ZnFe2O4 nanoparticles (ZFNPs) were developed as catalyst for the degradation of benzotriazole (BTA) by heterogeneous photoelectro- Fenton (PE-Fenton) like process. ZFNPs were prepared by a co-precipitation process and then characterized with transmission electron microscopy (TEM), X-ray fluorescence (XRF), X-ray diffraction (XRD) and BET surface area. Using such ZFNPs as catalyst, the degradation of BTA was investigated. Due to the high catalytic activity of ZFNPs, PE-Fenton like process showed efficient degradation of BTA. The influencing factors such as pH, dosage of ZFNPs, applied potential and initial concentration of BTA were systematically investigated. Under the optimum conditions, 91.2% of BTA was removed after 180 rain treatment.