This work compared the effect of soaking and roasting Phoenix dactylifera L. seeds pretreatment methods on oil yield. The conversion of the Phoenix dactylifera L. seed oil to fatty acid methyl ester (FAME) was conducted via transesterification reaction using Ce-Zr/Al-MCM-41 monometallic and bimetallic catalysts. The reaction conditions were optimized using response surface methodology based on the central composite design (RSM-CCD). The result shows a quadratic model fitting with an R2 value of ~0.98 from the analysis of variance. In addition, the optimum FAME yield of 93.83 was obtained at a reaction temperature of 60.5�C, a reaction time of 3.8 h, a catalyst concentration of 4 wt., and a methanol to oil molar ratio of 6.2:1 mol/mol. The effect of the regenerated catalyst was significantly maintained for five cycles. The fuel properties of the produced FAME lie within the values reported in studies, ASTM D6751, and EN14214 standards. © 2020 by the authors. Licensee MDPI, Basel, Switzerland.