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Oxide from Depleted Lead-Acid Batteries for Potential Reuse in Next Generation Electrochemical Systems

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Oxide from Depleted Lead-Acid Batteries for Potential Reuse in Next Generation Electrochemical Systems Hydrometallurgically Generated Nanostructured Lead(II) Oxide from Depleted Lead-Acid Batteries for Potential Reuse in Next Generation Electrochemical Systems Robert Chi Yung Liu Fitzwilliam College University of Cambridge A dissertation submitted for the degree of Doctor of Philosophy September 2016 Preface This dissertation is the result of my own work and includes nothing which is the outcome of work done in collaboration except as declared in the Preface and specified in the text. It is not substantially the same as any that I have submitted, or, is being concurrently submitted for a degree or diploma or other qualification at the University of Cambridge or any other University or similar institution except as declared in the Preface and specified in the text. I further state that no substantial part of my dissertation has already been submitted, or, is being concurrently submitted for any such degree, diploma or other qualification at the University of Cambridge or any other University of similar institution except as declared in the Preface and specified in the text. This dissertation does not exceed 60,000 words in length. i Acknowledgements I would like to thank Dr Vasant Kumar for his supervision and invaluable feedback and support during this project. To the past and present members of the Materials Chemistry Group, University of Cambridge, thank you for all your help and support. In particular, I would like to thank Dr Carsten Schwandt, Dr Daniel Jewell and Marcel Yiao for being excellent sources of electrochemical and chemistry knowledge. I am grateful to all the staff at the Department of Materials Science and Metallurgy for their invaluable help and advice over the years, especially Simon Griggs and Zlatko Saracevic for their help with SEM and BET respectively. I am also thankful to Mary Vickers and Andrew Moss for their invaluable assistance with XRD over the years. I would also like to express my gratitude to Rosie Ward for her help and advice over the years. I am indebted to and grateful to my mother, to whom I dedicate this thesis, for always supporting me and giving me the encouragement to move forward. I have been blessed to have had so many wonderful people to count on as friends for keeping my spirits up over the course of this journey. Thank you all for being the support, inspiration, distraction and counsel I needed: Wil, Steve, Kent, Adam, Fabrizia, Oksana, Julia, Leszek, Julian, Ellen, Clara, Alex, Juvereya, Xanthe, Nenad, Sylwia, Jaap, Carl, Varun, Amir, Mike, Alan, Omba, Emily, Bruno, Silvia, Alja, Jess, Maggi, Nick, Sean, Niamh, Ola, Seb, Paul, Iris, Jamie, Asaf, Mu, Anup, Elliott, Guy, Zane, Dafina, Morven, Christian, Kim, George and countless others for empathising and encouraging me when I needed it. A special thanks to my housemates Katarzyna and Matheus for their boundless enthusiasm and encouragement. I am very grateful to Dr Paul Coxon for his patience and support in reading and correcting this dissertation. I would also like to thank my girlfriend Harriet for her support and encouragement. “Live as if you were to die tomorrow. Learn as if you were to live forever” - Mahatma Gandhi ii Abstract The recycling of lead-acid batteries (LABs) is currently an energy intensive, inefficient and polluting procedure. An alternative hydrometallurgical recycling process is investigated in this study. PbO, PbO2, and PbSO4 were individually reacted with a mixture of aqueous citric acid and sodium hydroxide solution, with hydrogen peroxide being used as a reducing agent for PbO2. Pure lead citrate of either Pb(C6H6O7)·H2O or Pb3(C6H5O7)2·3H2O was the product crystallized in each leaching experiment depending on the initial conditions. Combined spent electroactive paste materials from industry were leached and processed. 2.5 M H2O2, 3.2 M C6H8O7·H2O and 3.5 M NaOH were used for optimal leaching and were successful in synthesising Pb3(C6H5O7)2·3H2O after less than one hour. These amounts could be reduced by individual leaching of plate materials. The combustion-calcination of Pb3(C6H5O7)2·3H2O was successful in generating PbO containing both forms of the polymorph α and β crystal phases together with metallic Pb. A novel method to generate PbO from lead citrate was found through a self-sustaining combustion route where leached waste materials were preheated to 270 °C for ~15 minutes and were found to self-sustain a smouldering reaction to produce PbO with a predominately β phase containing metallic Pb. Electrochemical analysis of PbO from Pb3(C6H5O7)2·3H2O demonstrated the viability in the by-product to be used in an electroactive paste and therefore reused in new LABs. Pure α-PbO was generated from both forms of lead citrate, Pb(C6H6O7)·H2O and Pb3(C6H5O7)2·3H2O using NaOH. Pure β-PbO was also generated from Pb(C6H6O7)·H2O and Pb3(C6H5O7)2·3H2O using NaOH through dissolution/re-precipitation reactions. PbCO3 was successfully generated from Pb(C6H6O7)·H2O and Pb3(C6H5O7)2·3H2O using NaOH, NaHCO3 and an acid in a series of disassociation and re-precipitation reactions. PbCO3 could be used to thermally generate α and β-PbO as well as Pb3O4 by calcination at 350, 600 and 450 °C respectively. Glycerol was entrained in both PbCO3 and α-PbO as an in-situ reducing agent to generate PbO containing metallic Pb. Acid reactivity and absorption characteristics of PbO derived from Pb3(C6H5O7)2·3H2O heated in CO2 were equal to and greater than those used in industry for both automotive and industrial batteries. iii Contents Preface ....................................................................................................................... i Acknowledgements .................................................................................................. ii Abstract .................................................................................................................... iii 1 Introduction ........................................................................................................ 1 2 Background and Principles of Operation ........................................................ 3 2.1 Electrode Processes ............................................................................................... 3 2.2 Manufacture of PbO for Lead-Acid Batteries ........................................................... 7 2.2.1 The Barton Pot Method ................................................................................................... 7 2.2.2 The Ball Mill Method ........................................................................................................ 8 2.3 Lead Oxides.......................................................................................................... 10 2.3.1 Lead(II) Oxide, PbO ...................................................................................................... 10 2.3.2 Lead (II, IV) Oxide, Pb3O4 ............................................................................................. 11 2.3.3 Lead(IV) Oxide, PbO2 .................................................................................................... 12 2.3.4 Summary ....................................................................................................................... 12 2.4 Cell Components .................................................................................................. 13 2.4.1 The Cathode .................................................................................................................. 13 2.4.2 The Anode ..................................................................................................................... 13 2.4.3 The Electrolyte .............................................................................................................. 14 2.4.4 The Separators .............................................................................................................. 15 2.5 Types of Lead-acid Batteries ................................................................................ 16 2.5.1 Flooded Batteries .......................................................................................................... 16 2.5.2 Sealed Valve-Regulated Lead–Acid (VRLA) Batteries ................................................. 16 2.5.3 SLI Batteries (Starting, Lighting and Ignition) ............................................................... 18 2.5.4 Deep Cycle Batteries .................................................................................................... 19 2.6 Overview of Lead-Acid Batteries ........................................................................... 20 2.7 Options for Improving the Lead-Acid Battery ......................................................... 24 2.7.1 The Expander ................................................................................................................ 24 2.7.2 The Electrodes .............................................................................................................. 26 2.7.3 Cell Design .................................................................................................................... 29 2.7.4 The Active Mass ............................................................................................................ 30 2.8 Lead-Acid Battery Recovery and Recycling .......................................................... 32 2.9 Summary .............................................................................................................. 37 iv 3 Experimental Procedures ..............................................................................
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