Abstract
Optimization studies for the esterification and transesterification of oil extracted from Croton gratissimus grains were carried out using the response surface methodology (RMS) that utilizes the central composite design (CCD) and the analysis of variance (ANOVA). A 23 full-factorial rotatable CCD for three independent variables at five levels was developed in each case, giving a total of 20 experiments needed per study. The three design factors chosen for study were the catalyst concentration, methanol-to-oil ratio, and the reaction temperature. The values of the acid value of oil (in esterification) and the percentage FAME yield and FAME purity (in transesterification) were taken as the responses of the designed experiments. In the optimization of the esterification and transesterification processes, the ANOVA showed that both quadratic regression models developed were significant. The optimum operating conditions for the esterification process that could give an optimum acid value of 2.693 mg KOH/g of oil were found to be 10.96 mass% SO42–/ZrO2 catalyst concentration, 27.60 methanol-to-oil ratio, and 64°C reaction temperature. In the optimization of the transesterification process, the model revealed that the catalyst concentration and the methanol-to-oil ratio were the terms that had the most influence on the % FAME yield and the % FAME purity of the final biodiesel product. From the combined regression model, it was established that optimum responses of the 84.51% FAME yield and 90.66% FAME purity could be achieved when operating the transesterification process at 1.439 mass% KOH catalyst concentration, 7.472 methanol-to-oil ratio, and at a temperature of 63.50°C. Furthermore, in the two-step biodiesel synthesis, a predominantly monoclinic-phased sulfated zirconia (SO42–/ZrO2) catalyst exhibited high activity in the esterification of high free fatty acid oil extracted from Croton gratissimus grains. A 91% reduction in the acid value of the Croton gratissimus oil from 21.46 mg KOH/g of oil to 2.006 mg KOH/g of oil, well below the 4 mg KOH/g of oil maximum limit, was achieved. This resulted in the high FAME yield and purity of the biodiesel produced in the subsequent catalytic transesterification of oil using KOH.
Highlights
Concerns of dwindling crude oil reserves and global environmental degradation arising from the extensive use of petroleum-based fuels have made the biofuels-focused research more relevant than ever
The two quadratic models developed for the transesterification process predicted two sets of factor values for catalyst concentration, the methanol-to-oil ratio, and reaction temperature corresponding to the optimum values of the 2 responses, FAME yield and FAME purity
The monoclinic sulfated zirconia, SO42–/ZrO2 catalyst has high acid strength and exhibits high catalytic activity; both qualities found in the tetragonal-phased type catalyst
Summary
Concerns of dwindling crude oil reserves and global environmental degradation arising from the extensive use of petroleum-based fuels have made the biofuels-focused research more relevant than ever. A biodiesel process must be energy efficient, allowing sufficient throughput volumes to be achieved whilst keeping the energy demand to a bare minimum It is for this reason that the wholesale of non-edible vegetable crops (Croton gratissimus being one of them) is being investigated as potential feedstock in biodiesel processes (Atabani et al, 2012) to produce high quality biodiesel whilst operating at moderate conditions, of temperature and pressure, and over shorter reaction times. The production of biodiesel from high FFA crops, unlike from oils extracted from edible vegetable crops, requires a conventional twostep process approach This begins by reducing the acid value of oil to below 4 mg KOH/g in the esterification reaction step over a homogeneous or heterogeneous acid catalyst before the main basecatalyzed transesterification reaction step. High free fatty acid oil extracted from the grains was subjected to an esterification reaction process carried out over a synthesized monoclinic ZrO2SO4 catalyst followed by a transesterification reaction process over a homogeneous KOH catalyst
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