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WO2008151367A1 - Système pour la production d'hydrogène - Google Patents

Système pour la production d'hydrogène Download PDF

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Publication number
WO2008151367A1
WO2008151367A1 PCT/AU2008/000838 AU2008000838W WO2008151367A1 WO 2008151367 A1 WO2008151367 A1 WO 2008151367A1 AU 2008000838 W AU2008000838 W AU 2008000838W WO 2008151367 A1 WO2008151367 A1 WO 2008151367A1
Authority
WO
WIPO (PCT)
Prior art keywords
hydrogen
steam
production
reactor
batch system
Prior art date
Application number
PCT/AU2008/000838
Other languages
English (en)
Inventor
Geoffrey David Will
Neville Charles Stephenson
Original Assignee
Alternative Energy International Ltd
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
Priority claimed from AU2007903150A external-priority patent/AU2007903150A0/en
Application filed by Alternative Energy International Ltd filed Critical Alternative Energy International Ltd
Publication of WO2008151367A1 publication Critical patent/WO2008151367A1/fr

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
    • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
    • C01B3/10—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents by reaction of water vapour with metals
    • 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
    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Definitions

  • the present invention relates to systems for the production of hydrogen and particularly to system for the efficient reduction of steam to hydrogen and inorganic salts.
  • the inventors of the present invention have also been active in this area previously.
  • PCT/AUOO/00446 provides an electrochemical cell (“Cell 1") that produces hydrogen, steam and heat by the reduction of water, at a high PH range using a solution of electro positive half cell reactions, each of which enhances the effectiveness of the other half-cell reactions .
  • the present application is directed towards a unique process used in enhancing the hydrogen output of the system.
  • the basic reaction involves the reduction of steam on the surface of metallic iron. This reaction is well documented in the chemical literature and leads to the formation of magnetite Fe 3 O 4 , hydrated Fe 2 O 3 ferrous oxide FeO and other hydrated iron oxides.
  • the objectives of this application are to describe the production of continuous streams of hydrogen that would be commercially viable and to control the thermodynamic parameters that are involved. hi addition, for the design to be compatible with national safety and use standards and legislative requirements and the resultant chemical products to be reconstituted for further use.
  • the present invention is directed to a system for the production of hydrogen, which may at least partially overcome at least one of the abovementioned disadvantages or provide the consumer with a useful or commercial choice.
  • the present invention in one form, resides broadly in a system for the production of hydrogen, the system including a fuel container adapted for use as a reactor, the fuel including an iron-based fuel source, a steam inlet to the fuel container to provide steam at an elevated temperature and pressure wherein the reactor is a fluidised bed reactor.
  • the system preferably operates on the basis of thermal decomposition of water to form hydrogen with the energy for the decomposition of the water gained from the steam provided at elevated temperature and pressure rather than electrolytic decomposition.
  • ferrous iron oxide an other forms such as iron hydroxides, for example
  • Fe(OH) 3 . xH 2 0 may also form.
  • the nature of the metallic products formed is typically dependant upon conditions such as wetness, operating temperature, operating pressure, time and the influence of contaminants in the feed iron.
  • the reactor of the present invention will typically be a batch reactor, wherein a pre-filled fuel canister can be installed into the system to function as the reactor vessel until the iron-based fuel material contained in the pre-filled canister is sufficiently exhausted.
  • the concept behind the integrated fuel canister/reactor is a timed (typically approximately 24 hour) batch hydrogen reaction, utilising a vessel that can be used for either in situ regeneration of the spent fuel or removal for reloading and/or external fuel regeneration.
  • the batch process eliminates the issues associated with continuous fuel handling and spent fuel handling operations. Such operations, although possible, and indeed provided for according to the present invention, greatly add to the complexity and cost of the system. Of more concern in any continuous handling system, is the increased chance that hydrogen leaks will occur. Any such leaks from the reaction system are highly likely to ignite, due to the elevated reaction temperature (which exceeds the auto-ignition temperature of hydrogen) and the thermodynamic properties of hydrogen which cause the hydrogen to heat up when vented to a lower pressure.
  • Steam is typically passed through the canister over the time period at a nominal ratio of steam per kilogram of iron fuel.
