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Photocatalytic Reduction of Selenate and Selenite: Water/Wastewater Treatment and the Formation of Nano-Selenium Compounds

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Photocatalytic Reduction of Selenate and Selenite: Water/Wastewater Treatment and the Formation of Nano-Selenium Compounds Photocatalytic Reduction of Selenate and Selenite: Water/Wastewater Treatment and The Formation of Nano-Selenium Compounds by Thatt Yang Timothy TAN, B.E. (Hons Class 1) A thesis submitted in fulfilment of the requirements for the degree of Doctor of Philosophy The School of Chemical Engineering and Industrial Chemistry The University of New South Wales Sydney Australia July 2003 A CERTIFICATE OF ORIGINALITY I hereby declare that this submission is my own work and to the best of my knowledge it contains no materials previously published or written by another person, nor material which to a substantial extent has been accepted for the award of any other degree or diploma at UNSW or any other educational institution, except where due acknowledgment is made in the thesis. Any contribution made to the research by others, with whom I have worked at UNSW or elsewhere, is explicitly acknowledged in the thesis. I also declare that the intellectual content of this thesis is the product of my own work, except to the extent that assistance from others in the project’s design and conception or in style, presentation and linguistic expression is acknowledged. ……………………………………………………….. B This thesis is especially dedicated to my parents, Boon Chew Tan & Ah Sioh Lee, And my sister, Foong Yee Tan. C Abstract The current work investigates the photocatalytic reduction of selenium (Se) ions, selenate Se(VI) and selenite Se(IV), from two perspectives: Se ion removal from water and wastewater and the formation of nano-Se compounds. Se ion pollution has become an environmental issue in recent years, and hence there is an urgent need for an efficient removal technique. In addition, there is increasing interest in the formation of nano-size semiconductors for niche applications. Since Se is a semiconductor, its formation onto the semiconductor TiO2 could lead to the discovery of new composite materials. The current study has successfully elucidated the mechanism of Se ions reduction by photocatalysis. Factors such as the simultaneous adsorption of the Se ions (the electron scavenger in this case) and a suitable organic compound (the hole scavenger), and the chemical properties of the hole scavenger were crucial for effective and efficient Se ions photoreduction. Optimum conditions in relation to pH, concentrations and types of hole scavenger were reported and discussed. It was also found that stoichiometric adsorption ratio of formate and selenate resulted to optimum photoreduction rate. A modified Langmuir-Hinshelwood kinetic model that considered the simultaneous adsorption of both solutes was derived. The current investigation has also seen the successful formation Se deposits of different morphologies onto the TiO2 particles. Discrete Se particles of various sizes in the nano-size range as well as a Se film were deposited onto the TiO2 particles under different initial experimental conditions. The Se-TiO2 composite semiconductor was explored for the 2+ removal of cadmium Cd ions, which resulted in the formation of CdSe-TiO2 systems. The photoreduction of Se ions using silver-modified TiO2 showed the enhanced reduction of Se 2- ions to Se in the form of H2Se gas. It is suggested that the H2Se gas generated from the current photoreduction process could be used as a safer and cheaper technique in the formation of Se-compounds such copper selenide, cadmium selenide and zinc selenide. All these compounds were widely used in optical and semiconducting devices. D Acknowledgements I would like to extend my most sincere acknowledgement and gratitude to a number of people and organisations. Without them, the quest towards my Ph.D. degree would be less rewarding, interesting and challenging. My greatest appreciation goes to my university supervisors, A/Prof Rose Amal and Dr Donia Beydoun, for their omnipresence in providing help, support, encouragement, guidance and never being tired of reading my works. I am particularly grateful to them for imparting their valuable knowledge and time. I would also like to thank Dr Myint Zaw for his help and guidance when I was conducting experiments in the Australian Nuclear Science and Technology Organisations (ANSTO). I would also like to thank Prof Paul Munroe and Miss Katie Levick from the Electron Microscopy unit in the University of New South Wales (UNSW) for their interpretation and assistance with electron microscopy analysis. Special thanks to Dr Kath Smith and Dr David Mitchell for their assistance in electron microscopy analysis in ANSTO. I also thank Dr Grainne Moran for her assistance in Uv-Vis spectroscopy analysis and Inna Bolkovsky for her help