PRODUCTION and CHARACTERIZATION of POLYSTYRENE RESINS CONTAINING FINE ACTIVATED CARBON PARTICLES by NURI HMIDI Thesis Submitted
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PRODUCTION AND CHARACTERIZATION OF POLYSTYRENE RESINS CONTAINING FINE ACTIVATED CARBON PARTICLES by NURI HMIDI Thesis submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy (PhD) in Natural Resources Engineering Faculty of Graduate Studies Laurentian University Sudbury, Ontario © Nuri Hmidi, 2017 THESIS DEFENCE COMMITTEE/COMITÉ DE SOUTENANCE DE THÈSE Laurentian Université/Université Laurentienne Faculty of Graduate Studies/Faculté des études supérieures Title of Thesis Titre de la thèse Production and Characterization of Polystyrene Resins Containing Fine Activated Carbon Particles Name of Candidate Nom du candidat Hmidi, Nuri Degree Diplôme Doctor of Philosophy Department/Program Date of Defence Département/Programme Natural Resources Engineering Date de la soutenance November 20, 2017 APPROVED/APPROUVÉ Thesis Examiners/Examinateurs de thèse: Dr. Eduard Guerra (Co-Supervisor/Co-directeur de thèse) Dr. Pedram Fatehi (Co-supervisor/Co-directeur de thèse) Dr. Turgut Yalcin (Committee member/Membre du comité) Dr. Ramesh Subramanian (Committee member/Membre du comité) Approved for the Faculty of Graduate Studies Approuvé pour la Faculté des études supérieures Dr. David Lesbarrères Monsieur David Lesbarrères Dr. James Vaughn Dean, Faculty of Graduate Studies (External Examiner/Examinateur externe) Doyen, Faculté des études supérieures Dr. Louis Mercier (Internal Examiner/Examinateur interne) ACCESSIBILITY CLAUSE AND PERMISSION TO USE I, Nuri Hmidi, hereby grant to Laurentian University and/or its agents the non-exclusive license to archive and make accessible my thesis, dissertation, or project report in whole or in part in all forms of media, now or for the duration of my copyright ownership. I retain all other ownership rights to the copyright of the thesis, dissertation or project report. I also reserve the right to use in future works (such as articles or books) all or part of this thesis, dissertation, or project report. I further agree that permission for copying of this thesis in any manner, in whole or in part, for scholarly purposes may be granted by the professor or professors who supervised my thesis work or, in their absence, by the Head of the Department in which my thesis work was done. It is understood that any copying or publication or use of this thesis or parts thereof for Financial gain shall not be allowed without my written permission. It is also understood that this copy is being made available in this form by the authority of the copyright owner solely for the purpose of private study and research and may not be copied or reproduced except as permitted by the copyright laws without written authority from the copyright owner. ii ABSTRACT The development of high capacity adsorbent using engineered activated carbon fines technology, and their ability to extract gold from solution is presented. The unique feature of these adsorbents is their ability to adsorb gold ions from low concentration solutions like mine effluent as well as from leached solutions in gold mills. Production of polystyrene ion exchange resins containing fine activated carbon particles denoted, PSAC, (Polystyrene Activated Carbon) and their gold stripping kinetics were studied. Polystyrene beads were prepared by simple suspension polymerization. However, addition of fine activated carbon (AC) during suspension polymerization was not successful in producing small beads, but rather a conglomerated mass, which was then broken up and shaped into smaller beads. PSAC beads were also produced by co-extrusion of polystyrene with activated carbon and by physical adsorption of activated carbon onto raw polystyrene beads in an autoclave at a temperature above the glass transition temperature of polystyrene. Stripping tests were performed which identified the latter bead type as being the most promising form of PSAC bead for future research. The work was aimed at optimizing the production of the beads in terms of their physical and chemical properties. This work led to the development of a new polystyrene/activated carbon ion exchange bead as an alternative to pure activated carbon. A mini-elution column was also designed to carry out the test work to study the performance of beads and loaded fine carbon stripping parameters under typical industrial conditions. Further development of this research may lead to a new method of stripping loaded fine carbon on mine sites as part of the existing gold milling and extracting circuits. iii KEYWORDS Activated carbon, polystyrene, ion exchange resins, gold loaded fine activated carbon PSAC, (Polystyrene Activated Carbon) beads, autoclave, stripping, gold recovery, elution, adsorption, desorption, cyanide