  • the reactor vessel will normally be fluidized, and the most preferred method is by mechanical vibration. In a single pass, roughly 25% of the steam will generally be converted to hydrogen, depending primarily on reaction temperature and extent of fuel conversion. Heat will also normally be liberated by the reactions, so that the product gas will be hotter than the reaction steam. This excess heat can be used to pre-heat the inlet steam or be retained in-system to maintain the temperature of the reactants.
  • the steam/hydrogen product gas is preferably partly cooled by exchange with the incoming reaction steam via a pipe-in-pipe heat exchange arrangement.
  • the steam is condensed from the steam/hydrogen mixture in a set of cooling coils. Heat is transferred from coiled tubes initially to steam vapour and then to deionised water which will preferably be provided in a lower part of each vessel, thereby generating the required steam and recycling enough heat to minimise the need for the addition of external heat.
  • the condensate saturation temperature will be a function of the system pressure and thus is expected to increase up to approximately 150 - 180°C after the initial start-up period.
  • Condensed water vapour is separated from the hydrogen product in the condensate separator and recycled to the steam generator via the condensate holding tank and condensate recycle pump.
  • the controls in the condensate recycle system influence how much condensate is recycled and to which part of the system generation circuit, thereby providing temperature control to the reactor vessel, which may otherwise tend towards thermal run-away.
  • vapour condenser and steam generator are preferably integrated as a single (modular) unit operation.
  • the design concept recognises the batch mode of the system of the present invention and continues encasing hydrogen piping inside steam piping/vessels to reduce the risk of a hydrogen leak to the atmosphere.
  • the vapour condenser/steam generated typically includes a plurality, preferably three, equally sized vessels which are pre-filled with deionised water.
  • One or more coils are preferably installed in each vessel to facilitate heat transfer from the hydrogen/steam mixture and the water in the steam generator chamber.
  • counter current heat exchange will occur between the hydrogen/steam mixture in the coiled tubes and the water/steam in the outer shell. In this manner, the final condensing temperature can be minimised while preserving the heat in the system.
  • the use of a number of tall, relatively small diameter units, as opposed to a single vessel, preferably enhances the desired temperature stratification effect on the water side without the need to resort to complex baffle designs.
  • the product hydrogen gas passes on to the hydrogen holding tank for further use or treatment.
  • the hydrogen is stored at the final system pressure, which will preferably not be greater than 1000 kPag.
  • This product is deemed as "wet” because the dew point of the moisture will be not lower than the temperature of the tank, which will be influenced by the temperature of the gas coming from the condensate separator.
  • industrial hydrogen gas is typically expected to have a moisture dew point of somewhat less than -20°C.
  • a pre-filled fuel canister may be provided.
  • a continuous feed cartridge may typically be provided.
  • the fuel will normally be iron particulate material. Other materials may be used for example a high surface area porous iron particulate.
  • the reactor is associated with a temperature regulation system to control the temperature in the reactor, normally by controlling the amount of heat provided from the product gas. In certain circumstances, the reactor may require cooling to prevent the reaction system "running away”.
  • Reconstitution of reaction products The chemical products produced at the catalyzed metallic surfaces are essentially oxides. These chemical products will generally be reconstituted in the present system in order to be at least partially recovered either for re-use in the system or for sale. These (generally) insoluble compounds can be reduced to metal by a number of well known methods such as the formation of soluble salts, for example, nitrates and subsequent recovery by electrolysis. Commonly used industrial methods presently use carbon (coke) or organics such as methane. However, these systems are undesirable due to the formation of oxides of carbon which are a contributor to global warming.
  • the spent fuel canister can be removed from the system and a replacement canister installed.
  • the spent fuel canister can then be connected to a reconstitution system for reconstitution of the fuel particles.
  • Figure 1 is a schematic block diagram of a hydrogen steam-iron process according to a preferred aspect of the present invention, showing preferred operating conditions.
  • a system for the production of hydrogen is provided.
  • the reactor of the illustrated embodiment is a batch reactor, namely a pre-filled fuel canister installed into the system to function as the reactor vessel until the particulate iron fuel material contained in the pre-filled canister is sufficiently exhausted.
  • the preferred embodiment has a canister containing approximately 150 kg of un-reacted iron particles which are oxidized over a 3-hour time frame, at a peak reaction temperature of approximately 550°C, to produce hydrogen.
