WO1981002004A1 - Materiau et procede de dissociation de l'eau - Google Patents

Materiau et procede de dissociation de l'eau Download PDF

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Publication number
WO1981002004A1
WO1981002004A1 PCT/US1981/000038 US8100038W WO8102004A1 WO 1981002004 A1 WO1981002004 A1 WO 1981002004A1 US 8100038 W US8100038 W US 8100038W WO 8102004 A1 WO8102004 A1 WO 8102004A1
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Prior art keywords
weight
alloy
amalgam
further characterized
inert atmosphere
Prior art date
Application number
PCT/US1981/000038
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English (en)
Inventor
E Anderson
Original Assignee
Horizon Mfg Corp
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 Horizon Mfg Corp filed Critical Horizon Mfg Corp
Priority to AU67735/81A priority Critical patent/AU6773581A/en
Publication of WO1981002004A1 publication Critical patent/WO1981002004A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C7/00—Alloys based on mercury
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/02—Preparation of oxygen
    • C01B13/0203—Preparation of oxygen from inorganic compounds
    • C01B13/0207—Water
    • 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
    • C01B3/08—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 with metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C24/00—Alloys based on an alkali or an alkaline earth metal
    • 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

  • This invention relates to a material for and method of effecting the decomposition/dissociation of water into hydrogen and oxygen.
  • the water is reacted with an amalgam of sodium, aluminun and mercury to form hydrogen and a metallic hydroxide denoted by the formula Na 3 AL(OH) 6 is unstable at the temperature of formation in the presence of a catalyst comprising platinum and at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium, cadmium, bismuth, lead, zinc, and tin and breaks down to form metallic sodium and aluminum thereby releasing oxygen and hydrogen.
  • Thermochemical cycles comprising metal-metaloid combinations for the generating of both hydrogen and oxygen are disclosed in U. S. Patent 3,969,495. Closed cycle processes for dissociation of water into hydrogen and oxygen are disclosed in U. S. Patents 3,821,358, 3,928,549 and 4,011,305. Combinations of various metals in multistep processes for dissociation of water are, therefore, well known; however, the simple and facile manner of producing hydrogen and oxygen utilizing an amalgam of alkali metal, aluminum and mercury combined with a catalytic alloy comprising platinum and at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium, cadmium, bismuth, lead, zinc, and tin has not been heretofore appreciated.
  • the material I have found to be suitable for the generation of hydrogen and oxygen from water without spon taneous combustion of the resultant evolved hydrogen and oxygen gases comprises an amalgam of (1) an alkali metal such as lithium, sodium, potassium, cesium, or combinations thereof, (2) aluminum and (3) mercury combined with a catalytic alloy comprising a metal selected from the platinum metals family and at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium, cadmium, bismuth, lead, zinc and tin.
  • an alkali metal such as lithium, sodium, potassium, cesium, or combinations thereof
  • aluminum and (3) mercury combined with a catalytic alloy comprising a metal selected from the platinum metals family and at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium, cadmium, bismuth, lead, zinc and tin.
  • the particle size of the sodium and aluminum is such as to enable formation of an amalgam and may fall within the range of from about 10 to about 100 mesh. Most preferably, the particle size of the aluminum should be about 10 mesh. Alkali metal of 1/4" diameter is suitable. The particle size of either the alkali metal or aluminum is not critical since the foregoing metals and mercury readily intermix. The smaller the particle size, of course, the more rapid the mixing.
  • the atomic weight ratio of alkali metal to mercury is from about 1:100 to about 100:1 and the atomic weight ratio of alkali metal to aluminum is from about 1:100 to about 100:1.
  • the atomic weight ratio of alkali metal to mercury is from about 3:1 to about 1:1.5 and the atomic weight ratio of alkali metal to aluminum is from about 1:1 to about 3:1.
  • the amalgam of alkali metal, aluminum and mercury is combined with a catalytically active alloy which is present in a catalytically effective amount and, at the conditions of hydrogen generation, functions to regenerate amalgam to the active metallic state. It is essential that the catalyst/alloy contain a platinum group metal.
  • the catalyst/alloy is generally comprised of a metal selected from the platinum metals family or group and at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium, cadmium, bismuth, lead, zinc, and tin.
  • the catalyst comprises at least one element selected from the group consisting of germanium, antimony, gallium, thallium, indium and cadmium.
  • Catalytic activity is further enhanced by the addition of minor amounts of zirconium and chromium.
  • Lead and/or gold may be incorporated in the catalyst as an alloying element to lower the melting point of the alloy.
