To efficiently address environmental pollution, we synthesized AC-coupled TiO2 nano-photo-catalysts and applied it to the degradation of high concentration 2,4-dichlorophenols (2,4-DCP). Herein, we have successfully coupled activated carbon (AC) to TiO2 by a sol gel method. The as-prepared optimized-amount TO/10AC nano-composites delivered unprecedented photo-catalytic activity as compared to the pristine TO nano-particles and degraded 100% 2,4-DCP in 2 h. According to the fluorescence spectrum, temperature-programed desorption curve, and O-2 electrochemical reduction curve related to the generated -OH amounts, it is inferred that the photo-catalytic activity is ascribed to the coupled AC for accepting electrons, promoting O-2 adsorption and promoting reactant adsorption. More importantly, no obvious deactivation was observed even after running at least five cycles; this excellent stability makes them auspicious photo-catalyst for the degradation of high concentration pollutants in practical applications. Besides, the scavenger experiments confirmed that super oxide radicals were the main active species that involve during the photo-catalytic degradation of 2,4-DCP. This work delivers a viable approach to develop the photo-catalysis by coupling a proper amount of AC with the TO for the remediation of high concentration environmental pollutants.