  • steam is passed through the canister over the nominal 3-hour period at a nominal ratio of 0.45kg of steam per kilogram of iron fuel, that is approximately 22.5 kg/hour.
  • the reactor vessel is fluidized by mechanical vibration. In a single pass through the reactor of the illustrated embodiment, roughly 25% of the steam will be converted to hydrogen, depending primarily on reaction temperature and extent of fuel conversion. Heat is also liberated by the reactions, so that the product gas is hotter than the reaction steam.
  • the steam/hydrogen product gas is partly cooled by exchange with the incoming reaction steam via a pipe-in-pipe heat exchange arrangement.
  • the steam is condensed from the steam/hydrogen mixture in a set of cooling coils. Heat is transferred from coiled tubes initially to steam vapour and then to deionised water in a lower part of each vessel, thereby generating the required steam and recycling enough heat to minimise the need for the addition of external heat.
  • the condensate saturation temperature is a function of the system pressure and thus is expected to increase up to approximately 150 - 180°C after the initial start-up period.
  • Condensed water vapour is separated from the hydrogen product in the condensate separator and recycled to the steam generator via the condensate holding tank and condensate recycle pump.
  • the controls in the condensate recycle system influence how much condensate is recycled and to which part of the system generation circuit, thereby providing temperature control to the reactor vessel, which may otherwise tend towards thermal run-away.
  • the product hydrogen gas passes on to the hydrogen holding tank for further use or treatment.
  • the hydrogen is stored at the final system pressure, which will preferably not be greater than 1000 kPag. This product is deemed as "wet" because the dew point of the moisture will be not lower than the temperature of the tank, which will be influenced by the temperature of the gas coming from the condensate separator.
  • industrial hydrogen gas is typically expected to have a moisture dew point was somewhat less than -20°C.
  • the two most important vessels in the system are the fuel canister/reactor and the vapour condenser/steam generator.
  • the fuel canister/reactor is a pressure vessel which is heated/cooled via a coil wrapped about the outside of the vessel.
  • the coil will normally be secured in place using hemispherical retainers installed every approximately 300 mm along the length of the coil.
  • This coil carries reaction steam from an inlet in the top flange and terminates near the bottom of the canister where the steam enters the vessel via a finely perforated (sintered) distributor plate. Additional heating is facilitated using electric radiant heating elements located in the chamber surrounding the fuel canister.
  • the inlet/outlet is configured as a pipe-in-pipe (double containment) arrangement and terminates at both the reactor and the condenser vessel inlet manifold and custom manufactured flanges, which provides separate channels and ports for the product gas and reaction steam to transfer to the appropriate locations.
  • the reaction steam port completely encircles the steam/hydrogen outlet port, so any leak from this area bridges to the steam circuit rather than to the atmosphere.
  • the steam circuit will operate at a higher pressure than the steam/hydrogen circuit, so any leaks will usually cause dilution of the product gas rather than hydrogen recycle into the reaction steam.
  • Leakage events are to be determined from a loss of pressure differential between the steam/hydrogen circuit and the steam supply circuit.
  • Sealing of the mating flanges is achieved by a pair of single-use low carbon steel, metal O-rings seated into two concentric grooves.
  • the inner ring seals the product gas outlet and the outer ring seals the reaction steam inlet.
  • Low carbon steel does not have long-term compatibility with steam at high temperatures however it has been selected to ensure that the O-ring is softer than the flange surfaces.
  • These O-rings are provided with a copper or soft chrome coating rather than the standard 8 micron zinc coating, because the zinc coating will fuse and rapidly oxidise once the vessel is heated above 450°C.
  • the canister is pre-filled with approximately 150 kg of particulate iron fuel.
  • the reaction steam inlet is used to purge the system with dry nitrogen during start-up, then to provide heating and once the reaction is fully underway to provide cooling to avoid excessive operating temperatures.
  • the canister is slid into and secured to the base that provides the means to vibrate the vessel at approximately 1000 Hz with an amplitude of approximately 5 mm.
  • the vibration fluidises the iron particle bed, because the steam flow is insufficient to do this unaided. Fluidisation not only enhance the passage of the reaction steam through the bed, but helps to reduce short-circuiting, reduces the potential for particle agglomeration and typically assists in the removal of the reaction inhibiting oxide layer from partially reacted particles.
  • the fuel canister is secured to the retainer using a clamp that is hinged on one side and can be tightened at the accessible side over a retaining ring welded to the base of the canister.
