding process.
  • the walls of the honeycomb bodies are then coated by one or more immersions in the coating dispersion with subsequent drying and calcination.
  • the catalytically active components can be applied at different times to the specific surface of the support materials.
  • the catalytically active components can be deposited on the support materials only after coating the honeycomb bodies with the dispersion coating by immersing the coated honeycomb bodies in an aqueous solution of soluble precursors of the catalytically active components.
  • the catalytically active components are applied to the pulverulent carrier materials in a step preceding the preparation of the dispersion coating.
  • the active components are supported on support materials comprising a mixed oxide comprising cerium oxide (CeO x ), lanthanum oxide (La 2 O 3 ), aluminum oxide (Al 2 O 3 ), yttrium oxide (Y 2 O 3 ), titanium oxide (TiO 2 ) , Zirconia (ZrO 2 ), silica (SiO 2 ) or mixtures thereof.
  • the carrier material mixed oxide can, for. B. It can be made impregnation of alumina with the nitrate salts of the respective other metals and subsequent calcination.
  • the support material is previously z. B. coated on monolithic cordierite honeycomb, dried and calcined; in one or more further impregnation, drying and calcination steps, the active components are deposited thereon.
  • the honeycomb monolithic carriers are known in the art and are described, for. B. used in the automotive industry. Examples of various monolithic supports are described in Handbook of Heterogenous Catalysis 4 - Environmental Catalysis, pages 1575-1583.
  • Other suitable methods for applying the active components to the supports are impregnation, spraying, ion exchange, precipitation, immersion, pumping and all other techniques described in the literature, as well as combinations of said methods.
  • a method is used for coating, which is referred to as dip-coating.
  • the catalyst supports according to the invention are particularly preferably in the form of honeycombs or honeycombs. However, other honeycomb geometries are also possible.
  • the catalyst supports can also be in other forms, for example as foam, fleece or mesh. Of course, combinations of individual shapes or designs can be used.
  • the annular honeycomb shape is advantageous because the relatively perfused geometric surface to the outer wall increases and thus a better heat input from the reactor wall to the honeycomb (and vice versa) can be realized. It may be advantageous to provide the catalyst support with heat transfer promoting elements wholly or partially, for example, to wrap it partially with a metal fleece before it is introduced into the overall reactor apparatus.
  • the catalyst support in whole or in part with positioning aid, for example, to wrap it with mineral wool before it is introduced into the overall reactor apparatus.
  • positioning aid for example, to wrap it with mineral wool before it is introduced into the overall reactor apparatus.
  • the reforming reaction in the first zone carried out in the context of the process according to the invention is preferably selected from the group consisting of steam reforming (STR), catalytic partial oxidation (CPO) and autothermal reforming reaction (ATR).
  • STR steam reforming
  • CPO catalytic partial oxidation
  • ATR autothermal reforming reaction
  • other reactions may also be carried out in the first zone of the catalyst which convert hydrocarbons to hydrogen and CO.
  • the first zone is supplied with a mixture of hydrocarbon and water vapor; for the CPO a mixture of hydrocarbon and oxygen; for the ATR a mixture of hydrocarbon, water vapor and oxygen.
  • the educt gas contains gaseous or vaporizable hydrocarbons.
  • Exemplary hydrocarbonaceous fuels include natural gas, LPG, gasoline, diesel, biogas, alcohols, synthetic fuels or the like.
  • the educt gas preferably contains methane. It may be advantageous to adjust a certain ratio of oxygen molecules to methane molecules for the reforming reaction. For example, a molar ratio of oxygen to carbon of from 0.1 to 0.9, preferably from 0.4 to 0.7, is suitable. It may also be advantageous to adjust a certain ratio of water vapor molecules to methane molecules for the reforming reaction. For example, a molar ratio of water to carbon of 1.0 to 5.0, preferably 1.5 to 3.5, is suitable. These ratios can be adjusted, for example, by modulating the flow rates of these substances, which then gives the desired molar flow rate.
