This work evaluated the efficiency and systemic application of heterogeneous photocatalytic degradation for dairy wastewater under advanced oxidation process (AOP) utilizing solar radiation and immobilized ZnO as measured by total organic carbon (TOC). The AOP system consisted of a semibatch reactor and glass tank operated with an initial volume of 3 L of dairy wastewater. ZnO was immobilized on a metal plate of 800 × 250 mm and used as a catalyst bed. Evaporation rate was considered when effective degradation of the photocatalytic system was determined. The AOP utilized Taguchi's L 8 orthogonal array. The entry variables were pH, reaction time, initial organic load in the effluent, and ZnO coating thickness on the catalyst bed. When optimized, an effective TOC degradation of 14.23% was obtained under variable values of pH 8.0, a metal-plate coating of 100 micrometers (µm) ZnO, and total reaction time of 180 min.