Fe-impregnated 13X (Fe-13X) catalysts were prepared for catalytic wet peroxide oxidation (CWPO) of methyl orange (MO) solution in batch and continuous fixed bed reactors. A systematical study was carried out to investigate the influence of the main operating parameters on the batch reactor performance. The kinetic curves were analyzed by using a pseudo-first-order kinetic equation over the 30–70 °C temperature range. In addition, the effects of catalysts filling amount and feed flow rate on the catalytic performance of Fe-13X catalysts in a fixed bed reactor were studied. The experimental results showed that the Fe-13X catalysts achieved the highest activity (100% MO conversion and 74.5% chemical oxygen demand (COD) elimination ratio, respectively) at 25 min with trace mount of Fe leaching concentration (<2.1 mg/L) at the optimized reaction conditions (namely 1.0 g/L catalyst concentration, pH 2.0, 17.6 mM H2O2, 70 °C) in a batch reactor. Kinetic studies showed that two different reaction regions existed, and an activation energy of 51.9 kJ/mol for the second region was found. Under the optimal operating conditions found (namely, catalysts filling amount of 3.5 g, feed flow rate of 4 mL/min), the Fe-13X catalysts displayed high MO conversion (99.4%) and COD elimination ratio (77.1%) after continuously ran for 200 min in a fixed bed reactor.

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