Abstract: In order to remove refractory phenolics, activated carbon fibers supported cobalt phthalocyanine combined with H2O2 as a catalytic oxidation system to catalytic degradation of substituted phenols was studied. The adsorption of ACF and the catalysis of cobalt phthalocyanine were brought into fullest play in this system. The effect of catalytic oxidation was analyzed by UPLC after 5h reaction which under the condition of CoPc-ACF 0.4g, H2O2 100 mmol/L, 25 oC and substituted phenols from 0.2 mmol/L to 0.5mmol/L. The results showed that surplus rate of phenols were under 3%, the kind and number of substitutent group has little effect on catalytic oxidation. The by-products formed in the catalytic oxidation of substituted phenols were identified by GC-MS methods. Catalytic oxidation degradation mechanism of substituted phenols by CoPc-ACF/ H2O2 was proposed