In this study, the performance of Ni-FSM-16 and TiO2-FSM-16 photocatalysts in phenol red removal was explored. The XRD, FE-SEM, and BET tests were used to characterize the catalysts. All experiments were performed at ambient temperature and under UV (20 W). The parameters including dye concentration (20-80 mg/L), photocatalyst concentration (0-8 g/L), UV exposure duration, and contact time (0-160 min) were optimized using RSM software. BET values of Ni-FSM-16 and TiO2-FSM-16 were 718.63 m2/g and 844.93 m2/g, respectively. TiO2-FSM-16 showed better performance in dye removal than Ni-FSM-16. At pH 3, the maximum dye removal by TiO2-FSM-16/UV and Ni-FSM-16/UV was obtained 87% and 64%, respectively. The positive hole species had the main role in photocatalytic phenol red removal. The reusability study was done for up to 7 cycles, but the catalysts can be reused effectively for up to 3 cycles. The synergistic factor for the TiO2-FSM-16 and TiO2-FSM-16/UV processes were calculated to be 1.55 and 2.12, respectively. The dye removal efficiency by TiO2-carbon and Ni-carbon was slightly lower than those obtained by the FSM-16 ones. The TiO2-FSM-16 and Ni-FSM-16 catalysts had a suitable surface and acceptable efficiency in phenol red removal.