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.