The hunt for efficient and environmentally friendly degradation processes has positioned the heterogeneous advanced oxidation processes as an alternative more interesting and economical rather than homogenous processes. Hence, the current study lies in investigating the efficiency of different heterogeneous catalysts using transition metals in order to prevent the generation of iron sludge and to extend the catalogue of possible catalysts to be used in advanced oxidation processes. In this

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... , nickel and zinc were tested and the ability for radical-generation degradation capacity of both ions as homogeneous was evaluated in the electro-Fenton-like degradation of 2-phenylphenol. In both cases, the degradation profiles followed a first-order kinetic model with the highest degradation rate for nickel (1 mM) with 2-phenylphenol removal level of 90.12% and a total organic reduction near 70% in 2 h. To synthesise the heterogeneous nickel catalyst, this transition metal was fixed on perlite by hydrothermal treatment and in a biochar or carbon nanofibers by adsorption. From the removal results using the three synthesized catalysts, it is concluded that the best catalysts were obtained by inclusion of nickel on biochar or nanofibers achieving in both with removal around 80% before 1 h. Thus, to synthetize a nickel electrocatalyst, nickel doped nanofibers were included on carbon felt. To do this, the amount of carbon black, nickel nanofibers and polytetrafluoroethylene to add on the carbon felt was optimized by Taguchi design. The obtained results revealed that under the optimised conditions, a near-complete removal was achieved after 2 h with high stability of the nickel electrocatalyst that open the applicability of this heterogeneous system to operate in flow systems.