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DISSERTATION O Attribution COPYRIGHT AND CITATION CONSIDERATIONS FOR THIS THESIS/ DISSERTATION o Attribution — You must give appropriate credit, provide a link to the license, and indicate if changes were made. You may do so in any reasonable manner, but not in any way that suggests the licensor endorses you or your use. o NonCommercial — You may not use the material for commercial purposes. o ShareAlike — If you remix, transform, or build upon the material, you must distribute your contributions under the same license as the original. How to cite this thesis Surname, Initial(s). (2012). Title of the thesis or dissertation (Doctoral Thesis / Master’s Dissertation). Johannesburg: University of Johannesburg. Available from: http://hdl.handle.net/102000/0002 (Accessed: 22 August 2017). Char extracted from coal ash as a replacement for natural graphite – “Charphite” By Charlotte Badenhorst Thesis Submitted in fulfilment of the requirements for the degree of PHILOSOPHIAE DOCTOR In Geology in the Faculty of Science at the University of Johannesburg, South Africa Supervisor: Prof. N.J. Wagner Co-supervisor: Prof. B.R.V. Valentim Co-supervisor: Prof. K.S. Viljoen November 2019 Acknowledgements This work is based on research supported by the National Research Foundation (NRF) of South Africa (Grant number 103466) and the Department of Science and Technology (DST)-NRF ERA-MIN grant for the Charphite project. The author also acknowledges DST-NRF Centre of Excellence for Integrated Mineral and Energy Resource Analysis (CIMERA) for additional financial assistance. K.S. Viljoen acknowledges financial support from the South African Department of Science and Technology through their Research Chairs initiative (Geometallurgy), as administered by the National Research Foundation. Prof. Nikki Wagner for allowing me to add my own special touches to my work, for minding my commas and semicolons, and for the opportunity to be supervised by one of the greatest. Prof. Bruno Valentim for encouraging me when the news was bad and for your always insightful inputs (from deciding on a colour scheme for my posters to complex scientific discussions on my papers!). Prof. Fanus Viljoen for your calm and collective presence, for your patience with all my queries and uncertainties, and for sharing your immense knowledge on everything and anything. The third ERA-MIN collaboration partners for allowing a rookie to be part of such a brilliant, experienced, and cultural diverse team. It was an honour to be working with you. UJ’s Geology Department, CIMERA, and Spectrau Laboratory for welcoming a non-geologist into your midst. After three years with you, I feel as old and wise as the world itself! A special thanks to everybody who contributed in some way to my research. The Coal Research Group for our bi-weekly discussions on all things coal, for our highly entertaining World Coal magazine talks, for our “safe environment” dry run presentations, and for growing from coal students into coal experts. Eskom, Sasol, and Jonkel Carbons and Grafites for supplying me with much needed samples and for dealing with all the red tape, for supplying me with even more samples when I miscalculated the extend of my research (special thanks to Dr. Kelley Reynolds- Clausen), and for tolerantly answering my sometimes annoying questions. i | P a g e South African Coal Ash Association for the opportunity to network and share my ideas and for your financial contribution to our (very expensive!) trip to the 2019 World of Coal Ash Conference in the United States of America (USA). What an experience! Thank you. Mfesane Tshazi and Dr. Natasia Naudé from the University of Pretoria for usage of your CoronaStat electrostatic separator. Willem Swanepoel and Sean Harbinson from Bureau Veritas Testing and Inspections South Africa for allowing me to spend the day in your labs. Sabine Verryn from XRD Analytical & Consulting for our discussion on XRD structural characterisation. MAK Analytical for thousands of LOI trials. Betachem for kindly providing the reagents used in the froth flotation experiments. To my family and friends. My mom for raising us on coffee (it came in handy this time). My dad for knowing more about my projects than I do (after 28 years I still think my dad is the smartest person alive). My siblings (four sisters and a not-so-little-anymore brother) for my stories. Jaganmoy Jodder for sharing this small office space with me and for showing me what kindness really means. For all the great people I have met on this journey - You have made me realise how much I still have to learn. ii | P a g e Abstract This thesis forms part of the third ERA-MIN collaboration between Portugal, Poland, Romania, Argentina, and South Africa under the project Charphite. The overall aim of the Charphite project was to determine if char found in coal ash can be used as a substitute replacement for natural graphite in green energy applications, including direct use of char in the electrocatalytic oxygen reduction reaction