Optimization of process conditions for biodiesel production through methanolysis of Indian mustard oil (MO) using magnesium-impregnated, precalcined fly ash heterogeneous base catalyst has been performed, using “response surface methodology” based on a four-factor, three-level “face-centered central composite design”. A quadratic polynomial model was formulated for estimation of biodiesel (fatty acid methyl ester, FAME) yield by multivariate regression analysis. Optimal parametric values corresponding to maximum experimental FAME yield (i.e., 97.5 wt %) were as follows: methanol:MO molar ratio, 13.13:1; calcination temperature, 950 °C; catalyst concentration, 3.44 wt %; and stirrer speed, 890 rpm. The optimal magnesium base catalyst possessed a BET specific surface area of 9.07 m2/g, a catalyst pore volume of 0.0255 cm3/g with a modal pore diameter of 6.5 nm, and appreciable (11.52 mmol HCl/g catalyst) catalyst basicity. The formulated B10 biodiesel conformed to ASTM/European specifications. Thus, the optimally prepared low-cost and reusable catalyst can craft economical avenues for fuel-grade biodiesel synthesis from mustard oil.

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Novel Ni-Fe solid acid catalyst was prepared through co-wet impregnation of Fe 2 (SO 4 ) 3 ·H 2 O and Ni (NO 3 ) 2 ·6H 2 O on fly ash (FA) support. XRD, BET-BJH, SEM-EDX, XPS and FTIR methods were employed to characterize the catalyst. The excellent catalyst activity was assessed and optimized in the production of methyl oleate (biodiesel/dieseladditive). The response surface methodology (RSM) computed optimal parametric values pertaining to maximum oleic acid (OA) conversion (98.37 ± 0.01%) were 15:1 methanol/OA molar ratio, 1:15:2 nickel nitrate: ferric sulphate:FA (wt. ratio) and 4 wt.% (of OA) catalyst concentration in 1 h under conventional heating at mild reaction temperature (60°C). The optimal catalyst possessed 27.64 m 2 /g specific surface area and 0.0233 cc/g pore volume with predominantly mesoporous framework. XPS bands confirmed the presence of Fe 3+ and mixed Ni 2+ /Ni 3+ species rendering an acidity of 5.5 mmol KOH/g. The catalyst comprised of crystalline Fe 2 O 3 , Ni 2 O 3 and NiS phases as revealed from XRD analysis. This study also reports the remarkable intensification of esterification reaction through an energy-efficient application of far-infrared radiation protocol (1/3 rd of conventional power requirement) resulting 99.20% OA conversion in only 10 min at the derived optimal conditions.

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