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1 vii TABLE OF CONTENTS CHAPTER TITLE PAGE DECLARATION DEDICATION ACKNOWLEDGEMENT ABSTRACT ABSTRAK TABLE OF CONTENTS LIST OF TABLES LIST OF FIGURES LIST OF SYMBOLS / ABBREVIATIONS LIST OF APPENDICES ii iii iv v vi vii xi xiii xvi xviii 1 INTRODUCTION 1.1 Problem Statement Objective of the Research Scope of Studies 4
2 viii 2 LITERATURE REVIEWS 2.1 Activated Carbon Physical Properties of Activated Carbon Agricultural By-product as Raw Material Preparation of Activated Carbon Selecting of Raw Materials Pre-treatment Carbonization Activation Activation with Zinc Chloride Washing Catalyst Support Activated Carbon as Catalyst Support Transition metal carbides Tungsten Carbide in Catalytic Usages Chlorofluorocarbons (CFCs) Remediation and Conversion of CFCs Hydrodehalogenation of CFCs on Tungsten Carbide Preparation of Tungsten Carbide Fourier Transform Infrared (FTIR) Nitrogen Adsorption Analysis Adsorption Isotherms Brunauer, Emmett and Teller (BET) Surface Area The t-plot Thermogravimetry Analysis (TGA) Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersive X-ray Spectroscopy (EDX) X-ray Powder Diffraction (XRD) Gas Chromatography (GC) 40
3 ix 3 EXPERIMENTAL 3.1 Instrumentations Chemicals Preparation of Activated Carbon Preparation of raw material Chemical activation Preparation of Tungsten Carbide Sample Characterization Characterization of Activated Carbon Characterization of Tungsten Carbide Catalytic testing-hydrodehalogenation of CFC RESULTS AND DISCUSSION 4.1 General Characterization of Activated Carbons Fourier Transform Infrared Spectroscopy Nitrogen Adsorption Analysis Single Point BET Surface Area BDDT Isotherms and Pore Size Distribution The t-plot FESEM analysis of Activated Carbons Energy Dispersive X-ray Analysis (EDX) Thermogravimetry Analysis Thermogravimetry Analysis of Raw palm Kernel Shell Thermogravimetry analysis of Activated Carbon in Air Flow Thermogravimetry Analysis of Activated Carbons in Nitrogen Flow Tungsten Carbide Catalyst X-ray Diffraction (XRD) XRD analysis of Tungsten Carbide Catalyst Supported on AC-1Z-N 82
4 x XRD analysis of Tungsten Carbide Catalyst Supported on AC-1Z-V Field Emission Scanning Electron Microscopy Single point BET Surface Area Hydrodehalogenation of CFC CONCLUSIONS 98 REFERENCES 100 APPENDICES 110
5 xi LIST OF TABLES TABLE NO. TITLE PAGE 2.1 Classification of pores of a porous material Agricultural by-products used to produce activated carbon Physical and chemical properties of supports Type of catalyst supports and their applications Notation for tungsten carbide catalyst produced Sample notation for activated carbons Vibration wavenumber and functional groups of the samples Surface area and pore volume of activated carbon EDX analysis of activated carbons Percentage of weight loss of AC-1Z-N and AC-1Z-V in air flow Percentage of weight loss of AC-1Z-N and AC-1Z-V in nitrogen flow Notation for the samples prepared Relative intensity of main peaks for AC-1Z-N
6 xii supported catalysts Relative intensity of main peaks for AC-1Z-V supported catalysts Single point BET surface area of samples 93
