WO1997043796A1 - Membrane reactor for producing co- and co2-free hydrogen - Google Patents

Membrane reactor for producing co- and co2-free hydrogen Download PDF

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Publication number
WO1997043796A1
WO1997043796A1 PCT/DE1997/000880 DE9700880W WO9743796A1 WO 1997043796 A1 WO1997043796 A1 WO 1997043796A1 DE 9700880 W DE9700880 W DE 9700880W WO 9743796 A1 WO9743796 A1 WO 9743796A1
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WO
Grant status
Application
Patent type
Prior art keywords
hydrogen
chamber
methanol
co2
membrane
Prior art date
Application number
PCT/DE1997/000880
Other languages
German (de)
French (fr)
Inventor
Josefin Meusinger
Haart Lambertus G. J. De
Ulrich Stimming
Original Assignee
Forschungszentrum Jülich GmbH
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

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Classifications

    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M8/00Fuel cells; Manufacture thereof
    • H01M8/06Combination of fuel cells with means for production of reactants or for treatment of residues
    • H01M8/0662Treatment of gaseous reactants or gaseous residues, e.g. cleaning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2475Membrane reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • B01J8/009Membranes, e.g. feeding or removing reactants or products to or from the catalyst bed through a membrane
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/04Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds
    • B01J8/0403Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the fluid flow within the beds being predominantly horizontal
    • B01J8/0407Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the fluid flow within the beds being predominantly horizontal through two or more cylindrical annular shaped beds
    • B01J8/0411Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid passing successively through two or more beds the fluid flow within the beds being predominantly horizontal through two or more cylindrical annular shaped beds the beds being concentric
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/323Catalytic reaction of gaseous or liquid organic compounds other than hydrocarbons with gasifying agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • C01B3/501Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by diffusion
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL INTO ELECTRICAL ENERGY
    • H01M8/00Fuel cells; Manufacture thereof
    • H01M8/06Combination of fuel cells with means for production of reactants or for treatment of residues
    • H01M8/0606Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
    • H01M8/0612Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants from carbon-containing material
    • H01M8/0625Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants from carbon-containing material in a modular combined reactor/fuel cell structure
    • H01M8/0631Reactor construction specially adapted for combination reactor/fuel cell
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00309Controlling the temperature by indirect heat exchange with two or more reactions in heat exchange with each other, such as an endothermic reaction in heat exchange with an exothermic reaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00504Controlling the temperature by means of a burner
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/02Processes carried out in the presence of solid particles; Reactors therefor with stationary particles
    • B01J2208/023Details
    • B01J2208/024Particulate material
    • B01J2208/025Two or more types of catalyst
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00117Controlling the temperature by indirect heating or cooling employing heat exchange fluids with two or more reactions in heat exchange with each other, such as an endothermic reaction in heat exchange with an exothermic reaction
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00157Controlling the temperature by means of a burner
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0405Purification by membrane separation
    • C01B2203/041In-situ membrane purification during hydrogen production
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465Composition of the impurity
    • C01B2203/0475Composition of the impurity the impurity being carbon dioxide

Abstract

The invention concerns a reactor for converting methanol into CO- and CO2-free hydrogen. The reactor comprises a membrane (1) which divides it into two chambers. The membrane filters CO2 out of a hydrogen-CO-CO2 mixture. Methanol is introduced into the first chamber (3) and is converted into hydrogen there by means of a catalyst. During this conversion, CO and CO2 are produced as by-products. A burner heats the first chamber, so ensuring that the required conversion temperatures are provided. CO and hydrogen are diffused through the membrane (1) into the second chamber (4) in which CO is converted into methane by means of a catalyst. The resultant hydrogen is now sufficiently free from CO and CO2 and can be fed directly as fuel gas to the anode side of a PEM fuel cell.

Description

Description

Membrane reactor for the production of CO and C0 2 -free hydrogen

The invention relates to a reactor for Um¬ conversion of methanol into hydrogen.

Such reactors intended for use in Ver¬ connection with fuel cells and in particular with PEM fuel cells are. The latter are to be used in the future as components of electric drive systems in vehicles.

