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In this work, a techno-economic study for the solvent based extraction of methacrylic acid from an aqueous solution is presented. The involved phase equilibrium calculations in process design are verified by measured experimental data. First, experiments are conducted with different solvent candidates to measure LLE (liquid–liquid equilibrium) data and to establish the effects of extraction temperature and dosage of solvent. Next, the binary interaction parameters for the UNIQUAC model to be used for equilibrium calculations are fine-tuned with measured data. Then, a process for the solvent based extraction of methacrylic acid recovery is designed and verified through simulation with the regressed UNIQUAC model parameters. The optimal configuration of the process flowsheet is determined by minimizing the total annualized cost. Among the three solvent candidates considered-cyclohexane, hexane and toluene-the highest efficiency and the lowest total annualized cost is found with toluene as the solvent.