Hydrodynamics and separation performance of a sieve tray column in heterogeneous distillation are studied experimentally under total reflux conditions. A correlation for clear liquid height in the heterogeneous liquid region is obtained by modifying the correlation of the homogeneous systems. The volumetric dimensionless diffusion fluxes in the heterogeneous liquid region are smaller than those in the homogeneous liquid region. This may be due to the mass transfer resistance in the liquid phases. In order to examine the effect of liquid-phase resistance on separation performance, a simulation is carried out by either considering or neglecting the liquid-phase resistance. The simulation shows that the liquid-phase resistance affects the vapor-phase concentration driving forces, volumetric diffusion fluxes and convective mass flux in the heterogeneous liquid region. It also shows that the predicted top vapor concentrations and flow rate are in reasonable agreement with the experimental data in the heterogeneous liquid region by considering the liquid-phase mass transfer resistance.