This study focused on the synthesis of TiO2–Zeolite nanocomposite through a sol–gel approach. The decrease in the size of the nanocomposite is considered a primary parameter to improve photocatalytic activity. In this regard, fabricated samples were exposed to laser irradiation (532 nm) for four different time intervals in order to investigate the size variation of the nanocomposite. FTIR, UV–Vis, XRD, DLS, SEM and EDX analyses were applied to characterize and determine the size of the products. An optimized nanocomposite sample, in term of the particle size, was used for photodegradation of 2,4-D herbicide from aqueous solution. Photodegradation was carried out under UV irradiation (12 W) and Xe lamp irradiation (200 W). The obtained results showed that laser irradiation time has a substantial effect on controlling the size of the nanocomposite. Results from the photocatalyst study indicated that the elimination of 2,4-D under the Xe lamp irradiation was higher compared with the UV irradiation. Also, the final synthesized nanocomposite exhibited higher catalytic activity for photodegradation of 2,4-D compared with pure Zeolite and pure anatase TiO2 samples. The reusability of TiO2–Zeolite nanocomposite was studied in four successive cycles to evaluate the removal of 2,4-D under UV irradiation.