adsorption/stripping, porosity, surface area, size distribution, leaching, in carbon-in-pulp (CIP), carbon-in-leach (CIL) processes, gold losses, Morphology, resin in pulp (RIP) iv ACKNOWLEDGMENTS Firstly, I’d like to credit my faith in God for giving me strength at all times and especially during the work period on this project. I would like to thank my supervisor Dr. Eduard Guerra; without his support and technical assistance this project would never have been completed. I’d like to also acknowledge Dr. Pedram Fatehi, who provided much of the technical support for this project. On a more personal level, I would like have a special thanks to my wife, Waded Omar Ibrahem, for your endless support and encouragement. Thank you so much for standing with me. My special thanks to mother, Amna Essa Amara, for her support. Your support meant so much to me. I’d also like to thank my children: Mohamed, Wadid, Rana and Rawasy and my sisters, especially Beninah and Ali El-Hmidi, my cousin, and my brothers, particularly Alttahir, for their support. Also, I would like to thank my wife‘s family, all my friends and each member of the El Hamidis families for their support and encouragement. Finally, I’d like to thank Dr. Turgut Yalcin, and Dr. Zhibin Ye at Laurentian University, and Dr. Guosheng Wu at Lakehead's central analytical laboratory for their help with the SEM and EDX analyses, Michael Sorokopud at Lakehead for the XPS analyses, Doug Town and his team at Musselwhite, at Goldcorp mine for the gold analyses. I’d like to also acknowledge Dr. Adil Aledresse, Mohammad Usman, Chris Taylor and Meliisa Martikkala at Goldcorp, Musselwhite Gold Mine, for their technical help in setting up the experiments and monitoring the system. Also, I would like to thank Kris Tietz at Red Lake gold mines for his technical assistance in experiments carried out at Goldcorp, Red Lake gold mines. I finally thank the Goldcorp organization for their endless support. I thank again my family for their belief in me and I thank all of those who have assisted, encouraged and inspired me to successfully complete this thesis. v ABSTRACT ................................................................................................................ III KEYWORDS .............................................................................................................. IV ACKNOWLEDGMENTS ........................................................................................... V LIST OF FIGURES ..................................................................................................... IX LIST OF TABLES ....................................................................................................... XI 1 INTRODUCTION ................................................................................................. 1 2 LITERATURE REVIEW ...................................................................................... 4 2.1 CIP AND CIL GOLD MILLING .......................................................................... 4 2.1.1 CHEMISTRY OF GOLD CYANIDATION ................................................. 7 2.1.2 ADSORPTION OF THE GOLD CYANIDE COMPLEX ONTO ACTIVATED CARBON ............................................................................................... 8 2.1.3 GOLD CYANIDE ELUTION FROM ACTIVATED CARBON ............... 10 2.1.4 ACID WASHING OF ACTIVATED CARBON ........................................ 12 2.1.5 GOLD LOSSES DUE TO ATTRITION OF ACTIVATED CARBON ..... 13 2.2 POLYSTYRENE BASED ION-EXCHANGE RESINS ..................................... 14 2.2.1 SUSPENSION POLYMERIZATION OF POLYSTYRENE BEADS ....... 17 2.2.2 POLYSTYRENE/ACTIVATED CARBON MATERIALS........................ 17 2.2.3 FUNCTIONALIZATION OF POLYSTYRENE BEADS FOR ION- EXCHANGE APPLICATIONS .................................................................................. 18 2.3 SUMMARY ......................................................................................................... 18 3 EXPERIMENTAL DETAILS ............................................................................. 19 3.1 EXPERIMENTAL METHODS FOR PRODUCTION OF PS-AC BEADS ...... 19 3.1.1 SUSPENSION POLYMERIZATION EXPERIMENTS ............................ 19 3.1.2 CO-EXTRUSION EXPERIMENTS ........................................................... 23 3.1.3 AUTOCLAVE EXPERIMENTS................................................................. 24 3.1.4 FACTORIAL EXPERIMENTS................................................................... 27 3.2 METHODS USED FOR PHYSICAL CHARACTERIZATION ........................ 28 3.2.1 BRUNAUER–EMMETT–TELLER (BET) ANALYSIS ............................ 28 3.2.2 THERMOGRAVIMETRIC ANALYSIS (TGA) ........................................ 29 3.2.3 X-RAY DIFFRACTION ............................................................................