Bisphenol F (BPF) is a substitute agent for bisphenol A and is widely used in the production of materials such as epoxy resins and plastics. BPF accumulates in surface water because of its nonbiodegradable and recalcitrant nature, making it difficult to remove. In this study, the removal of BPF through a photocatalytic process was evaluated using zinc oxide (ZnO)/reduced graphene oxide (RGO) microspheres. A spray drying method was used to prepare the ZnO/RGO microspheres, which combine the photocatalytic efficiency of ZnO with the high electron mobility and large surface area of RGO, achieving a bandgap of 2.53 eV. Structural and morphological analyses confirmed the successful hybridization of the ZnO/RGO microsphere composite. The photocatalytic activity of the ZnO/RGO microspheres was evaluated under various light sources, with the highest degradation efficiency achieved under ultraviolet C irradiation. The optimal catalyst dosage of the ZnO/RGO microspheres was determined to be 0.1 g/L for BPF removal (BPF initial concentration = 5 mg/L). Scavenger tests revealed the dominance of superoxide radicals ( O2 ·−) in the degradation process. The effects of pH (3.52–9.59), ions ( Cl−, NO3 −, and SO4 2−), and natural organic matter were also examined to assess the practical applicability of the ZnO/RGO microsphere photocatalytic system. High pH levels and the presence of NO3 − (> 10 mM) were found to enhance BPF removal. This research highlights the potential of the ZnO/RGO microspheres as efficient photocatalysts for the removal of BPF in aqueous solutions.