In this work, functionalized mesoporous zirconia have been synthesized by a simple chemical process, in the presence of pluronic F127, MPTMS and toluene. The microscopic assembly of the thiol functionalized material and the crystallinity of the pore walls were studied by using small X-ray powder diffractions. Batch adsorption study was conducted to investigate the removal of methyl blue from waste water by using thiol functionalized mesoporous zirconia. Adsorption experiments were conducted as a function of adsorbent dose, equilibrium pH, contact time, initial concentration, adsorption kinetics and adsorption isotherms. The characterization and mechanisms involved in adsorption of methyl blue on the material were studied by using instrumental technique like XRD, FTIR, SEM, BET and chemical methods. The adsorption kinetic studies indicated that the overall adsorption process was best described by pseudo-second-order kinetics. The adsorption data were fitted linearly transformed Langmuir isotherm with R2 (correlation coefficient) > 0.97. The results indicate that thiol functionalized mesoporous zirconia can be used as an effective and low cost adsorbent for the treatment of wastewater