In the present study, novel copper-incorporated MCM-41-type high-surface-area mesoporous materials were synthesized following a direct hydrothermal synthesis method and also by the impregnation of copper into the mesopores of the pre-synthesized MCM-41 structure. XRD results indicated the formation of a CuO phase within the MCM-41 structure. Sharp H2S breakthrough curves, quite high sorption rate parameters, and high sulfur retention capacities were obtained in high-temperature removal of H2S using these copperincorporated mesoporous materials. XRD patterns of the sulfided products indicated the formation of a Cu1.81S phase within the MCM-41 structure. A deactivation model gave good predictions of the experimental H2S breakthrough data.