Advantageously, a polymeric Festelektro- can be used lyte in PEM fuel cell compared to other fuel cells, which enables easy handling and the construction of compact cells. PEM fuel cells exhibit high power density of about 1 W / cm at operating temperatures of 80 ° C.

For the oxidation of pure hydrogen in acidic electrolyte as the PEM fuel cell, platinum proves (Pt) as the most effective Elektrokatalysa- tor. However, since the existing infrastructure for the car also be utilized in the future, ie liquid fuels to be marketed material, liquid methanol has to be implemented in the vehicle by a reforming reaction to Wasser¬ material.

A disadvantage occur in the conversion of methanol into hydrogen by-products such as CO, the torgifte as Katalysa¬ act for the electrocatalyst Pt. thus contains the fuel gas in addition to hydrogen and CO, enters a drastic reduction in cell performance.

Therefore, a gas treatment process for the production of water serstoffbrenngas with a CO content of less than 10 ppm between the reformer and PEM fuel cell must be carried out. The purity desired can currently only be achieved by use of a Pd / Ag membrane. The An¬ procurement costs for such a membrane are nachteil- way very high.

Another way to meet the purity requirements ge right, based on the chemical reaction of CO with hydrogen to form methane (Methanisierungsreak- tion). At low reaction temperatures (180 ° C) and use of noble metal catalysts it is possible to lower the CO content in such a Gasnachbehandlungs- unit 10 ppm. This requires, however, that before the C0 2 was removed from the gas mixture. C0 2 is subject in analog reaction conditions also the methanation or slightly higher reaction temperatures of Kon¬ set conversion to CO. The object of the invention is converted such that the hydrogen fuel cell directly as a fuel gas in a PEM Brenn¬ can be used to provide a reactor of the methanol in the hydrogen. The object is achieved by a reactor having the features of the main claim. The reactor used for carrying out the method according to independent claim.

The reactor has a membrane which divides the reactor into two chambers. The membrane filters C0 2 from a hydrogen-CO-C0 2 mixture out. It is folg¬ Lich practically impermeable to C0 second CO and especially hydrogen can pass through the membrane.

In particular, ceramic membranes are provided in the dung Erfin. In the first chamber methanol is introduced and converted into hydrogen. The conversion is carried spielsweise by a suitable catalyst at temperatures required for this conversion. Means for heating the first chamber provide for the provision of the required conversion temperatures. CO and hydrogen permeate through the membrane into the second chamber. Here, the CO will be delt umgewan¬ into methane.

The product gases produced in the second chamber are practically free from CO and C0. 2 They can now be directly supplied to the anode side of a membrane (PEM) fuel cell. Means are advantageously provided by means of which from the residual gases (= not into the second chamber diffused reaction products and unreacted methanol) heat of reaction for the methanol reforming reaction is produced. As means for generating the heat Reaktions¬ a conventional burner is suitable.

In an advantageously simple construction of the actuator Re¬ consists of a tubular membrane, which Neren located in the home of a further tube (reaction tube) is located.

This gives rise to an annular gap between the outer wall of the membrane and the inner wall of the reaction tube. This annular gap is ge with a reforming catalyst filled and takes over the function of the first chamber (first area). Required reaction heat in the er¬ sten chamber is provided by heating the outer wall of the Reak¬ tion tube is available. The second chamber (second region) is located within the gene röhrenförmi¬ membrane and is filled with a gate Methanisierungskatalysa-.

wan¬ due to the existing concentration and Druckge¬ Faelles between first and second reactor chamber countries hydrogen and generated in the first chamber CO gases through the membrane into the second chamber. Unreacted methanol and the other

(Oxygen-containing) reaction products in the first chamber exit the reactor via the annular gap. Means are advantageously provided that the residual gases from the first chamber and a re-challenges Heizmit¬ tel (Brenner) out. Here, the residual gases are erfor¬ derlichenfalls mixed with fresh methanol incinerated, thus forming reactive heat of reaction for methanol reform, that generates the heat the first reaction zone here.

