Polyacrylamide (PAM) microhydrogels supported with hexadecyltrimethylammonium (CTAB)-peroxo-tungstophosphate (PTP) complexes were synthesized and characterized using scanning electron microscopy (SEM), Fourier transform infrared (FT-IR), energy-dispersive X-ray spectrophotometer (EDX), and element-distribution map (EDM). The results indicate that a CTAB-PTP/PAM composite microsphere with surface-wrinkle morphology and a PAM microgel core/CTAB-PTP shell structure were obtained. The surface-wrinkle structure changed with the amount of (TAB-VIP supported on the PAM microgels. The CTAB-PTP/PAM composite microspheres may find applications as reused catalytic material in diphase catalysis based on the oxidation of dibenzothiophene (DBT) with hydrogen peroxide, and the composite microspheres can be recycled three times with a small decrease in activity. (C) 2011 Elsevier Ltd. All rights reserved.