A series of spherical activated carbons (SACs) with different pore structure were prepared from divinylbenzene-based polymer through CO2 activation. The effect of activation temperature and retention time on the yield and textural properties of the resulting SACs were studied. The SACs were characterized by N-2 adsorption, X-ray diffraction, scanning electron microscopy, and aqueous adsorption assays. Either increasing activation temperature or extending retention time decreases the yield of SACs. The BET surface area and pore volume increase with activation temperature and reach a maximum at 1000 degrees C and then decrease at higher activation temperatures. At 1000 degrees C, BET surface area, total pore volume, and mesopore pore volume increase with retention time from 0.5 to 2 h, and meanwhile micropore volume decreases. The micropores are gradually widened into mesopores with increasing activation temperature or extending retention time. SEM and XRD analyses of SAC10 verify the presence of developed porous structure composed of disordered micrographite stacking. Aqueous adsorption assays indicate that SACs have good adsorption capacity for phenol. (C) 2008 Wiley Periodicals, Inc.