  • the alloy and amalgam may be combined in weight ratios of from about 1:1 to about 1:5 and preferably from about 1:2 to about 1:3.
  • the alloy and amalgam may be compounded with an extender.
  • the extender functions both to dilute the amalgam-catalytic alloy combination and to provide a heat sump for heat generated during the dissociation of water by contact with the combined amalgam and catalytic alloy.
  • the extender is preferably copper; however, admixtures of tin and bismuth or gallium may also function as extenders.
  • the combination of amalgam and alloy or amalgam, alloy and extender is most suitably used in solid block form, hereinafter referred to as a reactor block. Where an extender is employed it may be present as a major constituent of the reactor block.
  • the water reacts with the alkali metal, e.g., sodium, and the aluminum liberating hydrogen and forming Na 3 AL(OH) 6 .
  • the Na 3 AL(0H) 6 is unstable, and in the presence of the alloy at the conditions of Na 3 AL ⁇ OH) 6 formation, the foregoing composition decomposes to form H 2 , O 2 and regenerated amalgam.
  • the alloy apparently functions to. catalyze the decomposition, and thereby extends the useful life of the amalgam.
  • the process may be depicted as follows: 2 Na + 2 H 2 O ⁇ 2 NaOH + H 2
  • chromium as an additional component of the alloy.
  • the incorporation of chromium as a component of the alloy appears to lower the heat of reaction.
  • the chromium is generally present in the alloy in an amount measured on a weight percent basis of said alloy of from about 0.7% to about 1.1% and preferably for about 0.8% to about 0.9%.
  • Each of the components of the alloy may be present in amounts of from about 0.4% by weight to about 28.5% by weight based on the weight of the combined catalytic alloy and amalgam.
  • the preferred alloy comprises (1) a metal selected from the platinum metals group present in an amount of from about 0.4 to about 2.3% by weight, (2) lead present in an amount of from about 42.9 to about 71.5% by weight, (3) antimony present in an amount of from about 25.5 to about 42.5% by weight, (4) chromium present in an amount of from about 0.7 to about 1.1% by weight, (5) zirconium present in an amount of from about 4.1 to about 6.8% by weight and gold present in an amount of from about 0.6 to about 2.3% by weight.
  • a specific example of said preferred alloy comprises about 1.4 weight percent of the selected platinum group members, about 57.3 weight percent lead, about 34.0 weight percent antimony, about 0.9 weight percent chromium, about 5.4 weight percent zirconium and about 1.0 weight percent gold.
  • the amalgam of sodium, aluminum and mercury is prepared utilizing any of the well known procedures with the added proviso that an inert atmosphere be employed. Amalgarmation may be facilitated by utilization of an elevated temperature, preferably around 200° C ⁇ 10° C. The amalgam is preferably maintained at this elevated temperature for about 10 minutes where 100 grams are being processed, and the time is extended about 1 minute for each additional 100 gram aliquot.
  • the resulting amalgam is cooled, generally to room temperature, utilizing an inert atmosphere.
  • an inert atmosphere for this purpose either helium or nitrogen are satisfactory. Cool ing is preferably effected in a desiccator to insure that no water contacts the amalgam.
  • the preparation of the alloy selected may be in any well known manner having in mind the proviso that an inert atmosphere be maintained.
  • the alloy upon solidification, and as a practical matter, upon cooling is ground into a powder, preferably a fine powder of about 10 mesh or less. Cooling may be effected in a dessicator to insure the absence of oxygen and moisture, whose presence is detrimental during preparation. Grinding/pulverizing may be effected in any well known manner including use of a ball, hammer and/or stamp mill.
  • the objective in combining the alloy and amalgam is to intimately admix the two respective components.
  • the specific manner of catalysis is not known, but generally catalysis is a surface phenomenon and consistent therewith in the instant invention it appears that the catalysis is related to both particle size and nature as well as uniformity of mixture of the amalgam and catalytic alloy.
  • the amalgam and catalytic alloy may be used (1) in particulate form such as a floating bed, or other intimate dispersion, (2) in the form of porous mass which may be formed by compression or sintering or (3) as a solid mass by alloying of the amalgam and catalytic alloy.
  • alloying it is meant that the amalgam and catalytic alloy are combined to form an admixture and alloyed under inert conditions at a temperature above the melting point of said admixture.
  • an extender such as gallium, tin, bismuth or copper, and preferably copper may be utilized.
  • the extender functions to vary activity and as a heat sink to retain at least a portion of the heat of reaction of sodium aluminum hydroxide formation, whereby catalysis of the unstable hydroxide to the metal and oxygen and hydrogen is enhanced.
