Rapid industrialization is causing a serious threat for the environment. Therefore, this research was aimed in developing ceramic cobalt ferrite (CoFe2O4) nanocomposite photocatalyst coated with coal fly ash (CFA-CoFe2O4) using facile hydrothermal synthesis route and their applications against methylene blue. The pristine cobalt ferrite photocatalyst was also prepared, characterized, and applied for efficiency comparison. Prepared photocatalyst were characterized by X-ray diffraction (XRD), fourier transformed infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy with energy dispersive spectroscopy (SEM/EDS). Optical response of catalysts was check using photoluminescence spectroscopy (PL). pH drift method was used for the surface charge characteristics of the material under acidic and basic conditions of solution pH. The photocatalytic degradation potential of all the materials were determined under ultra-violet irradiations. The influencing reaction parameters like pH, catalyst dose, oxidant dose, dye concentration, and irradiation time, were sequentially optimized to obtain best suited conditions. The 99% degradation of 10 ppm methylene blue was achieved within 60 min of reaction time under pH = 5 and 7, catalyst dose = 10 and 12 mg/100 mL, oxidant = 12 mM and 5 mM for cobalt ferrite and CFA-CoFe2O4 photocatalysts, respectively. Afterwards, the radical scavenging experiments were conducted to find out the effective radical scavengers (˙, h+, and e−) in photocatalytic degradation process. The kinetic study of the process was done by applying 1st order, 2nd order, and BMG models. Statistical assessment of interaction effect among experimental variables was achieved using response surface methodology (RSM).