in XRD analysis, and of course not forgetting Mr John Starling for his ever- timely ordering of materials. The awarding of the Australian Institute of Nuclear Science and Engineering (AINSE) Postgraduate Scholarship, the International Postgraduate Research Scholarship from The University of New South Wales (UNSW) and the Department of Education, Training and Youth Affairs (DETYA), the Supplementary Engineering Award from the Faculty of Engineering, and the scholarship from the Centre of Particle and Catalysts Technologies are all gratefully acknowledged. My sincere thanks also extend to everyone in the Centre of Particle and Catalyst Technologies; for their continual support, friendship and ceaseless humour in making a drilling day more tolerable, and especially for their generosity in lending laboratory apparatus during crucial moments. Most importantly, I would like to thank my parents, sister and all my family and friends in Sydney for their love and support. Last but not least, the continued support, love and care from Chun Poe Yuen and Pui Yik Chan are greatly appreciated. E Lists of Publications Journal Publications 1. Timothy T. Y. Tan, Donia Beydoun, Rose Amal. “Photocatalytic Reduction of Se(VI) in Aqueous Solutions in UV/TiO2 System : Importance of Stoichiometric Ratio of Reactants on TiO2 Surface”. Journal of Molecular Catalysis A: Chemical, 2003 202(1-2 ) Page. 73-85. (Chapter 3A) 2. Timothy T. Y. Tan, Donia Beydoun, Rose Amal. “Effects of Organic Hole Scavengers on the Photocatalytic Reduction of Se ions”. Journal of Photochemistry and Photobiology A: Chemistry, 2003 159(3), Pages 273-280. (Chapter 3B) 3. Timothy T. Y. Tan, Donia Beydoun, Rose Amal. “Photocatalytic Reduction of Se(VI) in Aqueous Solutions in UV/TiO2 System: Kinetic Modeling and Reaction Mechanism”. Journal of Physical Chemistry B, 2003 107(18) Pages 4296-4303. (Chapter 3C) 4. Timothy T. Y. Tan, Myint Zaw, Donia Beydoun, Rose Amal. “The Formation of Nano-Sized Selenium-Titanium Dioxide Composite Semiconductors by Photocatalysis”. Journal of Nanoparticle Research, 2002 4(6), Pages 541-552. (Chapter 4A) 5. Timothy T. Y. Tan, Chee Kin Yip, Donia Beydoun, Rose Amal. “Effects of Nano- Ag Particles Loading on TiO2 Photocatalytic Reduction of Selenate Ions”. Corrected proof available online in The Chemical Engineering Journal: Environmental. (Chapter 4B) 6. Timothy T. Y. Tan, Pierre Pichat, Donia Beydoun, Rose Amal. “A Study on the Photoconductance and Oxygen Isotopic Exchange of Se-loaded TiO2 Particles and their Photocatalytic Efficiency in Gas-Phase Methanol Photooxidation”. In preparation. Refereed Conference Proceedings 1. Timothy T. Y. Tan, Myint Zaw, Donia Beydoun, Rose Amal. “The Formation of Nano-sized Selenium-Titanium Dioxide Composite Semiconductors by Photocatalysis” in the World Congress of Particle Technology 4 (21 – 25 July, 2002), Sydney, Australia. 2. Timothy T. Y. Tan, Chee Kin Yip, Myint Zaw, Donia Beydoun, Rose Amal. “Effects of Nano-Ag Particles Loading on TiO2 Photocatalytic Reduction of Selenate Ions” in the 9th APCChE Congress and CHEMECA 2002, 29 September – 3 October 2002, Christchurch, New Zealand. Other Conference Proceedings 1. Timothy T.Y. Tan, Jason Scott, Myint Zaw, Donia Beydoun, Rose Amal. “Photocatalytic Reducitons of Se(IV) in Aqueous Solutions” in the The Fifth F International Conference on TiO2 Photocatalytic Purification and Treatment of Water and Air, 2000, Ontario, Canada. 2. Timothy T. Y. Tan, Myint Zaw, Donia Beydoun, Rose Amal. “The Formation of Nano-sized Selenium-Titanium Dioxide Composite Semiconductors by Photocatalysis” in the 1st International Student Congress of Particle Technology (19 – 21 July, 2002), Terrigal, Australia. 3. Timothy T. Y. Tan, Donia Beydoun, Myint Zaw, Rose Amal. “Deposition of Se Nano-particles onto TiO2 Photocatalyst using Se(IV) and Se(VI) as Se precursors” in the 14th International Conference On Photochemical Conversion And Storage Of Solar Energy (IPS-14) Hokkaido University, Sapporo, Japan August 4-9, 2002. 4. Timothy T. Y. Tan, Myint Zaw, Donia Beydoun, Rose Amal. “The Synthesis Of Nano Se-Tio2 P-N Composite Semiconductors By Photocatalysis” in the The Seventh International Conference on TiO2 Photocatalysis, November 17-21, 2002, Ontario, Canada. 5. Timothy T. Y. Tan, Myint Zaw, Donia Beydoun, Rose Amal. “Application Of The Photocatalytic Reduction of Se(VI) And Se(IV) by Ag-Modified And Unmodified TiO2 In The Synthesis of Nano Metallic Selenide Semiconductors” in the The Seventh International Conference on TiO2 Photocatalysis, November 17-21, 2002, Ontario, Canada. 6. Timothy T. Y. Tan, Donia Beydoun, Rose Amal. “The Synthesis of Se-TiO2 p-n Composite Semiconductor by Photocatalysis and its Implicationas” in the 7th International Conference on Solar Energy and Applied Photochemistry, 23-28 February, 2003, Luxor, Egypt. 7. Timothy T. Y. Tan, Donia Beydoun, Rose Amal. “Effects of Organic Hole Scavengers on the
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