The increasing demand of carboxylic acid products is drawing great attention toward its recovery from waste streams/dilute solutions. With the above aim, the reactive extraction of acrylic acid from aqueous solutions using tri-n-butyl phosphate (TBP) in different diluents (paraffin liquid, toluene, and butyl acetate) was studied. The distribution coefficients and equilibrium extraction coefficients were obtained. Comparison was made on the basis of different physical properties of the solvents like molecular weight, dipole moment, dielectric constant, and ET parameter. Results show that higher values of distribution coefficients by chemical extraction were obtained for TBP in inert diluents: paraffin liquid and toluene.