Phenol is an industrially important chemical, generally produced via sulphuric acid catalysed decomposition of cumene hydroperoxide (CHP). The effluent containing the acid used as catalyst has to be neutralised and extracted to avoid corrosion and environmental problems. In the current work, a simple process was developed based on the use of nanocrystalline ZSM-5 (Si/Al = 100) catalyst. The catalyst was characterised by XRD, SEM, TEM, DLS and FT-IR analyses. The activity of this catalyst was tested for the liquid-phase decomposition of cumene hydroperoxide. The effects of various parameters such as, catalyst weight, catalyst particle size, concentration of CHP, reaction temperature and reusability of catalyst were studied. It was observed that the nanocrystalline ZSM-5 with smaller particle size showed superior activity. In addition, these catalysts have excellent reusability and can be used instead of sulphuric acid for selective decomposition of CHP into phenol and acetone with 100% conversion.