In the present study, a highly mesoporous MCM-41nano-adsorbent was synthesised, characterised using FTIR, SEM, EDS and XRD analysis and applied for treatment of phenolic wastewater. In order to enhance the phenol adsorption efficiency, adsorption parameters, such as pH, MCM-41 dosage and initial phenol concentration was optimised by employing central composite design (CCD) and response surface methodology (RSM). Result revealed that pH and adsorbent dose were found to have significant influence on phenol adsorption on to MCM-41. Further, among these significant factors adsorbent dose showed a large positive effect and pH showed strong negative effect on the phenol removal efficiency. Further, it was observed that interaction effect between pH and phenol dose had significant effects on phenol removal efficiency from the synthetic wastewater. At an optimum combination of pH 5.2, phenol dose 132 mgl–1and 2.6 gl–1of MCM-41more than 99% phenol adsorption along with 96% of toxicity removal was achieved. Thus, mesoporous MCM-41 can be potentially employed for the treatment of industrial wastewater contaminated with phenol.