FINAL RAPORT Research, development and technologies for liquid hydrogen sulphide fuel cells to generate clean energy

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320 / 04. 10. 2006 CEEX Contractor principal: University Politehnica Bucharest Project manager: Partner Institutes: UPB

Eng. PhD. Adrian Teodorescu Ciocanea Partener 1 CO - University Politehnica Bucharest UPB, Partner 2 UB,

Mathematics Institute of Romanian Academy Partner 4 - INCDTCI - ICSI Rm. Valcea

IMAR, Partner 3 - University Bucharest

The main objective of the project consisted in research and developing technologies for a new fuel cell able to work with hydrogen sulphide. The target was to electrochemical oxidise the H2S from the Black Sea deep waters in-situ, in its liquid form, dissolved in salted water, at low concentrations and temperatures, 10C or less and high pressures, more than 2 MPa. The process is clean and neither specific forerunner operations (extraction, transportation, storage, fuel cleaning, fuel forming) nor risk of toxic effluents are involved. Project current stage: All the aimed specific objectives were reached. Thus: A scientific and technologic procedure for experiments was developed for various fuel cells to be tested, aiming the electrochemical oxidising of H2S from the Black Sea deep waters in-situ. A laboratory stand was realised for testing various pairs of electrodes and catalysts at variable H2S concentrations and ambient pressures. An autonomous submersible installation was designed and manufactured for in-situ testing of H2S fuel cell stacks. The fuel stack was made in conformity with the patent that originated the project. The installation was developed in accordance with the specifications for the above procedure implementation. It is able to perform at 200 meters depth and has few days autonomy. Porous and smooth electrodes loaded with specific catalysts for electrochemical oxidising of H2S (consisting in mixed MexSy, Me = Mo, Ni, W) were developed and tested. These studies initiated two new solutions in the thematic area. One refers to a method to obtain porous materials having pores controlled geometry. It makes the subject of the patent application submitted at OSIM, no A/00112/11.02.2008, title: Method to obtain porous electrodes , authors: O. Pacala, I. Stamatin, A. Teodorescu Ciocanea, M. Pacala. The other one refers to a method to load catalysts on smooth anodes (underway of checking before to be submitted at OSIM). All partners were equally been offered this opportunity. A H2S fuel cell stack was designed. It consists in sequential repeated modules, following the patented solution. (Pacala, O., Pacala, M., Ciocanea, A., Method and fuel cell to generate power RO 120736 B1/ 06. 2006).

The fuel cell stack was manufactured and tested. Various fuel cells behaviour were studied, all cells been dedicated to those cases when the fuel (H2S) is already mixed with the electrolyte. Cells having only one active electrode in PAFC configuration and PEM standard configuration have been tested. A methanol versus H2S dissolved in the electrolyte fuel cell comparative study was performed, in PEM standard configuration. Prototypes inherent technological problems were spotlighted. Since the problem supposes the miscible displacement of the electrolyte by the hydrogen sulphide, a first paperwork describing multiphase flows in porous medium was elaborated. By following the direction opened by the papers of Chavent, we gave a new formulation of the equations for the two-phase flows in the case of miscible fluids. In the non-miscible case, we showed that, for incompressible fluids, by introducing the classical hypotheses of relative permeability and capillary pressure, one could bring the equations in the same form as the equations for miscible fluids. Through an adequate management a technological network has been developed. The consortium partners are the main nodes of this network aiming clean power systems developing, improvement and innovation, as they were conceived during the common project activities. In this way, the competencies were identified: Theoretical research and mathematical simulation, Applied research at the physical and chemical phenomenon level, Porous electrodes manufacture, Manufacture of fuel cell stack constituent modules and testing on the reactor vessel, Ex-post analyses of the technological solutions.

Each phase notable results were disseminated through communications and articles within the framework of internal seminars, conferences and branch publications. A dedicated web page is under construction. Project contribution to the research infrastructure developing: A. Since special requests concerning both health legal providing and technical conditions had to be considered, the research infrastructure development has been directed as follows: 1. ICSI Rm. Valcea - FC Laboratories for tests and verifying, including simulation of work conditions (flows, temperatures, pressures); 2. UB 3 Nano Sae from Faculty of Physics Laboratories for electrodes preparing,

catalysts loading, preliminary tests and FC ex-post studies; 3. UPB Regenerative Power Supplies Laboratories from Faculty of Energetic for design

and verifying the new tests stand for in-situ experiments. The first two laboratories performed comparative experiments upon both standard configurations FC and patented one new. B. A stand for laboratory experiments was developed at ICSI Rm. Valcea. It was endowed with specific equipment able to ensure: the pressures control on both sides of membrane, electrolyte, fuel and air flows control data acquisition.

C. RAMAN Spectrophotometer, FEI Quanta 400 electronic microscop with scanner, Set Logger Temperature, carbon paper, Nafion Membrane, Si plates, TEFLON solution, W, Mo, Ni, etc. were purchased for obtaining and verifying the experimental electrocatalysts. D. The first stack with four modules each having a double fuel cell around one smooth anode and a mixture of Me1xSy as anodic catalyst was designed and realized, accordingly with the patented embodiment. E. In the view of proceeding to the in-situ experiments, an autonomous submersible installation was designed and manufactured for testing of H2S fuel cell stacks. It is able of data acquisition in various working regimes, data storage on several thousands measuring cycles and marine water samples deduction for further chemical analysis and accompanying data acquisition. It is endowed with a complete automation using OMRON Data Acquisition System with facilities for programming the acquisition cycles and a flexible hosting zone for various stacks that are to be tested. Opportunities for consortia building-up in the view of FP7 joining 1. CD&T activities conducted in the project framework proved the viability of a new class of fuel cells working with hydrogen sulphide as an alternative clean power source.

2. The conducted research pointed that waste consuming through electrochemical oxidising is a valid way to eliminate waste simultaneously with power generating. Thus, cleaning costs may be lowered. 3. New study theme in the FC area has been opened having a positive impact on environment. Low concentrated fuels in various liquids may be electrochemically oxidised, leading to different target media cleaning, such as sour gases and sulphide waters. 4. New methods are the object of patent applications in a European research thematic area nano sciences, nano technologies, new materials and new production processes . 5. Through oriented research, the project opens a way towards immediate technologic applications co generative power supplies for buildings or residential districts, hybrid

applications such as solar/ wind and fuel cells, etc. 6. Theoretical and experimental researchers from Romania had the opportunity of specialising in the view of becoming partners to the future European Community Enterprise for Hydrogen and Fuel Cells, whose regulation is to be approved in the European Parliament. 7. The existing consortium wishes to begin a collaboration with The Black Sea Institute from Turkey, aiming the extension of research and experimental achievements. Conclusions The reached solution might be enlarged, generating a new vision upon different types of waste electrochemical oxidation, in a zone of compromise between power efficiency and cleaning efficiency of the target medium. Finally, the procedure is an alternative to the waste burning in the air, for a large class of those that fit the described procedure, and leads to waste processing costs deductions from the generated power.

Me Mo, Ni, W, etc.

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