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Sorbents containing Fe loading on porous Al2O3 substrate with a high surface area for the desulfurization of hydrogen sulfide were synthesized by wet incipient method. The Fe loading content of 19.34 wt% is close to the theoretical value of 20 wt%, verified by the results of inductively coupled plasma (ICP) analysis. Various techniques such as X-ray diffraction (XRD), scanning electron microscopy-energy dispersive spectrometer (SEM-EDS), Brunauer–Emmett–Teller (BET) method, and Barrett–Joyner–Halenda (BJH) method were implemented to characterize the prepared sorbents. Multicycles of sulfidation/regeneration tests in a fixed-bed reactor showed that the 20 wt% Fe2O3/Al2O3 (cited as 20FA hereafter) sorbents can be regenerated and thus reused after the regeneration process. After ten sulfidation/regeneration cycles, the sulfur capacity of the tenth cycle remained approximately on a level of 64% of the sulfur capacity in the first cycle. It was observed that the sulfur capacity decreased during early sulfidation/regeneration cycles, while it kept at a constant value after the seventh cycle. The results based on the material characterization and sulfidation/regeneration performance evaluation showed that 20FA sorbent has desirable physical and chemical properties for the desulfurization of simulated syngas at high-temperature range. Therefore, 20FA sorbent has a potential useful for the multi-cyclic operation of sulfidation/regeneration process.