Abstract A low-cost NaP zeolite@TiO2 nanocomposite catalyst with zeolite Si/Al ratio lower than three were synthesized for the first time under hydrothermal condition. The nanocomposites were characterized by different methods such as Fourier transform infrared (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS), N2 physisorption, NH3 temperature-programmed desorption (NH3-TPD), fluorescence microscopy, thermal analysis (TGA/DTA) and zeta potential analysis. The results showed that a micro-meso structure NaP zeolite with higher surface area and acidity with respect to pure zeolite was prepared. TiO 2 nanoparticle was dispersed over the whole of zeolite without aggregation. A reduction of the TiO 2 bandgap nanoparticle was observed from DRS spectra. The photocatalytic activity of low-cost NaP zeolite@TiO 2 nanocomposite was tested for simultaneous methylene blue dye (MB) and chemical oxygen demand (COD) under solar and ultraviolet light. The result showed that the nanocomposite catalyst has great potential (above 90%) for COD removal discolouring of MB (about 99.6%) at room temperature. The optimum amount of some parameters such as the loaded amount of TiO 2 (0.36 g), catalyst dosage (0.1 g), time (2 h), initial dye concentration (100 mg/L), solution pH value (about 7) under solar light were considered. In addition, present negative charge in the surface that show in zeta potential confirm the high activity of catalyst to interaction with cationic dye. As a further advantage, the NaP zeolite@TiO 2 nanocomposite was easier to be separated in aqueous media than the pure TiO 2 powders, making possible the reuse several times (over five runs) without using oxidant. Finally, the NaP zeolite@TiO 2 nanocomposite was used for COD abatement in wastewater from two real industrial streams. The MB degradation kinetics were fitted by a pseudo-first-order model with K = 0.534 h −1 .