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Preparation methods and catalysis activity of the photocatalyst of nanometer TiO2/conjugated polymer complex were studied in the present research. The target catalyst could be activated by absorbing both ultraviolet and visible light (190–700 nm), whereas pure TiO2 absorbs ultraviolet rays (<380 nm) only. Furthermore, studies showed that the photocatalyst employed in this paper could depigmentize methyl orange solution in a few minutes under visible light. TiO2/conjugated polymer complex was a photocatalyst with high catalytical activity. The temperature of calcination plays an important role in depigmentation. The effect is summarized as—520≥560≫600>480≫440≫400 °C. The effect contributed to the TiO2 structure form changes and the increase of the degree of polymer conjugation. [Copyright &y& Elsevier]