This study investigates the photocatalytic degradation of Procion Red MX-5B (PRM) using ZnO and Ni-doped ZnO catalysts derived from okra stalks through a green synthesis method. Various parameters, including hydrogen peroxide concentration (HPC), catalyst amount, nickel (Ni) doping amount, initial PRM concentration, and pH, are systematically studied to assess their impact on PRM degradation efficiency. The results reveal that both ZnO and Ni-doped ZnO catalysts exhibit promising photocatalytic activity, with the highest PRM degradation efficiency achieved at the following reaction conditions: 6 mM of HPC, 40 mg of Ni(7%):ZnO catalyst, 10 ppm initial PRM concentration, and pH = 6. Under these conditions, the Ni-doped ZnO catalyst demonstrated a degradation efficiency of 98.08% compared to 82.99% for the ZnO catalyst. The study highlights the potential of these catalysts for efficient organic pollutant removal and provides valuable insights into the factors influencing their photocatalytic performance.