In this work, a heterogeneous catalyst was developed from waste fish bone. ZnO was deposited onto the waste fish bone to enhance the surface properties along with ion exchangeability. After characterization, the developed catalyst was found to have a much higher surface area (217 m2 · g−1) than that of raw fish bone (10 m2 · g−1). This catalyst was used during peroxidation of oleic acid rich Azadirachta indica oil (neem oil) to observe its suitability and efficiency. A quadratic model was developed with five input variables (temperature (T), time (t), g/g of catalyst (HZn), H2O2:oil ratio (γH:FA), formic acid:oil ratio (γF:FA)) and 2 output variables (Iodine value, Oxirane Oxygen Conversion). The optimized parametric values for T, t, HZn, γH:FA, and γF:FA were found to be 60 °C, 3.88 h, 20 g/g, 19.05:1, and 19.85:1 respectively. The final epoxidized oil was characterized using FTIR and 1HNMR. The reusability of the catalyst was studied both quantitatively and qualitatively.