Methyl orange (MO) molecules had been removed from aqueous solution by nano-TiO 2 /exfoliated graphite composites with the combination of ultrasound/adsorption/photocatalysis. The experimental results had showed that nano-TiO 2 /exfoliated graphite composites provided with the adsorptive capability of exfoliated graphite and the photocatalysis capability of nano-TiO 2 synchronously. It had been proved that the removal ratios related to the adsorption and photocatalysis capability of the composites and were influenced by US and UV irradiation, the reaction times, the reaction temperatures, the initial pH values, the dosages and the initial MO solution concentrations. Moreover, it had been illuminated that the combination was very effective and useful on removing MO molecules from aqueous solution.