  • the vibration exciter is mounted underneath the canister container baseplate.
  • the vibration exciter has a centre of mass in line with the canister vertical centre line.
  • a variable speed hazardous-area-rated motor rotates an exciter arm at a nominal speed of approximately 1000 rpm.
  • the exciter arm includes 5 kg eccentric mass with an adjustable shaft offset to provide an equivalent of a 50 mm load offset.
  • a split plumber block bearing supports the non-drive end of the rotating mass.
  • rollers are located to either side of the frame and are capable of movement towards and away from the canister, so that the canister can be slid into place during installation after the rollers are pivoted away from the canister.
  • Stop means are integrated into the base plate in order to limit the maximum vibration amplitude to 10 mm so as to avoid excessive stress of being placed on the inlet-outlet connection pipe connected to the top of the vessel.
  • the fuel canister/reactor is purged with dry nitrogen. This ensures that any air and moisture are displaced from the canister.
  • dry nitrogen As the steam supply heats up, and pressurizes the steam system, a mixture of nitrogen and steam enters their reactor via the steam inlet ports on the filter vessel. This mixing of dry nitrogen and steam is continued until the reaction temperature exceeds the saturation temperature of the reaction steam. Apart from eliminating explosion risks, this action reduces the risk of iron hydroxides forming and the presence of liquid water, as these may cause particle agglomeration and loss of reactive surface area.
  • the steam sourced from the steam generator during startup is heated by two electric elements. One is immersed in the bottom of the vapour condenser/steam generator and generates saturated vapour, and the other is located in the top of the vapour condenser/steam generator to superheat the vapour as condensation is undesirable downstream of the steam generator.
  • the steam is recycled between the condenser and the steam generator until the steam is superheated in excess of 50°C. Electric heating continues until a minimum reaction steam temperature is achieved, namely approximately 45O 0 C.
  • the other important vessel in the system is the vapour condenser/steam generator.
  • the pipe-in-pipe transfer pipe described above is typically divided using a manifold and the steam/hydrogen mixture enters the condenser via flexible braided hoses to a manifold and then into the particular top flange on each of the vapour condenser vessels of which there will typically be a plurality.
  • the preferred design includes three seam welded tubular vessels. Each vessel has a large height to diameter ratio. Located inside each vessel is a concentric heat transfer coil, with one coil located inside the second. Total coil length is calculated according to an average in transfer rate. For example for an average of 25 kW heat transfer rate, approximately 79 m of coil is required.
  • each vessel is partly filled with deionised water, ideally ⁇ 1 mg per litre of dissolved solids, ⁇ 1 mg per litre suspended solids, and >one megaohm conductivity ( ⁇ 1 microsiemens conductivity).
  • deionised water ideally ⁇ 1 mg per litre of dissolved solids, ⁇ 1 mg per litre suspended solids, and >one megaohm conductivity ( ⁇ 1 microsiemens conductivity).
  • Heat is transferred initially to the steam in the upper part of the vapour condenser/steam generator shell and then into the boiling water located in the lower part of the vessel.
  • the steam/hydrogen coils exit via the bottom flange. Water entry and steam exit ports are located through the lower and upper shell walls. There is also an entry point in the lower third of the vessel where hot condensate recovered from the steam/hydrogen stream is returned.
  • the cooling of the steam/hydrogen mixture causes condensation of the steam vapour until the saturation temperature at that operating pressure is reached. For a 1000 kPag operating pressure, this is approximately 184°C.
  • the condensate is returned to the steam generator shell by the condensate return pump. Retention of condensate in the holding tank is used as a secondary means to control the reactor temperature, that is, retaining condensate will result in increased steam flow as the condenser water level falls and the temperature rises.
  • the primary means for temperature control in the reaction is through the removal of condensate to the reaction steam, that is steam attemperation by progressively diverting the condensate to a spray nozzle installed in the vapour condenser/steam generator.
  • the final steam temperature exiting the vapour condenser/steam generator is monitored to ensure it does not fall below 250°C in order to avoid condensate droplet formation. It is important that the system is operated so that it does not result in large thermal shocks, hence the maximum condensate flow is limited through appropriate pipe size selection and the configuration and operation of the automatic control system.
  • Electric heating elements in both the upper and lower sections of the first steam generator vessel are used for start-up.
  • the lower elements generates saturated steam that the other element then superheats.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Hydrogen, Water And Hydrids (AREA)

