| Summary: | Heterogeneous photo-electro-Fenton process is an attractive technology for the removal of recalcitrant pollutants. To better exploit the presence of an irradiation source, a bifunctional catalyst with TiO<sub>2</sub> nanoparticles embedded into an iron–chitosan matrix was developed. The catalytic activity of the catalyst was improved by the optimization of the loaded TiO<sub>2</sub> content. The prepared composite catalysts based on TiO<sub>2</sub>, Fe<sub>3</sub>O<sub>4</sub> and chitosan were called TiO<sub>2</sub>/Fe<sub>3</sub>O<sub>4</sub>-CS beads. The best catalyst with an optimal ratio TiO<sub>2</sub>/Fe = 2 exhibited a high efficiency in the degradation and mineralization of chlordimeform (CDM) insecticide. Under the optimum conditions (concentration of catalyst equal to 1 g L<sup>−1</sup> and applied current intensity equal to 70 mA), a real effluent doped with 30 mg L<sup>−1</sup> of CDM was efficiently treated, leading to 80.8 ± 1.9% TOC reduction after 6 h of treatment, with total removal of CDM after only 1 h.The generated carboxylic acids and minerals were identified and quantified. Furthermore, the stability and reusability of the developed catalyst was examined, and an insignificant reduction in catalytic activity was noticed for four consecutive cycles of the photo-electro-Fenton process. Analyses using SEM, XRD and VSM showed a good stability of the physicochemical properties of the catalyst after use.
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