SCHOOL OF MATERIALS AND MINERAL RESOURCES ENGINEERING UNIVERSITY SAINS MALAYSIA DEVELOPMENT OF MARCO-POROUS ECOTILES FROM FRESH WATER SLUDGE FOR CADMIUM REMOVAL By YEOH KAR KEAT Supervisor: ASSOC. PROF. DR. YEOH FEI YEE Dissertation submitted in partial fulfilment of the requirements For the degree of Bachelor of engineering with honours (MATERIALS ENGINEERING) UNIVERSITI SAINS MALAYSIA JUNE 2019 ACKNOWLEDGEMENT First of all, I would like to wish a thousand thanks to Universiti Sains Malaysia for giving me the opportunity the complete my degree of Bachelor of Materials Engineering. Great thanks to School of Materials and Mineral Resources Engineering to provide me adequate equipment and Laboratory to complete this research. Secondly, I would like to thank my supervisor, Assoc. Prof. Dr Yeoh Fei Yee for giving me proper advice and guidance throughout my research despite his busy schedule. This research would not be done successfully without his support and supervision. Besides that, I would also like to thank to all of the research team who have helped and contributed in this research, especially Ooi Chee Heong and Kelvin Heng which provide tones of helps throughout this experiment. Great thanks to the technical staff in School of Materials And Mineral Resources who have provided their service, help and advice along the progress of the experiment. Without their help, this research would not be successful. Last but not least, I would like to thank my friends and family who gives me full support either directky or indirectly in this research. With their support and encouragement, I was able to complete my degree successfully. Table of content ACKNOWLEDGEMENT .............................................................................................. i LIST OF TABLES ........................................................................................................ vi LIST OF FIGURES ..................................................................................................... vii LIST OF ABBREVIATIONS ....................................................................................... ix ABSTRACT ................................................................................................................... x ABSTRAK .................................................................................................................... xi Chapter 1 Introduction ................................................................................................... 1 1.1 Preface ............................................................................................................. 1 1.2 Introduction .......................................................................................................... 1 1.2 Problem statement ........................................................................................... 5 1.3 Research objective........................................................................................... 6 1.4 Scope of research ............................................................................................ 6 CHAPTER 2 LITERATURE REVIEW ........................................................................ 7 2.1 Sludge Problem ............................................................................................... 7 2.2 Coagulation of Sludge.......................................................................................... 8 2.3 Alternative Solution to Disposed Of Water Sludge ........................................... 11 2.4 Fabrication of Porous Ceramic Body ................................................................. 15 2.5 Heavy Metal Adsorption .................................................................................... 18 ii 2.6 Types of Cadmium Removal ............................................................................. 20 2.7 Porous medium for Cadmium Removal ............................................................ 21 2.8 Urea Functionalisation of Clay .......................................................................... 23 2.9 Heavy Metal Adsorption by Chelating Agent, Urea .......................................... 25 CHAPTER 3 MATERIALS AND METHODOLOGY .............................................. 27 3.1 Introduction ........................................................................................................ 27 3.2 Preparation of Raw Materials ............................................................................ 28 3.2.1 Drying ......................................................................................................... 28 3.2.2 Grinding ...................................................................................................... 29 3.2.3 Sieving ........................................................................................................ 30 3.3 Slip Casting ........................................................................................................ 31 3.3.1 Mixing ......................................................................................................... 31 3.3.2 Casting ........................................................................................................ 33 3.3.3 Firing ........................................................................................................... 33 3.3.4 Determination of the parameter .................................................................. 34 3.4 Physical Testing ................................................................................................. 34 3.4.1 Modulus of Rupture Test ............................................................................ 34 3.4.2 Preparation of Urea Solution ...................................................................... 35 3.4.3 Functionalisation of Ecoclay ....................................................................... 35 3.5 Scanning Electron Microscope (SEM) .............................................................. 36 3.6 X-ray Diffraction ............................................................................................... 36 iii 3.5 Determining the Urea Functionalisation ............................................................ 37 3.5.1 Fourier-transform infrared spectroscopy (FTIR) ........................................ 37 3.5.2 Urea Concentration Measurement .............................................................. 37 3.6 Heavy metal Adsorption .................................................................................... 38 3.6.1 Determining Time Taken for Adsorption ................................................... 38 3.6.2 Determining How Porosity Affect Heavy Metal Adsorption ..................... 39 3.6.3 Inductively coupled plasma - optical emission spectrometry (ICP-OES) .. 40 Chapter 4 Results and Discussion ................................................................................ 42 4.0 Introduction ........................................................................................................ 42 4.1 Ecoclay Tiles Characterisation .......................................................................... 42 4.1.1 Determination of the parameters ................................................................. 42 4.1.2 Modulus of Rupture (MOR) Test ............................................................... 46 4.1.2 FTIR result of Functionalised Ecoclay Tiles .............................................. 48 4.1.3 Urea Concentration Measurement .............................................................. 51 4.1.4 X-ray Diffraction Analysis ......................................................................... 53 4.1.5 Scanning Electron Microscope ................................................................... 61 4.2 Heavy Metal Adsorption Capability of Porous Ecoclay Tiles ........................... 66 4.2.1 Time Taken to Reach Maximum Adsorption Capacity .............................. 66 4.2.2 Effect of Amount of Pore-Forming Agent on the Cadmium Adsorption Capacity ............................................................................................................... 68 Chapter 5 Conclusion and Recommendation ............................................................... 72 5.1 Conclusion ......................................................................................................... 72 iv Future Recommendation .......................................................................................... 73 References .................................................................................................................... 74 v LIST OF TABLES Table 2. 1 Chemical composition and physical test of different samples from different plants of alum sludge by X-ray fluorescence (XRF) ..................................................... 8 Table 2. 2List of primary coagulant used for water treatment. .................................... 10 Table 3. 1 Composition of clay body sample with different amount of sludge. .......... 31 Table 3. 2Composition of clay boy with difference amount of rice husk .................... 32 Table 4. 1MOR value for Ecoclay ............................................................................... 46 Table 4. 2 Amount of urea functionalised on to the ecoclay sample ........................... 52 Table 4. 3 Position and relative intensity of XRD peak of sludge with respective d- spacing ........................................................................................................................