LiFe(WO4)(2) particles were synthesized successfully and used as a Fenton-like catalyst. The structure and morphology were characterized using scanning electron microscopy (SEM) and X-ray powder diffraction (XRD). The degradation of methylene blue (MB) under atmospheric pressure was studied as a model experiment to evaluate the catalytic activity of these particles. The results showed that the catalyst had catalytic activity in the treatment of solution containing MB and 99.7% decolorization efficiency of MB (500 mg L-1) was achieved within 60 min under the optimum conditions. Moreover, LiFe(WO4)(2) was demonstrated to have good stability and reusability, indicating it could be a suitable heterogeneous Fenton-like catalyst. Based on the results, a reasonable mechanism was investigated to interpret the degradation process of MB. Crown Copyright (C) 2010 Published by Elsevier B.V. All rights reserved.