The hydrogen-CO mixture in the second chamber is (sufficiently) free of C0. 2 It is directly connected to the methanation in the second chamber

(Interior) of the reactor and contacted the so converted CO in methane. The product gases can then be fed to the anode side of the PEM fuel cell.

is at the tubular structure, a strong endotherm with a strongly exothermic reaction through the permeable membrane coupled in an advantageous manner: An unwanted Tempe¬ raturanstieg in the methanation is prevented by the running in the shell reforming reaction.

The reactor is in particular made of ceramic materi- lien.

The membrane is advantageously made of an oxide on Ba¬ sis of Al 2 0 3 and / or SiO. These materials have high separation factors for hydrogen / C0 2 at reaction conditions of methanol reforming. They do not age, are not problematic with regard to design and inexpensive.

The invention is further illustrated by the figure and the subsequent data. The figure shows in cross section a tubular membrane 1, which is surrounded by an enveloping tube. 2 The annular gap 3 forms the first chamber. The second chamber 4 is located inside of the tubular membrane 1. The membrane is closed at one pipe end. At the other end, the product gases are fed via a discharge line 5 of a PEM fuel cell. Methanol is fed via a supply line 6 of the first chamber of the reactor. In the first chamber resulting residual gases to a burner, not shown here are fed via the outlet 7, which heated the reactor if necessary, from the outside.

A passenger car the performance class required 70 kW, a fuel cell that delivers 170 kW of electrical power. This results in a value for the bereitzu¬ Vice forming hydrogen stream of about 0.158 mol / s. This hydrogen must be incurred in pure form (less than 10 ppm CO) according to the second chamber. Starting from experi¬ Mentell certain permeation rates for ceramic diaphragms at 200 ° C for hydrogen (20 * 10 "7 mol / m 2 / s / Pa) is given at a differential pressure of 5 * 10 Pa a min¬ least necessary membrane area of 15.8 dm 2.

The generation of hydrogen based on the methanol reforming in the first zone. At a temperature of 250 ° C the necessary reforming catalyst volume may speed of the experimentally determined Bildungsge¬ of hydrogen (2-4 Nm / h / dm kat) starting, are determined: 3.16 dm. 4 1 of a highly active noble metal catalyst in the second reaction zone placed, it comes at a self-adjusting temperature to 180 ° C for methanation of CO contained in the permeate's. The resulting in reforming proportion of 2 vol .-% CO is so degraded at sufficiently low space velocities at 10 ppm.

Claims

P atentanspr ü che
1. Reactor for the conversion of methanol into hydrogen
- with a diaphragm (1) for dividing the Reak¬ gate into two chambers (3, 4), wherein the membrane causes a filtering out of C0 2 from a hydrogen-CO-C0 2 mixture,
- with means for the introduction of methanol in the er¬ ste chamber and for conversion of the methanol in Was¬ serstoffhaltige gases in said first chamber,
- with means for the conversion of CO in methane in the second chamber.
2. A tubular reactor according to the preceding claim having a tubular membrane (1) which separates the first chamber (3) from the second chamber (4).
3. A process for the conversion of methanol into hydrogen, comprising the steps:
- conversion of methanol into an existing from hydrogen, carbon dioxide and carbon monoxide gas mixtures mixed,
- removal of carbon dioxide from the gas mixture,
- conversion of carbon monoxide into methane.
PCT/DE1997/000880 1996-05-10 1997-04-26 Membrane reactor for producing co- and co2-free hydrogen WO1997043796A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DE1996118816 DE19618816C2 (en) 1996-05-10 1996-05-10 Membrane reactor for the production of CO and hydrogen-free CO¶2¶
DE19618816.4 1996-05-10

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP54037497A JP2000510433A (en) 1996-05-10 1997-04-26 Membrane reactor to produce hydrogen not containing Co and co ▲ under 2 ▼
US09185228 US6129861A (en) 1996-05-10 1998-11-03 Membrane reactor for producing CO- and CO2 -free hydrogen

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US09185228 Continuation US6129861A (en) 1996-05-10 1998-11-03 Membrane reactor for producing CO- and CO2 -free hydrogen

Publications (1)

Publication Number Publication Date
WO1997043796A1 true true WO1997043796A1 (en) 1997-11-20

