Water resources are depleting, and the availability and supply of clean, potable water are a global concern. Advanced oxidation processes (AOPs) possess immense prospects in water and wastewater treatment settings. This study investigated and optimized the photocatalytic treatment of wastewater using titanium dioxide (TiO2) as the photocatalyst. The one-factor-at-a-time (OFAT) technique was employed to evaluate the effects of reaction time (20–100 min), mixing speed (20–100 rpm), and catalyst load (0.3–1.5 g/L) on pH, colour, turbidity, and chemical oxygen demand (COD) removal from actual municipal wastewater. Reaction time and catalyst load were then identified as the two key factors selected to be modeled and were optimized for turbidity and COD removal using the Central Composite Design (CCD) of response surface methodology (RSM). These statistical models were developed and used to optimize the operating conditions. The results obtained showed a desirability efficiency of 74.7% at a 95% confidence level. The RSM model predicted results at the optimum conditions and showed reasonable agreement with the experimental results obtained. The optimal responses achieved were 32.64% COD removal and 95.17% turbidity removal. A comparative study between UV light and visible light was also conducted at optimum conditions, whereby the UV light was demonstrated to be highly effective for turbidity and COD removal. The optimal responses achieved were 25.58% COD removal and 66.88% turbidity removal for visible light.