In this work, the separation of 1,3-propanediol (1,3-PD) from dilute fermentation broth coupling the reversible reaction 1,3-PD with acetaldehyde to form 2-methyl-1,3-dioxane (2MD) and a synchronous extraction of 2MD by o-xylene was studied experimentally. The equilibrium and reaction kinetics of the reactive extraction were established catalyzed by cation exchange resin HD-8. After eliminating the influence of internal and external diffusion, the rate constants of positive and reverse reaction were obtained by fitting the experimental data to a pseudo-homogeneous model. The results indicated that the reaction was a weakly exothermal reaction. The kinetics was found to be first-order in the concentrations of the reactants and the products. The results can help to design the reactor of reactive extraction of 13,-PD.