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JP (1) JP2000510433A (en)
DE (1) DE19618816C2 (en)
WO (1) WO1997043796A1 (en)

Cited By (9)

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Publication number Priority date Publication date Assignee Title
US6221117B1 (en) 1996-10-30 2001-04-24 Idatech, Llc Hydrogen producing fuel processing system
US6319306B1 (en) 2000-03-23 2001-11-20 Idatech, Llc Hydrogen-selective metal membrane modules and method of forming the same
US6419726B1 (en) 1999-10-21 2002-07-16 Ati Properties, Inc. Fluid separation assembly and fluid separation module
US6419728B1 (en) 1999-03-22 2002-07-16 Idatech, Llc Hydrogen-permeable metal membrane and method for producing the same
US6451464B1 (en) 2000-01-03 2002-09-17 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
US6572837B1 (en) 2000-07-19 2003-06-03 Ballard Power Systems Inc. Fuel processing system
US6582499B2 (en) * 1998-11-10 2003-06-24 Ati Properties, Inc. Fluid separation assembly
US6602325B1 (en) 1999-10-21 2003-08-05 Ati Properties, Inc. Fluid separation assembly
US7390347B2 (en) 2000-08-07 2008-06-24 Noritake Co., Ltd. Zeolite membranes for selective oxidation of carbon monoxide in mixed hydrogen gas source

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US5997594A (en) * 1996-10-30 1999-12-07 Northwest Power Systems, Llc Steam reformer with internal hydrogen purification
DE19817534A1 (en) * 1998-04-16 1999-10-21 Mannesmann Ag Production of electrical energy from hydrogen-rich crude gas
DE19904401C2 (en) * 1999-02-04 2001-05-17 Daimler Chrysler Ag Hydrogen production plant with membrane reactor
WO2002004347A1 (en) * 2000-04-21 2002-01-17 Institut Français Du Petrole Hydrogen derived from methanol cracking is used as a clean fuel for power generation while reinjecting co-product carbon dioxide
JP4742405B2 (en) 2000-06-28 2011-08-10 トヨタ自動車株式会社 Fuel reformer
JP4682403B2 (en) * 2000-08-31 2011-05-11 株式会社Ihi Co removing device and the fuel cell power generation system using the same
EP1365990A2 (en) * 2001-03-05 2003-12-03 Shell Internationale Research Maatschappij B.V. Apparatus and process for the production of hydrogen

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Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6221117B1 (en) 1996-10-30 2001-04-24 Idatech, Llc Hydrogen producing fuel processing system
US6582499B2 (en) * 1998-11-10 2003-06-24 Ati Properties, Inc. Fluid separation assembly
US6419728B1 (en) 1999-03-22 2002-07-16 Idatech, Llc Hydrogen-permeable metal membrane and method for producing the same
US6419726B1 (en) 1999-10-21 2002-07-16 Ati Properties, Inc. Fluid separation assembly and fluid separation module
US6602325B1 (en) 1999-10-21 2003-08-05 Ati Properties, Inc. Fluid separation assembly
US6451464B1 (en) 2000-01-03 2002-09-17 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
US6818335B2 (en) 2000-01-03 2004-11-16 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
US7008708B2 (en) 2000-01-03 2006-03-07 Idatech, Llc System and method for early detection of contaminants in a fuel processing system
US6458189B1 (en) 2000-03-23 2002-10-01 Idatech, Llc Hydrogen-selective metal membrane modules and method of forming the same
US6319306B1 (en) 2000-03-23 2001-11-20 Idatech, Llc Hydrogen-selective metal membrane modules and method of forming the same
US6572837B1 (en) 2000-07-19 2003-06-03 Ballard Power Systems Inc. Fuel processing system
US7390347B2 (en) 2000-08-07 2008-06-24 Noritake Co., Ltd. Zeolite membranes for selective oxidation of carbon monoxide in mixed hydrogen gas source

Also Published As

Publication number Publication date Type
JP2000510433A (en) 2000-08-15 application
DE19618816A1 (en) 1997-11-13 application
DE19618816C2 (en) 1999-08-26 grant

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