The sol-gel method combined with electrospinning was used to synthesize polyvinylpyrrolidone nanofibers loaded with a mixture of Zn(Ac)(2)center dot 2H(2)O, Fe(NO3)(3)center dot 9H(2)O and AgNO3, which generated mesoporous carbon fibers loaded with compounds including ZnFe2O4, Fe3O4 and Ag after heat treatment at 850 degrees C in a N-2 atmosphere. Mesoporous carbon fibers loaded with ZnFe2O4-Fe3O4-Ag had a uniform pore size distribution, high specific surface area and strong ferromagnetism. They displayed high photocatalytic activity toward the degradation of methylene blue and methyl orange under visible light irradiation. This kind of complex magnetic semi-conductive mesoporous carbon fiber can be repeatedly used as a photocatalyst to dispose of organic wastewater. This simple synthesis method can be used to prepare other complex materials with multi-functional components. Crown Copyright (C) 2011 Published by Elsevier Ltd. All rights reserved.