This paper presents an optimization technique, based on Supertargeting Approach, for the synthesis of solvent extraction and ion exchange network, which broadly falls under Mass Exchange Network (MEN). The present work is related to the recovery of zinc from spent pickle liquor and the rinse water, an effluent of galvanizing and metal finishing industry. The minimum composition difference of zinc, 'epsilon', between operating condition and equilibrium condition is found to be a key optimization variable. This paper describes the targeting as well as designing procedures for optimization of present MEN. During the design stage, it has been possible to achieve the targeted results.