MIL-53 (Fe) Metal Organic Framework (MOF) was synthesized by a hydrothermal method and characterized by SEM, XRD, FT-IR and Brunauer−Emmett −Teller techniques. The synthesized MOF was successfully applied as an efficient catalyst at Electro-Fenton degradation of linear alkyl benzene sulfonate (LAS) surfactant, so that Kapp for LAS degradation showed significantly higher amounts in presence of Fe MOF. Effect of experimental parameters on Electro-Fenton degradation including pH, MOF amount, applied current, Fe (II) concentration and electrodes distance were investigated and optimized amounts were found. Applying of MOF caused efficient removal of LAS in higher pHs in compared when MOF not applied. Catalytic electrochemical degradation in this work showed removal more than 98% of initial surfactant in completely satisfying time duration.