The present work describes an attractive and economically viable novel separation technique using superabsorbing hydrophilic polymer gel for dewatering an industrial o-toluidine-water emulsion. It is demonstrated that the initial water content of 30% in the emulsion is reduced to 3% within 10 min by using a semicontinuous separation strategy, which can have significant energy savings over the conventional distillation process. The mechanism of water removal and the effect of the presence of interfacial agents on the rate of water removal are also studied.