Extraction followed by heterogeneous azeotropic distillation is an effective and energy-saving method to separate acrylic acid from aqueous solution. In this work, the liquidliquid equilibria data for the system of water + acrylic acid + cyclopentyl methyl ether at three temperatures were determined at 100.249 kPa. The reliability of the liquidliquid equilibria data was ascertained by using Hand and OthmerTobias correlations. The separation factors of cyclopentyl methyl ether at different temperatures were compared. NRTL and UNIQUAC models were used to correlate the liquidliquid equilibria experimental data. Moreover, a comparative study on the three solvents, including cyclopentyl methyl ether, isobutyl ethanoate, and 4-methyl-2-pentanone, was made in terms of basic physical properties and extraction ability.