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Biofuel is a type of fuel that is made from biomass using modern techniques rather than the relatively slow geological processes that lead to the development of fossil fuels. In Europe, biodiesel is the most widely used biofuel. The sanitary ware industry generates a lot of hazardous waste, such as waste gypsum molds. These molds are broken, pulverized, and reacted with NaCO3 to make CaCO3, which is then heated to produce CaO. The resulting CaO catalyzes the reaction between waste frying oil and methanol for biodiesel synthesis. To evaluate the effect of reaction parameters on the production of biodiesel, the independent reaction parameters that were chosen are as follows: reaction temperature in the range 50–70° C, methanol to oil (M:O) molar ratio in the range 9–15, catalyst loading in the range 1–5%, and time in the range 2–6 hrs. The influence of the independent factors on the reaction-dependent responses was evaluated and it was found that reaction temperature and methanol-to-oil ratio have a major effect on the biodiesel yield. Reaction condition optimization has been studied to maximize biodiesel yield at minimum reaction conditions. The optimum process conditions are 93.4% biodiesel yield at an M:O molar ratio of 15 : 1, catalyst loading of 1%, reaction temperature of 53.6° C, and reaction time of 2 h. The results showed that resulted biodiesel catalyst (CaO) can be used one time; then, a fresh catalyst will be used.