Mexican dolomites were doped with sodium nitrate and calcined at 900 °C to generate the corresponding CaO/MgO and Na-CaO/MgO mixed metal oxides. The resulting oxides were tested with regard to the catalytic transesterification of commercial canola oil in a batch reactor for biodiesel production. The catalysts were characterized using several spectroscopic and physicochemical techniques. Among all catalysts, Na-CaO/MgO effected the highest conversion rate, at 95.4%. The experimental catalytic parameters were processed in a nonlinear program to obtain the optimal theoretical conversion rate of 97.46%, consistent with the experimental results.