Abstract

L'invention concerne un système fonctionnant de façon discontinue pour la production d'hydrogène, lequel comprend une cuve de combustible adaptée pour être utilisée en tant que réacteur, le combustible comprenant une source de combustible à base de fer, une entrée de vapeur vers la cuve de combustible pour introduire de la vapeur à haute température et haute pression, caractérisé en ce que ledit réacteur est un réacteur à lit fluidisé.
PCT/AU2008/000838 2007-06-12 2008-06-12 Système pour la production d'hydrogène WO2008151367A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
AU2007903150A AU2007903150A0 (en) 2007-06-12 A System for the Production of Hydrogen
AU2007903150 2007-06-12

Publications (1)

Publication Number Publication Date
WO2008151367A1 true WO2008151367A1 (fr) 2008-12-18

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PCT/AU2008/000838 WO2008151367A1 (fr) 2007-06-12 2008-06-12 Système pour la production d'hydrogène

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Country Link
WO (1) WO2008151367A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017105692A (ja) * 2015-07-08 2017-06-15 フレンド株式会社 水素ガス発生装置
JP2017190275A (ja) * 2016-04-15 2017-10-19 株式会社Ｋｓｆ 副生水素生成装置
JP2020506871A (ja) * 2017-02-03 2020-03-05 ギャラクシー エフシーティー スンディリアン ブルハド バッファタンクを備えた水素ガス発生システムおよび方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB130701A (en) * 1918-03-19 1919-08-14 R & J Dempster Ltd Improvements relating to Hydrogen Gas Plants.
GB902338A (en) * 1958-05-14 1962-08-01 Exxon Research Engineering Co Hydrogen production
JPH04318124A (ja) * 1991-04-17 1992-11-09 Sumitomo Metal Ind Ltd 鉄系スクラップの再利用方法
WO1993022044A2 (fr) * 1992-04-24 1993-11-11 H-Power Corporation Systeme perfectionne de production d'hydrogene
US20030072705A1 (en) * 2001-03-06 2003-04-17 Kindig James Kelly Method for the production of hydrogen and applications thereof
JP2005112704A (ja) * 2003-10-06 2005-04-28 Ryozo Oshima 水素ガス発生装置及び水素ガス供給装置
JP2007112672A (ja) * 2005-10-21 2007-05-10 Toho Gas Co Ltd 水素製造装置および水素製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB130701A (en) * 1918-03-19 1919-08-14 R & J Dempster Ltd Improvements relating to Hydrogen Gas Plants.
GB902338A (en) * 1958-05-14 1962-08-01 Exxon Research Engineering Co Hydrogen production
JPH04318124A (ja) * 1991-04-17 1992-11-09 Sumitomo Metal Ind Ltd 鉄系スクラップの再利用方法
WO1993022044A2 (fr) * 1992-04-24 1993-11-11 H-Power Corporation Systeme perfectionne de production d'hydrogene
US20030072705A1 (en) * 2001-03-06 2003-04-17 Kindig James Kelly Method for the production of hydrogen and applications thereof
JP2005112704A (ja) * 2003-10-06 2005-04-28 Ryozo Oshima 水素ガス発生装置及び水素ガス供給装置
JP2007112672A (ja) * 2005-10-21 2007-05-10 Toho Gas Co Ltd 水素製造装置および水素製造方法

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
DATABASE CAPLUS [online] JUNG ET AL.: "Hydrogen production from steam decomposition by wustite at elevated temperatures", accession no. STN Database accession no. (139:38582) *
DATABASE JAPIO [online] accession no. STN Database accession no. (1992-318124) *
DATABASE JAPIO [online] accession no. STN Database accession no. (2005-112704) *
DATABASE JAPIO [online] accession no. STN Database accession no. (2007-112672) *
TAECHAN KUMSOK, CHAERYO HAKOECHI, vol. 40, no. 11, 2002, pages 1223 - 1227 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2017105692A (ja) * 2015-07-08 2017-06-15 フレンド株式会社 水素ガス発生装置
JP2017190275A (ja) * 2016-04-15 2017-10-19 株式会社Ｋｓｆ 副生水素生成装置
JP2020506871A (ja) * 2017-02-03 2020-03-05 ギャラクシー エフシーティー スンディリアン ブルハド バッファタンクを備えた水素ガス発生システムおよび方法

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