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United States Patent (19) 11 3,970,745 Takeuchi (45) July 20, 1976

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United States Patent (19) 11 3,970,745 Takeuchi (45) July 20, 1976 United States Patent (19) 11 3,970,745 Takeuchi (45) July 20, 1976 (54) METHOD FOR PRODUCING HYDROGEN son, vol. 3, 1949 Ed., p. 535, Reinhold Pub. Corp., FROM WATER New York. 75) Inventor: Norio Takeuchi, Isehara, Japan P. Pascal's “Nouveau Traite' de Chimie Minerale', Tome 8, 1963, pp. 54, 55; Masson et Cie., Paris, 73 Assignee: Director-General of the Agency of France. Industrial Science and Technology, J. W. Mellor's "A Comp. Treatise on Inorg. and Theo. Tokyo, Japan Chem.", vol. 7, Longmans, Green & Co., N. Y. 22 Filed: Mar. 24, 1975 Primary Examiner-Edward Stern (21 Appl. No.: 561,161 Attorney, Agent, or Firm-William J. Daniel 30 Foreign Application Priority Data 57 ABSTRACT May 9, 1974 Japan................................ 49-51.538 A method for producing hydrogen from water in May 17, 1974 Japan................................ 49-54504 which hydrogen is produced by reducing water using metallic germanium and the by-product, germanium 52 U.S. Cl................................... 423/657; 423193; monoxide, is reduced with a reducing agent to metal 423/532; 423/539; 423/655; 4231592 lic germanium which is recycled and reused. In this 51) Int. C.’.................so e s so C01B 1/07; COB 1102; case, it is necessary to regulate the oxidation of metal CO1G 7700 lic germanium so as to stop at the germanium monox (58) Field of Search............. 423/657, 539, 532, 93, ide stage since the reduction of germanium dioxide to 423/592 metallic germanium is difficult. Therefore, water 56) References Cited vapor is advantageously reduced by using not less than 1 mole of metallic germanium to 1 mole of water OTHER PUBLICATIONS vapor or it is indirectly reduced with an intermediate "Comp. Inorg. Chem.', by J. C. Bailar et al., 1973 of carbon dioxide. Ed., p. 8, Pergamon Press, Elsmford, New York. “Encyclopedia of Chem. Reactions", by C. A. Jacob 5 Claims, No Drawings 3,970,745 2 1 water vapor to react thermally with 1 or more moles of METHOD FOR PRODUCING HYDROGEN FROM metallic germanium. s WATER . ; In this case, it is necessary to use the metallic germa nium as a reducing agent in order to carry out the BACKGROUND OF THE INVENTION thermal decomposition of water with mild but efficient This invention relates to a method for producing conditions. When the metallic germanium is used, hydrogen from water. More particularly, the invention water can be thermally decomposed at a relatively relates to a method of a closed system for continuously lower temperature in the range of about 300 to 900°C. producing hydrogen from water vapor, in which the The reaction between water and metallic, germanium latter is reduced to hydrogen in the presence of metal 10 according to the method of the present invention is lic germanium as a reducing agent and the germanium represented by the following reaction equation: monoxide generated as a by-product is then reduced to metallic germanium to be recycled. Ge + H.O - Geo +H, (1) In recent years, a serious world-wide problem has arisen in that oil resources are running low and this 5 In the practice of this reaction, the ratio of germanium problem has been taken up in order to alleviate same. to water must be set at a value not less than 1 in molar As the material to take the place of the oil resources, ratio, and preferably more than 2, so as to form easily several energy sources such as nuclear energy, solar reducible germanium monoxide. When this molar ratio energy, geothermal energy' and hydrogen energy are is less than 1, a by-product of germanium dioxide 20 (GeO) is formed and it is extremely difficult to reduce now being eagerly investigated. Above all, hydrogen this germanium dioxide to metallic germanium, which energy has an advantage in that it can be abundantly prevents the process from becoming a completely produced from infinitely existing water. In addition, it closed system. can be easily stored and transported since it is chemical The metallic germanium is used in the form of pow energy. Further, this hydrogen energy can be employed 25 der and the larger the ratio to water is, the larger the for a variety of purposes such as cooking fuel and heat yield of hydrogen becomes. The reaction between me ing fuel as well as automobile fuel, aviation fuel, fuel tallic germanium and water can be carried out either in cell material and so forth. Still further, being different a batch-wise process or in a continuous process. The from the known fossil fuels, it does not produce any separation of hydrogen from reaction products is con poisonous or noxious gases such as carbon monoxide 30 siderably easy because the reaction is a solid-liquid when it is burned. system and solid-liquid separation means may be gener As disclosed in the