  • Admixture of extender with the amalgam and catalytic alloy is effected Utilizing the extender in a particulate form of comparable size to the other components, which size is generally from about 10 to about 100 mesh.
  • the resulting amalgam is cooled to room temperature in a dessicator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a dessicator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by passing steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10° C above the melting point of the mass and maintained at said temperature for about 10 ⁇ 1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a dessicator wherein an inert atmosphere is maintained and the mass is allowed to cool.
  • the resulting block is ready for use.
  • amalgam and alloy prepared above and an extender of powdered copper of about 10 mesh are admixed in the following proportions:
  • the resultant mixture is compressed to form a solid mass by application of pressure of about: 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an eleuated temperature of about 10° C. above the melting point of the mass and this temperature is maintained for about 10 ⁇ 1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained.
  • the resulting block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.14 gallons of water per minute.
  • the resulting amalgam is cooled to room temperature in a dessicator in an inert nitrogen atmosphere. There after, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by passing steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resulting block is heated to an elevated temperature of about 10° C above the melting point of the mass and maintained at said temperature for about 10 ⁇ 1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a dessicator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling the resultant block is ready for use.
  • amalgam and alloy prepared above and an extender of powdered copper of about 10 mesh are admixed in the following proportions:
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10 ⁇ 1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained. Upon cooling the resultant block is ready for use.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.20 gallons of water per minute.
  • An amalgam comprising 22.947 parts by weight of aluminum, 18.391 parts by weight sodium and 58.662 parts by weight mercury is formed in a graphite crucible in an inert atmosphere of nitrogen at an elevated temperature of 200°C.
  • the resulting amalgam is cooled to room temperature in a dessicator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by immmersion in water whereby water is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and a powdered extender comprising 50 weight percent tin and 50 weight percent bismuth of about 10 mesh are admixed in the following proportions: 21.775 parts by weight amalgam. 5.625 parts by weight alloy. 72.6 parts by weight copper.
  • the weighing and blending of the foregoing metallie compounds should be done in an inert atmosphere. After blending to provide a uniform mixture, the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.12 gallons of water per minute.
  • EXAMPLE IV Preparation of Amalgam An amalgam comprising 19.383 parts by weight aluminum, 31.068 parts by weight potassium and 49.549 parts by weight mercury is formed in a graphite crucible in an inert atmosphere of nitrogen at an elevated temperature of 200°C.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by spraying water on the admixture whereby water is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to. cool. Upon cooling, the resultant block is ready for use.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained. Upon cooling the resultant block is ready for use.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the caseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is depen dent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.14 gallons of water per minute.
  • An amalgam comprising 37.688 parts by weight aluminum, 32.112 parts by weight cesium and 30.2 parts by weight mercury is formed in a graphite crucible in an inert atmosphere of nitrogen at an elevated temperature of 200°C.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere.
  • the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen. It is important to prepare the amalgam in an inert gas atmosphere to prevent hydroxide formation.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmos phere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and an extender of powdered gallium of about 10 mesh are admixed in the following proportions:
  • the weighing and blending of the foregoing metallie compounds should be done in an inert atmosphere.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the crucible and its contents are trandferred to a desiccator wherein an inert atmosphere is maintained.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity there Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric en vironment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.20 gallons of water per minute.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by passing steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resulting block is heated to an elevated temper ature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out in an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "noison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • amalgam and alloy prepared above and an extender of powdered gallium of about 10 mesh are admixed in the following proportions:
