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United States Patent (19) 11 3,969,493 Fujii Et Al

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United States Patent (19) 11 3,969,493 Fujii Et Al United States Patent (19) 11 3,969,493 Fujii et al. (45) July 13, 1976 54 THERMOCHEMICAL PROCESS FOR MANUFACTURE OF HYDROGEN AND Primary Examiner-Earl C. Thomas OXYGEN FROM WATER Attorney, Agent, or Firm-Kurt Kelman 75 inventors: Kinjiro Fujii, Komae; Wakichi Kondo, Kanagawa, both of Japan (57) ABSTRACT Calcium hydroxide and iodine are reacted with each 73) Assignee: Agency of Industrial Science & other in the presence of water to produce calcium io Technology, Tokyo, Japan date and calcium iodide, the former of which precipi 22 Filed: June 20, 1975 tates from the reaction solution and is obtained by fil tration and the latter of which is thereafter separated (21) Appl. No.: 588,873 from the filtrate by evaporation separation. The cal cium iodate is heated until it is converted into calcium (30) Foreign Application Priority Data oxide, whereafter there ensues generation of a mixed gas of iodine and oxygen. The mixed gas is cooled June 2, 1974 Japan................................ 49-7097 causing the iodine component thereof to solidify and (52) U.S. Cl................................. 423/579; 423/475; pure oxygen gas is consequently liberated to be ob tained as one product. The calcium iodide is solidified 423/481; 423/497; 4231507; 423/648 and subsequently heated under a current of steam to (5) Int. C.’.......................................... C01B 13/00 cause it to undergo conversion into calcium oxide with 58 Field of Search........... 423/579, 648, 475, 497, liberation of hydrogen iodide gas. The hydrogen io 423/507, 48 dide gas thus liberated is then separated by a known 56 - References Cited method into iodine and hydrogen which is obtained as another product. The calcium oxide and iodine re UNITED STATES PATENTS maining after separation of oxygen and hydrogen are 382,358 6/1974 Interrante et al................... 4231579 recycled to serve again as starting reactants. 3,839,550 1 011974 Wentorf, Jr......................... 4231579 3,842, 164 (). 1974 Wentorf, Jr......................... 4231579 6 Claims, 1 Drawing Figure i:"...r.o. c. - U.S. Patent July 13, 1976 3,969,493 zIeOgsz(EOI)eo Ca lz nH2O Oe0 3,969,493 1 2 thermal energy is involved. Even in this stage, the con THERMOCHEMICAL PROCESS FOR centration of the filtrate can be increased to an ex MANUFACTURE OF HYDROGEN AND OXYGEN tremely high level in the case of this process. Accord FROM WATER ingly, the energy consumption involved in this process is notably small as compared with that involved in the BACKGROUND OF THE INVENTION conventional process for the manufacture of oxygen The present invention relates to a thermochemical and hydrogen from water. process for the manufacture of hydrogen and oxygen Other objects and other characteristic features of the from water. '.. present invention will become apparent from the de A cycle for the production of hydrogen by virtue of 10 scription to be given in further detail herein below with the oxidation reaction of iodine has been suggested by reference to the accompanying drawing. Abraham and Schridnir Science, 180959 (1973). In this cycle, lithium nitrite is oxidized by iodine at about BRIEF EXPLANATION OF THE DRAWING 27C to produce lithium nitrate and hydrogen iodide, The drawing represents a flow sheet illustrating one so that hydrogen iodide produces hydrogen through 15 preferred embodiment of the process of this invention. thermal dissociation and lithium nitrate produces oxy gen through thermal decomposition respectively. The DETALED DESCRIPTION OF THE INVENTION oxidation of lithium nitrite by iodine involved in this The thermochemical process for the manufacture of cycle, however, can hardly be described as proceeding hydrogen from water is underlain by a principle that in smoothly. This utiliation of lithium, therefore, can 20 several chemical reactions involved therein which are hardly be called advantageous from the standpoint of effected by virtue of thermal energy, all the substances natural resources. participating in said reactions are invariably recycled An object of the present invention is to provide a with the exception of water so as to have water eventu thermochemical process for the manufacture of hydro ally separated into hydrogen and oxygen. gen and oxygen from water, said process being such 25 The inventors pursued a study in search for a method that it involves only a few unit reactions which invari whereby hydrogen and oxygen are thermochemically ably proceed smoothly to give reaction products capa produced from water by virtue of the redox reaction of ble of being separated by easy operations. iodine. They have, consequently, discovered that by Another object of this invention is to provide a ther use of iodine and calcium or barium hydroxide, the unit mochemical process for the manufacture of hydrogen 30 