and the hydrogen oxidation reaction. Ash is a waste product resulting from the combustion of coal. The landfilling or ponding of ash can lead to serious environmental and health concerns, and therefore the utilisation of ash / certain components in the ash is desired. Literature shows that South African coal ash samples (>50 mill ton ash per annum) contain 0.5 to 8 % carbon in ash (chars) and also a significant amount of unburned carbon is associated with carbonaceous shale containing <10 % carbon and >90 % mineral matter. Char in coal ash has a high degree of structural order and can possibly be used as a substitute for natural graphite. The European Union, the United States, and the United Kingdom have all listed natural graphite as one of their raw critical commodities; hence the project has significant merits. Research on producing synthetic graphite from char in coal ash is scarce, with only a limited amount of papers being published as yet. Due to the extensive nature of the ERA-MIN collaboration, only the results pertaining to the South African involvement are presented in this thesis (see https://www.fc.up.pt/charphite/ for overall results). The characterisation of South African coal ash sources, the separation of char from these sources, and the characterisation / evaluation of the extracted char as a possible precursor for synthetic graphite are presented. A desktop study on natural graphite occurrences in southern Africa, and characterisation of selected samples are also provided. A combination of size, electrostatic, and magnetic separation steps were used for char extraction. All carbon percentages were determined with the loss on ignition method. The final product grades ranged between 45 and 66 wt. % carbon. A density separation step was added to one of the fly ash samples and a final grade of 83 wt. % of carbon was achieved. Although a significant increase from the initial char in ash percentages was obtained, the carbon recoveries were unfortunately very low (6 to 32 %). Due to the low starting carbon in ash percentages, a significant amount has to be recovered to make economic sense. The reason for the low carbon recoveries might be due to small, unliberated ash minerals that formed part of the char matrix. The evaluation of the extracted chars (proximate and ultimate analyses, carbon forms, X-ray diffraction mineralogy and structure analyses, petrography and reflectance analyses, and iii | P a g e Raman microspectroscopy analysis) showed the presence of strong carbon-carbon bonds, similar to those found in graphite, and limited impurities (oxygen, nitrogen, sulphur, and hydrogen). The anisotropy percentages of the samples ranged between 22 and 49 %; the reference natural graphite sample had an anisotropy of 86 %. The three-dimensional structure of the chars can be described as turbostratic, with randomly orientated carbon layers, small graphite crystallite sizes, and large interlayer spacings. Raman microspectroscopy classified the chars as being “transitional” (being somewhere between amorphous and graphitic carbon) with the possibility as a precursor for synthetic graphite. iv | P a g e Contribution to science Journal publications published Badenhorst, C.J., Wagner, N.J., Valentim, B.R.V., Viljoen, K.S., Santos, A.C., Guedes, A., 2019. Separation of unburned carbon from coal conversion ash: Development and assessment of a dry method. Coal Combustion and Gasification Products 11, 89-96. https://doi.org/10.4177/CCGP-D-19-00002.1 Journal publications in preparation Badenhorst, C.J., Wagner, N.J., Valentim, B.R.V., Viljoen, K.S., 2019. A review of natural graphite occurrences and mining in southern Africa. Journal of African Earth Sciences. Badenhorst, C.J., Santos, A.C., Abagiu, T.A., Białecka, B., Całus-Moszko, J., Cruceru, M., Guedes, A., Lázaro-Martínez, J.M., Moreira, K., Popescu, L.G., Predeanu, G., Viljoen, K.S., Valentim, B.R.V., Wagner, N.J., 2019. Recovery of char concentrates for graphite substitution. Minerals. International conferences Badenhorst, C., Wagner, N., Valentim, B., Viljoen, F., 2018. Fifty shades of grey: The extraction of char from a variety of coal ash for consideration as synthetic graphite, in: 70th Annual Meeting of the International Committee of Coal and Organic Petrology (ICCP) extended abstracts. ICCP, Brisbane. https://www.iccop.org/documents/70th- iccp-meeting-program-and-abstracts.pdf/ Badenhorst, C., Wagner, N., 2018. Coal char as a substituting material of natural graphite in green energy technologies – Charphite (ERA-MIN meeting feedback presentation, Târgu Jiu). Badenhorst, C.J., Wagner, N.J., Valentim, B.R.V., Santos, A.C., Guedes, A., Białecka, B., Całus, J., Popescu, L.G., Cruceru, M., Predeanu, G., Viljoen, K.S., Lázaro-Martínez, J.M., Abagiu, T.A., 2019. Char from coal ash as a possible precursor for synthetic graphite – Recent developments of the Charphite project, in: World of Coal Ash (WOCA) Conference proceedings papers. University of Kentucky Center for Applied Energy Research, St.
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