Biodiesel as a renewable fuel is made from renewable materials such as animal fats, plant oils, and can be used in compression ignition (diesel) engines by mixing with conventional diesel. Recently, nanocatalysts are being used to generate biodiesel, as they are able to make these reactions more sufficient by having a large surface-to-volume ratio. TiO2 and ZnO nanoparticles are categorized as metal oxide nanoparticles. Each of them has its own special characteristics. Besides, they show a level of cooperation which is discussed below.In this paper, in addition to the surface method employed for numerical analysis, the experiments on the biodiesel production from waste sunflower oil are implemented by transesterification method using TiO2ZnO nanocatalyst. Effective process parameters, including the reaction temperature, oil: alcohol molar ratio, catalyst percentage, and optimal conditions are determined and optimized accordingly. The highest product yield was 96.4% in the ratio of 1–6 methanol to oil, 60 °C, and 200 mg/L TiO2–ZnO nanocatalyst. An optimization study shows that the highest biodiesel production is possible using nanocatalysts of 264 mg/L at a temperature of 66 °C.