  • a water gas shift reaction (WGS) is catalyzed, which, as shown above, converts CO to CO 2 , thereby lowering the CO content of the gas leaving the first zone.
  • the temperature profile according to the invention can be generated, for example, by means of an active or passive heat exchanger principle.
  • Active heat exchangers, or heat exchangers or heat exchangers for short are devices which serve to transfer heat from one liquid or gaseous substance to another. The heat is transferred through a partition from fluid to fluid. While in an active heat exchanger, the resulting heat is actively removed by means of a suitable cooling medium, in passive heat exchange systems, the resulting heat will be transferred to the heat storage and / or to the environment.
  • cooling fins, fins, etc., and / or fillers such as metallic balls, discs, etc., are used.
  • active heat exchangers are used in the process according to the invention.
  • the gas inlet temperature at the first zone i) between 600 and 900 0 C, more preferably between 700 and 800 0 C, and the gas outlet temperature at the end of the second zone ii) between 150 and 350 ° C, more preferably between 150 and 250 ° C.
  • the minimum temperature in the zone i) is in particular> 500 0 C, preferably> 600 0 C, particularly preferably> 625 ° C.
  • the maximum temperature in the zone ii) is in particular ⁇ 400 ° C, preferably ⁇ 350 0 C, particularly preferably ⁇ 325 ° C.
  • the cooling for setting the lower temperature in the second zone for example, by means of a cooling loop, which is wound around the reactor or the catalyst support.
  • the cooling loop can be operated for example with water as the cooling medium.
  • the dissipated heat is absorbed by the cooling medium. This effect can be used to full advantage in terms of energy by using the reaction water required for the SR or ATR reactions as the cooling medium and therefore preheating or completely or partially evaporating before the reaction.
  • the cooling medium is guided in countercurrent to the gas flow.
  • the reactors according to the invention may comprise a zone i 'upstream of the zone i) with a minimum temperature above the temperature of the second zone. This will be three
  • the zones i ') and i) have the same setpoint temperature and, moreover, are of the same design with regard to the generation of heat.
  • the present invention furthermore relates to an integrated fuel cell system comprising a reactor according to the invention, a fuel cell and optionally an oxidation unit.
  • the fuel cell may be a high temperature PEM fuel cell operating at a higher temperature level, e.g. B. from 120 0 C, or a low-temperature PEM fuel cell, which runs at a temperature level of about 80 0 C act.
  • a high-temperature PEM fuel cell having a working temperature of at least 120 ° C. is preferably used.
  • Such a fuel cell system preferably contains a desulfurization unit upstream of the reactor.
  • the hydrocarbon-containing educt gas is first passed through the desulfurization unit, then through the reactor according to the invention and finally by a PEM fuel cell for energy.
  • the gas emerging from the fuel cell which still contains residues of hydrogen and carbon monoxide, can finally be passed through an oxidation unit for purification.
  • FIG. 1 shows a reactor 99 according to the invention
  • FIG. 2 shows a fuel cell system 102 according to the invention
  • FIG. 3 shows a graph with information on temperature and gas composition.
  • thermocouple 12 thermocouple 20: lower flange
  • feedstock for educt gas 102 fuel cell system
  • reactor 130 according to the invention: feed for air and / or water
  • the central bore of the honeycomb 1 is closed with a plug (not shown) to avoid a bypass flow of the reaction gas.
  • the honeycomb 1 is inserted into the reactor tube 4 with a metal fleece 2 and a mineral wool wrapper 3.
  • the gas inlet of the educt gas is located at the upper end of the reactor 99 (symbolized by a targeting the reactor double arrow) at the upper flange 21, the gas outlet at the lower flange 20.
  • a thermocouple 11, 12 is positioned to the Gas inlet or gas outlet temperature to measure.
  • the reactor is divided into three heating zones 30, 31, 32, wherein the upper two zones 30, 31 are set to maximum heating power with 890 0 C target temperature and the lowermost zone 32 is actively cooled with a cooling loop winding 10 around the reactor 99.
