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In this study, a novel photocatalyst of TiCX/porous carbon-carbon sphere (TiO2/PC-CS) composites was prepared by a sol-gel combined hydrothermal method. The obtained materials were characterized via SEM, XRT), contact angle analysis, Nv adsorption-desorption and FT-IR. The photocatalytic performance was measured by degrading the simulated wastewater contained toluene solubilized by TX-100. Based on the characterizations and photocatalytic results, a possible photocatalytic mechanism was proposed. The results reveal that the as-obtained PC showed favorable features for adsorption, such as high specific surface area and developed pore structure. After loading CS and TiO2, the interface hydrophilicity of the composites was adjusted, and Ti-O-C bond was formed between TiOv. and PC-CS. The photocatalytic degradation process of solubilized toluene was consistent with the pseudo-first-order kinetic equation, and the correlation coefficient was above 0.97. Compared with photocatalytic degradation effect of toluene and TX-100, it could be seen that the TiO2/PC-CS had selective adsorption and degradation ability in treating solubilized toluene in wastewater. In the case of the concentration of TX-100 was 0.2 mmol / L at 25 °C, the selective photocatalytic degradation efficiency of TiO2/10% (PC-CS) towards toluene was as high as 87.45%. [ABSTRACT FROM AUTHOR]