Abstract: Expanded graphite-based carbon/carbon composite was prepared with sucrose as carbon source and phosphoric acid as activator. The thickness of acticarbon film could be controlled by changing sucrose solution concentration. Microstructure was observed and the effect of carbon film thickness of the composite on phenol adsorption kinetics was analyzed. The results show that the adsorption property of phenol adsorption kinetics correlated well with the pseudo-second rate equation. The initial adsorption rates raised with the decrease of thickness of the acticarbon film. The particle internal dispersion mechanic dominated during phenol adsorption of composite.