| Summary: | <i>N,N</i>-Bis(2-hydroxyethyl) alkylamide or fatty acid diethanolamides (FADs) were prepared from a variety of triglycerides using diethanolamine in the presence of different transition metal-doped CaO nanocrystalline heterogeneous catalysts. The Zn-doped Cao nanospheroids were found to be the most efficient heterogeneous catalyst, with complete conversion of natural triglycerides to fatty acid diethanolamide in 30 min at 90 °C. The Zn/CaO nanoparticles were recyclable for up to six reaction cycles and showed complete conversion even at room temperature. The amidation reaction of natural triglycerides was found to follow the pseudo-first-order kinetic model, and the first-order rate constant was calculated as 0.171 min<sup>−1</sup> for jatropha oil aminolysis. The activation energy (<i>E</i>a) and pre-exponential factor (<i>A</i>) for the same reaction were found to be 47.8 kJ mol<sup>−1</sup> and 4.75 × 10<sup>8</sup> min<sup>−1</sup>, respectively.
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