above, hydrogen energy is quite ally employed. Further in this reaction, some water within the bounds of possibility as the substitute for oil vapor is contained in the produced hydrogen, but, how resources. In order to realize the use of hydrogen en ever, the water vapor can be easily removed from hy ergy, however, it is necessary to meet the demand to 35 drogen by cooling the reaction product. produce hydrogen at low cost and causing no environ According to the method of the present invention, mental hazards such as pollution of air, etc. the byproduct, germanium monoxide, is reduced to metallic germanium so as to be used for the above-. BRIEF SUMMARY OF THE INVENTION mentioned reaction (I) by recycling. This reduction Accordingly, it is an object of the present invention 40 treatment can be carried out by various methods. How to provide an improved method for producing hydro ever, in view of operation and economical efficiency of gen from water. , , , , ! : . the reaction process, it has been found that sulfur diox It is another object of the present invention to pro ide and cobaltous oxide can be advantageously used for vide a closed reaction system for continuously produc this purpose. ing hydrogen from water, in which water is reduced to 45 When sulfur dioxide is used as a reducing agent, the hydrogen by using metallic germanium and germanium reaction is represented by the following equation: monoxide as a by-product is then reduced to metallic germanium so as to be recycled and reused. Geo + So, - Ge+ so, (II) It is a further object of the present invention to pro vide a method for producing hydrogen by indirectly 50 This reaction is carried out at a temperature of 400 to reducing water with metallic germanium through the 800°C. A higher pressure of sulfur dioxide is preferable intermediate action of carbon monoxide, in which and the reaction is advantageously proceeded at a pres water is firstly reacted with carbon monoxide to pro sure higher than 100 atm. duce water gas, and generated carbon dioxide in the The sulfur trioxide produced through this reaction water gas is then reduced to carbon monoxide by me 55 (II) can be used as it is for several other purposes in tallic germanium. industrial production as a raw material. Meanwhile, in It is still a further object of the present invention to order to make the process a completely closed system, provide the selection of conditions of forming no ger it may be reduced to sulfur dioxide and recycled as the manium dioxide in order to effectively carry out the raw material of the above-mentioned reaction (II). In regeneration of the germanium monoxide to metallic 60 this case, various reducing agents can be theoretically germanium. used. However, the selection of the reducing agents is Other and further objects, features and advantages of important from an economical standpoint and closed the invention will appear more fully from the following system of the process. It has been found by the present description. - inventors that the powders of lead oxide, co-baltous 65. oxide and cuprous oxide are most suitable as such re DETAILED DESCRIPTION OF THE INVENTION ducing agents. These oxides react easily with sulfur In an embodiment of the method of the present in trioxide and in addition, the produced higher oxides vention, hydrogen is produced by causing 1 mole of decompose easily by heating and release oxygen gas. 3,970,745 3 4 When these metallic lower oxides are used as the re pletely closed system. The above-mentioned reaction ducing agents, the process can be made into a com between metallic germanium and carbon dioxide is pletely closed system as presented by the following represented by the following equation: equations: Ge -- CO --> GeO -- CO (VI) SO - (M)O -> SO -- (M).O. (III) When metallic germanium is reacted with carbon (M)O, -) (M)O + 4/20, (IV) monoxide, the ratio of germanium to carbon dioxide (Ge/CO) is to be a value not less than 1 in molar ratio. in which M is Pb, Co or Cu and m and n are integers If the above ratio is less than 1, germanium dioxide determined by the valences of metals. (GeO) is produced as a by-product. Being different The reaction temperatures of reactions (III) and (IV) from germanium monoxide, this germanium dioxide is are different according to metal used, while they are reduced with difficulty so that the closed system of the always lower than 1000°C, so that the reactions may be process cannot be accomplished. The metallic germa industrially carried out without any particular diffi 15 culty. That is, when M is lead, the raction (III) is pro nium is used in the form of powder and the larger quan ceeded at a temperature of 100 to 300°C and SO tity of metallic germanium used in proportion to the pressure of 50 atm or higher and the reaction (IV) is quantity of carbon dioxide, the higher the yield of car proceeded at a temperature of not lower than 300°C.
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