This work is a fundamental study for applying hybrid process coupling adsorption with microfiltration to waste-water treatment. Phenol was separated by adsorption on powdered activated carbon, adsorbed phenol with activated carbon was separated by microfiltration. As the particle size in suspension increased, filtration resistance decreased, and effect of particle concentration on resistance was less pronounced. The rate of uptake was greatly dependent on the degree of phenol loading. For a smaller amounts of activated carbon, the change of permeate concentration before break point and phenol loading with time were steeper than in the case of large amounts. Permeate concentration before break point decreased with decreasing particle size, this could be due to the increase of outer surface of particle and film mass transfer coefficient.