reactions involved invariably proceed more...safely with and oxygen from water, said process being such that higher operational ease than those involved in the con the process involves less consumption of thermal en ventional process using iodine and lithium nitrate and ergy than the conventional method and, therefore, that the iodine and calcium (or barium) oxide remain proves advantageous from the economical point of ing after recovery of oxygen and hydrogen can be recy view. 35 cled to the reaction system for further use in the pro cess. The present invention has been accomplished on SUMMARY OF THE INVENTION the basis of this discovery. To be specific, the process To accomplish the aforementioned objects, the pre of the present invention comprises the four unit reac sent invention provides a process which comprises the tions indicated below to produce hydrogen and oxygen steps of allowing iodine and calcium hydroxide to react 40 from water while having iodine and calcium oxide recy with each other in the presence of water at 20 to cled through the reaction system. 100°C, separating calcium iodate and calcium iodide from the resultant reaction product, heating calcium 6CaO + 61, -->Ca(IO) + 5Cal, (1) iodate until it is converted into calcium oxide for thereby generating a mixed gas of iodine and oxygen, 45 Ca(IO), CaO + -- 2.50, (2) cooling the generated mixed gas thereby allowing the iodine component thereof to be educed in the form of 5Cal, +SHO-5CaO + 10H (3) crystals and simultaneously effecting liberation of oxy 10HI-> 5H, +51, (4) gen gas therefrom, causing calcium iodide to react with steam at 400 to 750°C to give rise to hydrogen iodine 50 First, iodine and calcium oxide are mixed in the pres and decomposing the generated hydrogen iodide into ence of water and the resultant mixture is heated with hydrogen and iodine. Thus, the number of unit reac simultaneous agitation to about 20 to 100°C. Conse tions involved therein is small and the individual reac quently, there ensues a reaction of the formula (1) to tions require absolutely no harsh conditions. Thus, the produce calcium iodate (Ca(IO),) and calcium iodide reactions proceed smoothly and the separation and 55 (Cal.). The former compound is rather sparingly solu recovery of oxygen gas and hydrogen gas from the ble in water and, therefore, settles to the bottom of the reaction products are accomplished with ease. Further reaction mixture. The latter compound is readily solu since the iodine and calcium oxide remaining in the ble in water and remains suspended in the reaction reaction system can be recycled for further use in this mixture. The two compounds, therefore, can easily be process, it is water alone that is actually consumed in 60 separated as by filtration, for example. In the reaction the whole course of the process. The process proves described above, the produced calcium iodide is sepa advantageous also in this respect. In all the unit reac rated and recovered by a process of evaporation, as will tions of the process of this invention, the highest tem be described afterward, from the reaction mixture. In perature at which any heating is performed at all is this connection, the amount of thermal energy to be about 800°C. If barium is used, all the reactions can be 65 consumed in the process of evaporation decreases with carried out satisfactorily at temperatures lower than the increasing concentration of said compound in the 700°C. It is only in the stage of recovery of calcium mixture. If iodine and calcium hydroxide are subjected iodide from the filtrate that a heavy consumption of to said reaction at high concentration satisfying their 3.969,493 3 4 stoichiometric proportion so that the concentration of permits iodine and calcium oxide to be used cyclically the produced calcium iodide in the resultant mixture through the process thereof without being consumed at exceeds 35% (at 90°C), then undesirable substances all in the said unit reactions. such as 3Ca(OH)2, Cal and Ca(IO)3~4HO are Now, one working example of the process of this by-produced in the mixture. As these substances pre invention will be described with reference to the at cipitate, in solid phase, it becomes more difficult to tached fow sheet. recover calcium iodide from the mixture in proportion In the flow, sheet, a reaction tank 1 containing water to the amount of these substances produced. When the is charged with iodine and calcium oxide. The contents reaction described above is carried out by using therein are now heated to about 90°C with simultaneous agita iodine in an excess amount of from 1.5 to 4 times as 10 tion, with the result that a precipitate occurs in the large as is stoichiometrically required on the basis of reaction solution. The reaction solution is forwarded to the amount of calcium oxide in use therefore, calcium a filter 2 to be separated into the precipitate. and the iodate in the form of a precipitate and calcium iodide in filtrate.
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