Sulfated zirconia (SZ) is a widely used catalyst, which is synthesized by a solvent free method and the synthesized catalyst has been characterized. Neem Methyl Ester (Biodiesel) was prepared by a two-step process of esterification and transesterification from Neem oil with methanol in the presence of catalyst. Acid catalyst was used for the esterification and alkali catalyst (KOH) for the transesterification reaction. Optimal Free Fatty Acid (FFA) conversion was achieved using 1 wt% SZ as an acid catalyst with a methanol-to-oil molar ratio of 9:1, temperature of 65ºC and reaction time of 2 h. The acid value was reduced to 94% of the raw oil (24.76 mg KOH/g), which confirmed the conversion. Consequently, this pretreatment reduces the overall complexity of the process and a conversion efficiency of 95% is achieved when pretreated oil reacts with methanol in the presence of KOH.