Mesomacroporous silica containing iron oxide nanoparticles (15-20 nm) was synthesized by formulating solid lipid nanoparticles and metallosurfactant as both template and metal source. Because of the high active surface area of the catalyst, the material exhibits an excellent performance in a Fenton-like reaction for methylene blue (MB) degradation, even at low amount of iron oxide (5% TOC after 14 h).