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