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Department of Chemical and Environmental Department of Chemical and Environmental Engineering Treatment of Produced Water by Simultaneous Removal of Heavy Metals and Dissolved Polycyclic Aromatic Hydrocarbons in a Photoelectrochemical Cell By Ebenezer Temitope Igunnu BSc (Hons), MSc, MRSC Thesis submitted to the University of Nottingham for the degree of Doctor of Philosophy January 2014 Abstract Early produced water treatment technologies were developed before carbon dioxide emissions and hazardous waste discharge were recognised as operational priority. These technologies are deficient in the removal of dissolved hydrocarbons and dissolved heavy metal ions which have been identified as major contributors to the high environmental impact factor of produced water. The simultaneous removal of heavy metals and polycyclic aromatic hydrocarbon (PAH) from produced water via photoelectrochemical process was identified in this work as a produced water treatment alternative with the potential to virtually eliminate the cost for chemical reagents and high energy input. Several grades of simulated produced water were synthesised and used to understand different parameters necessary for developing a successful photoelectrochemical treatment. The process demonstrated in this work followed a simple two–electrode photoelectrochemical cell where heavy metals were recovered on a platinum electrode with simultaneous degradation of PAH (phenanthrene) on a photoanode, with the aid of sunlight (simulated) and an applied cell voltage of 1.0 V. Multiwall CNT-TiO2 synthesised via a modified sol-gel method served as the photoanode after it was immobilised at a loading of 2.5 mg/cm2 on a titanium plate. The results obtained from the photoelectrochemical treatment showed a recovery of 1.6 g/cm2 of lead, 0.2 g/cm2 of copper and 0.1 g/cm2 of nickel from produced water on a 0.1 cm diameter platinum electrode after 24 hours of irradiation with simulated sunlight at 1.0 V cell voltage and a simultaneous degradation of up to 16 % phenanthrene on the photoanode, which gives a potential of scaling up the process to a commercial throughput. ii List of Publications Peer-Reviewed Publication G. Kim, E.T Igunnu and G.Z. Chen (2014). "A sunlight assisted dual purpose photoelectrochemical cell for low voltage removal of heavy metals and organic pollutants in wastewater." Chemical Engineering Journal 244(0): 411-421. E. T. Igunnu, and G. Z. Chen (2012). "Produced water treatment technologies." International Journal of Low-Carbon Technologies 1(0): 1 -21. Conference Presentations E.T. Igunnu, G. Kim and G.Z. Chen (2013). “Case studies of a dual purpose photoelectrochemical cell for heavy metal recovery and decomposition of organic pollutants.” Midlands Electrochemistry Group meeting, University of Nottingham, April 17, 2013. E.T. Igunnu, Z. Li and G.Z. Chen (2013). “Removal of dissolved hydrocarbons from produced water by photo-electro-catalysis o n a CNT-TiO2 hybrid anode.” Young Environmental Scientist conference, Krakow, Poland, Feb.11-13, 2013. E.T. Igunnu and G.Z. Chen (2012). “Photoelectrochemical Treatment of produced water.” Midlands Electrochemistry Group meeting, University of Birmingham, June 27, 2012. E.T. Igunnu and G.Z. Chen (2011). “Electrochemical probe of Pb deposition from produced water.” Midlands Electrochemistry Group meeting, University of Warwick, May 5, 2011. E.T. Igunnu and G.Z. Chen (2010). “ Electrochemical mining of oilfield produced water for valuable metals.” Midlands Electrochemistry Group meeting,University of Leicester April 19, 2010. iii Acknowledgements I would like to thank the Almighty God for the grace He has given me to complete this research. I would also like to specially thank my supervisor, Professor George Z. Chen and my internal assessor Professor Peter Licence for their support and guidance throughout this PhD. I would also like to gratefully acknowledge the University of Nottingham’s Dean of Engineering Research Scholarship for funding this work; the Society of Environmental Toxicology and Chemistry Travel Fund, the Midlands Electrochemical Group and the University of Nottingham’s Electrochemical Technologies Group (ETG) for making it possible for this research to be disseminated in various conferences and seminars. I would like to thank my fellow PhD students and postdoctoral research fellows in the ETG in particular Gwangjun Kim, Dr. Mathew Li and Dr. Hu Di for their friendship, help and support. I would like to express my gratitude to David Clift for his help in performing SEM, EDX and XRD analyses and sharing his expertise. Acknowledgement of technical support should continue by thanking Dr. Nigel whose guidance and help in performing TEM analysis has been invaluable, and the rest of the technical staff at the Department of Chemical and Environmental Engineering. Support from Sarah Ulikhifun, Olaosebikan Folorunso and Peter Faraibi is also gratefully acknowledged. I would like to specially thank Anike Akinrinlade for her love, support, encouragement and taking her time to proof read this thesis. Finally I would like to thank my parents, Mr & Mrs D.D. Igunnu, and my siblings, Dayo, Sola, Funmi and Bolu, for their constant support and help, not just during the course of this PhD but also throughout my academic life. I would have not got here without them. Big thanks to the Beeston free church family and the Graduate Christian Fellowship. iv Table of Contents ABSTRACT .................................................................................................................................. II LIST OF PUBLICATIONS .............................................................................................................. III ACKNOWLEDGEMENTS.............................................................................................................. IV LIST OF ABBREVIATIONS............................................................................................................. X 1.1. PRODUCED WATER: DEFINITION AND KEY PROJECT AIM ................................................................ 13 1.2. NATURE AND PRODUCTION OF PRODUCED WATER ...................................................................... 15 1.3. BRIEF OVERVIEW OF PRODUCED WATER MANAGEMENT ............................................................... 16 1.3.1. Minimization ........................................................................................................... 17 1.3.2. Recycle/Re-use ........................................................................................................ 18 1.3.3. Disposal ................................................................................................................... 19 1.4. ENVIRONMENTAL IMPACT OF PRODUCED WATER DISPOSAL........................................................... 20 1.5. RESEARCH AIM, THESIS OUTLINE AND SUMMARY ........................................................................ 21 2.1. INTRODUCTION.................................................................................................................... 25 2.2. ORIGIN AND COMPOSITION OF PRODUCED WATER ...................................................................... 25 2.2.1. Oil content............................................................................................................... 27 2.2.2. Dissolved minerals................................................................................................... 28 2.2.3. Production chemicals .............................................................................................. 32 2.2.4. Produced solids ....................................................................................................... 33 2.2.5. Dissolved Gases....................................................................................................... 33 2.2.6. Heavy metals in Produced Water............................................................................ 33 2.2.7. Polycyclic Aromatic Hydrocarbons in produced water............................................ 35 2.3. PRODUCED WATER LEGISLATION ............................................................................................. 38 2.4. PRODUCED WATER TREATMENT TECHNOLOGIES ......................................................................... 39 2.4.1. Membrane Filtration Technology............................................................................ 40 2.4.1.1. Microfiltration/Ultrafiltration............................................................................................41 v 2.4.1.2. Polymeric/Ceramic Membranes........................................................................................41 2.4.1.3. Reverse Osmosis (RO) and Nanofiltration (NF)..................................................................41 2.4.2. Thermal Technologies ............................................................................................. 43 2.4.2.1. Multi Stage Flash ...............................................................................................................44 2.4.2.2. Multi Effect Distillation (MED)...........................................................................................44 2.4.2.3. Vapour Compression Distillation (VCD).............................................................................45 2.4.2.4. Multi Effect Distillation – Vapour compression Hybrid .....................................................46 2.4.3. Biological Aerated Filters .......................................................................................
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