Biodiesel manufacturing using waste cooking oil is a cost-effective method for lowering the costs of production. Composites composed of CaO and MgO recovered from industrial waste may be utilized to create ecologically heterogeneous transesterification catalysts. The activity of the catalysts and the impacts of calcination temperatures and various weight percentages were examined. The efficiency of the MgO/CaO catalyst for producing biodiesel from waste cooking oil was studied under optimum conditions. The properties and structure of the catalysts were characterized by scanning electron microscopy, X-ray diffraction, and Fourier transform infrared, which proved the acceptable performance of the catalysts for transesterification of waste cooking oil.