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained. Upon cooling the resultant block is ready for use.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.15 gallons of water per minute.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by passing steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desic cator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and an extender pf powdered gallium of about 10 mesh are admixed in the following proportions:
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained. Upon cooling the resultant block is ready for use.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.12 gallons of water per minute.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes. in the oven utilized for heating, an inert atmosphere is maintained. Thereafter, the mass comprised of amalgam and alloy. is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and a powdered extender comprising 50 weight percent of tin and 50 weight percent of bismuth of about 10 mesh are admixed in the following proportions:
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.25 gallons of water per minute.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and catalytic alloy.
  • the admixture may be utilized by steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the. oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and extender of powdered gallium of about 10 mesh are admixed in the following proportions: 21.775 parts by weight amalgam. 5.678 parts by weight alloy. 72.547 parts by weight gallium.
  • the weighing and blending of the foregoing metallie compounds should be done in an inert atmosphere. After blending to provide a uniform mixture, the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.08 gallons of water per minute.
  • An amalgam comprising 37.688 parts by weight of aluminum, 32.112 parts by weight cesium and 30.2 parts by weight mercury is formed in a graphite crucible in an inert atmosphere of nitrogen at an elevated temperature of 200°C.
  • the resulting amalgam is cooled to room temperature in a desiccator in an inert nitrogen atmosphere. Thereafter, the amalgam is formed into a fine powder of about 10 mesh utilizing a ball mill. Grinding is effected in an inert atmosphere of nitrogen.
  • the resulting alloy is cooled in a desiccator to about room temperature in an inert helium atmosphere. Thereafter the amalgam is formed into a fine powder of about 10 mesh or less utilizing a ball mill. Grinding is effected in an inert atmosphere of helium.
  • the inert atmosphere is used to prevent oxidation of the alloy.
  • Three parts by weight of powdered amalgam is admixed with one part by weight powdered alloy in an inert atmosphere to obtain a uniform mixture of the amalgam and cata lytic alloy.
  • the admixture may be utilized by passing steam upwardly therethrough whereby steam is dissociated into hydrogen and oxygen.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the mold utilized produces a cubical block.
  • the resulting block is heated to an elevated temperature of about 10°C above the melting point of the mass and maintained at said temperature for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the mass comprised of amalgam and alloy is transferred to a desiccator wherein an inert atmosphere is maintained and the mass is allowed to cool. Upon cooling, the resultant block is ready for use.
  • amalgam and alloy prepared above and extender of powdered copper of about 10 mesh are admixed in the following proportions:
  • the weighing and blending of the foregoing metallie compounds should be done in an inert atmosphere.
  • the resultant mixture is compressed to form a solid mass by application of pressure of about 40,000 pounds per square inch in a graphite mold conforming to the desired shape of the finished product.
  • the compressed mass in a crucible conforming to the shape thereof is heated to an elevated temperature of about 10°C above the melting point of the mass and this temperature is maintained for about 10+1 minutes.
  • an inert atmosphere is maintained in the oven utilized for heating.
  • the crucible and its contents are transferred to a desiccator wherein an inert atmosphere is maintained.
  • the resultant block is ready for use.
  • the entire foregoing procedure should be carried out under an inert atmosphere such as helium or nitrogen and in the absence of contaminants. Oxidation of the metallic components and/or hydroxide formation will "poison" the resulting reactor block and reduce the activity thereof. Moreover, during the steps of the process operated at elevated temperature, the presence of any oxygen will cause the mass to ignite.
  • the reactor blocks are contacted with a fine spray of water at about room temperature in an atmospheric environment.
  • the gaseous effluent from said contact comprises hydrogen and oxygen and burns when subjected to electrical sparking.
  • the volume of gas evolved is dependent on the reactor block surface area and the volume of water impinging thereon. Generally a 2.5 square cm surface will react with 0.22 gallons of water per minute.

