Fe-Mo-W catalysts were prepared by a sol-gel method and used in the catalytic selective oxidation of p-xylene (PX) to prepare terephthalaldehyde (TPAL). The results showed that Mo, Fe, and W exist as oxides in the composite, and the Fe-Mo and Fe-Mo-W catalysts were stable between 400 and 600 degrees C. The Fe-Mo-W catalyst was more easily reduced to a lower valence state, and the lattice oxygen of the Fe-Mo-W catalyst was higher than that of the Fe-Mo catalyst. These phenomena demonstrated a higher oxidation performance than the Fe-Mo catalyst. The Fe-Mo-W catalyst calcined at 550 degrees C was reacted at 500 degrees C for 3 h with a catalyst dosage of 0.5 g, an air flow rate of 1000 mL min(-1), and a PX liquid hourly space velocity of 1.2 mL g(cat)(-1) h(-1), the conversion of PX, the selectivity and the yield of TPAL was 99.5%, 74.0%, and 73.6%, respectively, and the Fe-Mo-W catalyst was stable after 50 h. (C) 2014 Elsevier B.V. All rights reserved.