In this study, a micro-scale parallel plate reactor was built to electrochemically generate hydrogen peroxide (HO) and to develop the Fenton reaction in situ, for the treatment of toxic organic pollutants. Two types of carbon materials were compared and used as cathodes: unidirectional carbon fiber (CF) and reticulated vitreous carbon (RVC). As anode, a stainless steel mesh was used. The results of HO were experimentally compared by means of electrogeneration process. RVC cathode with dimensions of 2.5 × 1 × 5 cm (170 mA and variable voltage V = 2.0-2.7) and 180 min produced 5.3 mM HO, with an HO production efficiency of 54%. Unidirectional carbon fiber cathode produced 7.5 mM of HO (96% of HO production efficiency) when a voltage of 1.8 V was applied during 180 min to a total area of 480 cm of this material. Acid Orange 7 (AO7) was degraded to a concentration of 0.16 mM during the first 40 min of the process, which represented 95% of the initial concentration. Electrolysis process removed nearly 100% of the AO7 using both cathodes at the end of these experiments (180 min).
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