Heterogeneous Fenton-like degradation of methoxychlor in water was studied over two FeS@LHDs and Fe3O4@LHDs catalysts prepared by anchoring hydrotalcites (LHDs) onto nano-FeS and nano-Fe3O4 particles respectively via an in situ growth method. The effects of different heterogeneous Fenton system, pH value, initial concentrations of methoxychlor, dioctylsulfosuccinate sodium (AOT) and H2O2, and temperature on the degradation of methoxychlor were systematically investigated. Typically, within the pH range studied (2.5-3.5) the maximum methoxychlor removal of 57.54% was achieved after degradation reaction time of 120 min. The methoxychlor degradation followed pseudo-second-order kinetic model, and its initial degradation efficiency was found to follow the equation of - v(o)=72.627e(-36.71/RT)(CMethoxychlor)(2). Methoxychlor was degraded by the Fenton system in two stages and the intermediates were mineralized to hexanoic acid, 3-hydroxy-4-methoxy benzoic acid, water and dioxide. The results demonstrate that heterogeneous Fenton process catalyzed by Fe3O4@LDHs and FeS@LDHs is promising in wastewater treatment.