The nitration of toluene using solid acid catalyst is carried out in batch and semi-batch reactors with or without continuous water withdrawal. The effect of process parameters viz., nature of catalyst, agitation speed, nitric acid-toluene dispersion morphology, catalyst to toluene ratio, temperature, nitric acid dosing and boil-up rates (BRs) on overall conversions, and para-selectivity is investigated. The micro-reaction environment around the catalyst particle and its influence on lattice aluminum transformation to achieve improved para-selectivity has received special attention. These studies have established the importance of dispersion morphology of reactants and microenvironment around catalyst particles for achieving preferred conversion and para-selectivity in toluene nitration.