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The Fe-TiO₂ photocatalysts synthesized by a sol–gel method have the mesoporous structure with a narrow pore size distribution, large pore volume and high surface area. The incorporated Fe³⁺ substitutes the octahedrally coordinated Ti⁴⁺ in the TiO₂ lattice to extend the absorption of TiO₂ to visible light region and promote the formation of electron–hole pair. Additionally, the separation and transportation efficiency increase with the doping of Fe³⁺ increasing from 0.1% to 0.7%, while decreases remarkably with the doping concentration increasing from 0.7% to 1.5%. The Fe-TiO₂ shows excellent photocatalytic performance for toluene degradation under visible light irradiation. The optimal Fe/Ti ratio is 0.7%. Partial deactivation of the photocatalytic activity was observed after 20 consecutive reaction runs. From the in situ DRIFTS experiment, the deactivation reason can be attributed to the formation of stable …