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TitlePreparation and characterisation of graphitisable carbon from coal solution
AuthorKgobane, B.T. (Bethuel Lesole)
AbstractThe energy demands by the industrial world are continuing to rise, while the rate of new oil discoveries is falling. Within the next 30 years, available petroleum supplies are likely to fail to meet the demand, and oil will no longer be able to serve as the world’s major energy source. Coal, being relatively abundant worldwide and potentially adaptable for use in existing plants that have been engineered for petroleum use, can serve as an inexpensive substitute for, or successor to, the more expensive oil fuels in use today. Graphitisable carbon is one of the high-value products from petroleum as its value lies partly in the nuclear industry. Making graphitisable isotropic carbon from well-purified coal is therefore a primary motivation for this study. However, its purity is far too low. Substantial purification is obtained by dissolving the organic part of coal in dimethylformamide with the addition of a little alkali. Results indicated that more than 90% of the organic part of a 10% ash flotation product dissolved in N, N dimethylformamide on addition of 10% NaOH. The bulk of the impurities are removed by centrifugation and the dissolved organic material is recovered by water precipitation. Subsequently, the ash level is lowered from 10% in the coal to high S-2 coal extracts derived at high temperature (GSF-25HT) and no S-2 coal extracts derived at room temperature (GSF-0RT) > no S-2 coal extracts derived at high temperature (GSF-0HT), corresponding to 79 > 75% and 67 > 25% respectively. The interlayer spacing (d002 -value) of the graphites follows the order GSF-25RT (3.37Å) 61 > 62%, corresponding to 0.44 > 0.88 > 1.60 acetylene black. With the addition of carbon black, the decreasing order of graphitisation was 57.7 > 56.5 > 51.5%, corresponding to 0.44 > 0.88 > 1.60 wt % respectively. The interlayer spacing d002, increased in the same order, suggesting a shift towards a turbostratic and formation of a poorly graphitised, and turbostratic carbon. Raman spectroscopy revealed that the intensity ratio R of the g to the d peak decreased with increasing dosage of the carbon additive. Cokes produced from the coal extracts prepared at 25oC but without S-2 showed also a remarkable degree of flow texture. Its crystalline domain units were relatively small. The resin-mounted coke samples observed under an optical microscope (objective x 25) showed reduced flow texture with the addition of carbon black. The graphitisability of the resultant cokes also decreased on addition of carbon black. The optimum dosage observed for reducing the flow texture without reducing the crystallinity was found to be < 0.22%. Improved degree of graphitisation of the carbon was studied on addition of iron (lll) compounds. Iron (lll) compounds showed a promising improvement in the graphitisability of the carbon when added in small amounts. The intracellular hard carbon is converted to soft carbon, thereby improving the degree of graphitisation. The overall effect was a more isotropic graphitic carbon but the degree of graphitisation obtained was far too low: on addition of 1% and 3% (by wt) of iron (lll), the compounds were 21% and 27% respectively. Oxygen intrusion into the precursor’s coal material prior to heat treatment is thought to have inhibited the degree of graphitisation. Increasing the amounts of the iron (lll) compound and prohibiting the intrusion of oxygen during mixing could improve the graphitisability of carbon. However, the optimum amount to be used remains an important subject to be explored in future.
AbstractThesis (PhD (Chemistry))--University of Pretoria, 2007.
IdentifierKgobane, B 2007, Preparation and characterisation of graphitisable carbon from coal solution, PhD thesis, University of Pretoria, Pretoria, viewed yymmdd