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Biodiesel is considered a renewable, green fuel as it is derived from renewable living resources like animal fats or vegetable oils. This research is utilized to investigate the possibility of using Solvay wastewater as a source of biodiesel catalyst, which is CaO. CaCl2 from Solvay wastewater reacts with CO2 to produce CaCO3. CaCO3 is then heated to produce pure CaO. Waste cooking oil, wastewater, and CO2, which are considered dangerous materials to the environment, are used to produce valuable products. This research has environmental and economic benefit benefits of using waste materials as a replacement for raw materials. The selected experimental parameters for the CaCO3 production step are stirring rate (500–1300) rpm, CO2 gas flow rate(900–2000) mL/min, amount of ammonia (15–35) mL, and glycerol volume (0–25) mL. The selected experimental parameters for the biodiesel production step are reaction time (2–6) h, methanol to oil ratio (9–15), catalyst loading (1–5) %, and reaction temperature (50–70) ◦C. The impact of reaction parameters on reaction responses was assessed using the response surface methodology technique. A formula that represents the reaction response as a function of all the independent factors has been created. The optimization of the process is done in two steps: the first one is for the CaCO3process while the second one is biodiesel production optimization. The first optimization was done to get the CaCO3 with minimum particle size and yield. The second optimization was done to get the maximum amount of biodiesel using minimum energy and low reaction conditions. Process optimization resulted in another economic benefit for this research. The resulted biodiesel yield equals 95.8% biodiesel yield at 2 h reaction time, 15:1 molar ratio of methanol to oil, 56 ◦C reaction temperature, and 1% catalyst loading.