Industrial　solid　waste　can　be　used　as　nanoparticles　potential　supports　to　form　heterogeneous　catalysts　for　removing　organic　substances.　Herein,　coal　gangue　was　modified　by　sulfuric　acid　pickling　and　high-temperature　calcination,　and　FeCo2O4/modified　coal　gangue　(FC-MCG)　catalysts　were　synthesized　via　a　citric　acid　combustion　method.　The　crystal　structures,　surface　morphology　and　elemental　valence　of　the　synthesized　composites　were　investigated.　The　20%　FC-MCG　possessed　higher　catalytic　performance　for　HA　degradation　than　other　composites,　achieving　almost　85%　degradation　efficiency　of　HA　(20　mg/L)　in　the　presence　of　PMS.　The　fluorescence　EEMs　and　FTIR　spectra　revealed　the　effective　destruction　of　HA　structure　after　reaction　in　the　20%　FC-MCG/PMS　system.　Electron　paramagnetic　resonance　(EPR)　tests　and　quenching　experiments　showed　that　the　SO4　center　dot-,　(OH)-O-center　dot　and　O-1(2)　were　produced　in　the　PMS　activation　process.　Additionally,　the　20%　FC-MCG　catalyst　still　kept　excellent　catalytic　performance　after　four　times　repeated　use.　This　study　was　a　meaningful　exploration　for　conversion　of　industrial　solid　waste　to　high　effective　catalyst　for　wastewater　treatment.