7 xiii LIST OF FIGURES FIGURE NO. TITLE PAGE 2.1 Structure of transition metal carbides The gas sorption process Types of BDDT physisorption isotherm X-ray scattered by atoms in an ordered lattice interfere constructively in direction given by Braggs Law Diagram of a gas chromatograph Flow diagram for the preparation of activated carbon Schematic diagram of vacuum line system Schematic set-up used for heat-treatment of tungsten carbide catalyst Schematic set-up for hydrodehalogenation catalytic reaction FTIR spectra for raw palm kernel shell, commercial activated carbon and samples activate in vacuum condition FTIR spectra for raw pal kernel shell, commercial activated carbon and samples activate in nitrogen flow Single point BET surface area of raw-pks, P-AC and prepared activated carbons. 58
8 xiv 4.4 BDDT isotherm of AC-1Z-N and AC-1Z-V Pore size distribution graph of AC-1Z-N Pore size distribution graph of AC-1Z-V BDDT isotherm of AC-2Z-N and AC-2Z-V Pore size distribution of AC-2Z-N Pore size distribution of AC-2Z-V Micrograph of raw-pks with magnification of 500x Micrograph of AC-1Z-Nwith magnification of 150x Micrograph of AC-1Z-N with magnification of 7500x Micrograph of AC-1Z-V with magnification of 150x Micrograph of AC-1Z-V with magnification of 500x Micrograph of AC-2Z-N with magnification of 250x Micrograph of AC-2Z-N with magnification of 350x TGA/DTG of raw-pks TGA/DTG of AC-1Z-N in air flow TGA/DTG of AC-1Z-V in air flow TGA/DTG of AC-1Z-N in nitrogen flow TGA/DTG of AC-1Z-V in nitrogen flow X-ray diffractogram of samples with 6 percent of tungsten content supported on AC-1Z-N X-ray diffractogram of samples with 15 percent of tungsten content supported on AC-1Z-N X-ray diffractogram of samples with 6 percent of tungsten content supported on AC-1Z-V X-ray diffractogram of samples with 15 percent of tungsten
9 xv content supported on AC-1Z-V Micrograph of ACN with magnification of 140x Micrograph of ACV with magnification of 800x EDX of ACN EDX of ACV Caption of CFC-12 gas without catalyst Caption of product mixture at different temperature in the presence of Catalyst Conversion of CFC-12 using ACN at different temperatures. 97
10 xvi LIST OF SYMBOLS / ABBREVIATIONS C - degree Celsius μm - micrometer BET - Brunauer-Emmett-Teller cm - centimeter DTA - Differential thermal analysis EDX - Energy Dispersive X-ray analysis Eq. - Equation FTIR - Fourier Transformation Infra red g - gram ID - internal diameter K - Kelvin ksi - kips per linear foot kv - kilo volt ma - mili ampere NA - nitrogen adsorption ml - milliliter nm - nanometer rpm - rotation per minute
11 xvii TG - Thermogravimetry XRD - X-ray Diffraction θ - Half angle of diffraction beam λ - wavelength
12 xviii LIST OF APPENDICES APPENDIX NO. TITLE PAGE 1.0 Calculation of weight used from atomic weight percentage ratio of tungsten and activated carbon support in tungsten carbide preparation Nitrogen Adsorption Data of AC-1Z-N Nitrogen Adsorption Data of AC-1Z-V Nitrogen Adsorption Data of AC-2Z-N Nitrogen Adsorption Data of AC-2Z-V t-plot Analysis of AC-1Z-N t-plot Analysis of AC-1Z-V t-plot Analysis of AC-2Z-N t-plot Analysis of AC-2Z-V EDX Spectrum of AC-1Z-N EDX Spectrum of AC-1Z-V EDX Spectrum of AC-2Z-N EDX Spectrum of ACN EDX Spectrum of ACN
13 xix 15.0 Calculation of conversion of CFC-12 using ACN at different temperatures List of paper presented /contributed 129
TABLE OF CONTENTS CHAPTER TITLE PAGE DECLARATION ACKNOWLEDGEMENT ABSTRACT LIST OF TABLES LIST OF FIGURES LIST OF SYMBOLS LIST OF APPENDICES
vii TABLE OF CONTENTS CHAPTER TITLE PAGE DECLARATION ii ACKNOWLEDGEMENT iv ABSTRACT v TABLE OF CONTENTS vii LIST OF TABLES xii LIST OF FIGURES xiv LIST OF SYMBOLS xvii LIST OF APPENDICES xviii 1 INTRODUCTION
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