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Abstract

Un materiau et un procede de decomposition/dissociation de l'eau en hydrogene et en oxygene sont decrits. Le materiau consiste en un amalgame de metal alcalin, de mercure, et d'aluminium combines avec une quantite a effet catalytique d'un alliage comprenant un metal choisi parmi les metaux de la famille du platine et au moins un metal choisi parmi le groupe constitue par le germanium, l'antimoine, le gallium, le thallium, l'indium, le cadmium, le bismuth, le plomb, le zinc et l'etain.
PCT/US1981/000038 1980-01-07 1981-01-07 Materiau et procede de dissociation de l'eau WO1981002004A1 (fr)

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Application Number Priority Date Filing Date Title
AU67735/81A AU6773581A (en) 1980-01-07 1981-01-07 Water dissociation method and material

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US110217 1980-01-07
US06/110,217 US4287169A (en) 1978-05-04 1980-01-07 Water dissociation method and material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4588577A (en) * 1984-03-20 1986-05-13 Cardinal Earl V Method for generating hydrogen
US20180370795A1 (en) * 2016-06-22 2018-12-27 Earl Lorenzo Hamm Apparatus and method for hydrogen production from an alkali metal and hydrogen dioxide
CN109133000A (zh) * 2018-08-23 2019-01-04 杭州氢源素生物科技有限公司 一种铝基微纳米复合水解制氢材料
CN109694962A (zh) * 2019-01-29 2019-04-30 大连理工大学 一种Al合金铸锭、其制备方法及用途

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR337722A (fr) * 1903-12-14 1904-04-22 Narcisse Alfred Helouis Système d'éclairage à incandescence par application des alliages d'aluminium et autres alliages équivalents
GB190903188A (en) * 1909-02-09 1909-09-30 George William Johnson Improvements in Means for the Preparation of Pure Hydrogen.
US2083648A (en) * 1932-02-25 1937-06-15 Ig Farbenindustrie Ag Preparation of alkali metal hydroxide solutions
US2837408A (en) * 1954-06-29 1958-06-03 Olin Mathieson Process and apparatus for the catalytic decomposition of alkali metal amalgams
US3313598A (en) * 1965-06-07 1967-04-11 Ethyl Corp Method of controlled hydrogen generation
US3490871A (en) * 1965-10-19 1970-01-20 Aerojet General Co Process for producing hydrogen from water using an alkali metal
US3540854A (en) * 1967-05-26 1970-11-17 United Aircraft Corp Metal-water fueled reactor for generating steam and hydrogen
US3833357A (en) * 1970-11-24 1974-09-03 Oronzio De Nora Impianti A process for decomposing alkali metal amalgams into mercury, hydrogen and alkali metal hydroxide solutions
US3985866A (en) * 1974-10-07 1976-10-12 Hitachi Shipbuilding And Engineering Co., Ltd. Method of producing high-pressure hydrogen containing gas for use as a power source
WO1979001031A1 (fr) * 1978-05-04 1979-11-29 Anderson Energy Systems Inc Materiau et procede de dissociation de l'eau
US4182748A (en) * 1978-05-04 1980-01-08 Horizon Manufacturing Corporation Material and method for obtaining hydrogen and oxygen by dissociation of water
US4207095A (en) * 1978-05-04 1980-06-10 Horizon Manufacturing Corporation Material and method for obtaining hydrogen by dissociation of water

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR337722A (fr) * 1903-12-14 1904-04-22 Narcisse Alfred Helouis Système d'éclairage à incandescence par application des alliages d'aluminium et autres alliages équivalents
GB190903188A (en) * 1909-02-09 1909-09-30 George William Johnson Improvements in Means for the Preparation of Pure Hydrogen.
US2083648A (en) * 1932-02-25 1937-06-15 Ig Farbenindustrie Ag Preparation of alkali metal hydroxide solutions
US2837408A (en) * 1954-06-29 1958-06-03 Olin Mathieson Process and apparatus for the catalytic decomposition of alkali metal amalgams
US3313598A (en) * 1965-06-07 1967-04-11 Ethyl Corp Method of controlled hydrogen generation
US3490871A (en) * 1965-10-19 1970-01-20 Aerojet General Co Process for producing hydrogen from water using an alkali metal
US3540854A (en) * 1967-05-26 1970-11-17 United Aircraft Corp Metal-water fueled reactor for generating steam and hydrogen
US3833357A (en) * 1970-11-24 1974-09-03 Oronzio De Nora Impianti A process for decomposing alkali metal amalgams into mercury, hydrogen and alkali metal hydroxide solutions
US3985866A (en) * 1974-10-07 1976-10-12 Hitachi Shipbuilding And Engineering Co., Ltd. Method of producing high-pressure hydrogen containing gas for use as a power source
WO1979001031A1 (fr) * 1978-05-04 1979-11-29 Anderson Energy Systems Inc Materiau et procede de dissociation de l'eau
US4182748A (en) * 1978-05-04 1980-01-08 Horizon Manufacturing Corporation Material and method for obtaining hydrogen and oxygen by dissociation of water
US4207095A (en) * 1978-05-04 1980-06-10 Horizon Manufacturing Corporation Material and method for obtaining hydrogen by dissociation of water

Also Published As

Publication number Publication date
EP0042874A1 (fr) 1982-01-06
US4287169A (en) 1981-09-01
OA06386A (fr) 1981-08-31

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