  • the cooling loop consists of a 3 mm Swagelok cable with a length of about 6 m and about 20 to 30 wraps.
  • the cooling medium is water, which is pumped with an HPLC pump and a temperature of about 20 0 C in the cooling zone 32.
  • the coolant is passed in countercurrent to the gas flow.
  • the gas inlet temperature of the fed methane / steam mixture in the honeycomb 1 is 760 ° C (optimal range for the STR reaction), during the forced by the cooling gas exit temperature from the comb 1 in the steady-state condition of about 200 0 C is ( optimal range for the WGS reaction).
  • the molar steam / carbon ratio of the educt gas is 3: 1.
  • the gas mixture leaving the reactor 99 has an H 2 content of about 75% by volume, a CO 2 content of about 18% by volume, a CH 4 content of about 8% by volume and a CO content of about 1.5% by volume, making it ideal for operating an HT-PEM fuel cell.
  • the gas inlet and outlet temperature and the gas composition of the product gas are shown in Fig. 3.
  • the fuel cell system 102 shown in FIG. 2 is equipped with a fuel conditioning system 104 and an exhaust oxidation system 106.
  • a hydrocarbonaceous substance is passed as it is, for example, to desulfurization unit 110, which may contain, for example, sulfur adsorbents such as activated carbon.
  • the desulfurized educt gas is passed into the reactor 120 according to the invention, the reactor 120 being supplied with air and water via the feed 130 for the reforming and shift reactions taking place in the reactor 120.
  • the reactor exhaust gas, that is the fuel for the fuel cell stack 160 is supplied to the fuel cell stack 160 via the feed 150. Through the air supply 170, the fuel cell stack 160 air is supplied.
  • the exhaust of the fuel cell stack 160 exits through the feed 180 and into the oxidation unit 190.
  • the oxidation unit 190 may be, for example, an "anode tail gas oxidizer" (ATO), a combustor, or a boiler operating at higher temperatures (e.g., 800 ° C) with a suitable oxidation catalyst (e.g., platinum).
  • ATO an "anode tail gas oxidizer”
  • combustor a combustor
  • boiler operating at higher temperatures (e.g., 800 ° C) with a suitable oxidation catalyst (e.g., platinum).
  • a suitable oxidation catalyst e.g., platinum
  • substantially simplified fuel cells can be produced by the process according to the invention and the reactor according to the invention.
  • HT-PEM fuel cells can be operated directly with the hydrogen-rich and low carbon monoxide gas mixtures obtained according to the present invention. But even with NT-PEM fuel cells or other applications with the need to reduce the CO content in the fuel shift stages or stages for fine cleaning can be sized smaller and thereby advantages in terms of reaction and / or plant size can be achieved.

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Abstract

L'invention concerne un réacteur et un procédé de fabrication d'un mélange gazeux contenant de l'hydrogène. Selon l'invention, un support de catalyseurs comportant un ou plusieurs catalyseurs pour catalyser une réaction de reformage et une réaction de conversion à la vapeur d'eau est employé dans un réacteur. Un profil de température axial comportant deux zones, c.-à-d. i) une première zone dans laquelle se déroule essentiellement une réaction de reformage, dont la température minimale est supérieure à la température de la deuxième zone, et ii) une deuxième zone dans laquelle se déroule essentiellement une réaction de conversion à la vapeur d'eau, dont la température maximale est inférieure à la température de la première zone, est présent dans le support de catalyseurs.
PCT/EP2009/054520 2008-04-28 2009-04-16 Procédé de fabrication d'un mélange gazeux contenant de l'hydrogène Ceased WO2009153079A1 (fr)

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EP09765659A EP2285738A1 (fr) 2008-04-28 2009-04-16 Procédé de fabrication d'un mélange gazeux contenant de l'hydrogène

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DE102008021083A DE102008021083A1 (de) 2008-04-28 2008-04-28 Verfahren zur Herstellung eines wasserstoffhaltigen Gasgemisches
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