ZnFe 2 O 4 /AC composites were prepared by the one-pot hydrothermal method using the activated carbon (AC) as a carrier. e synthesis conditions were optimized by a single-factor experiment. e structural, textural, and surface properties of the adsorbent have been comprehensively characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier-transform infrared (FT-IR) spectroscopy, Brunauer-Emmett-Teller (BET) measurements, and X-ray photoelectron spectroscopy (XPS) analysis. e SO 2 removal capacities of the composites were investigated via testing the adsorption capacity at the self-made desulfurization equipment. e results show that the adsorption capacity of ZnFe 2 O 4 /AC composites is much higher than that of the AC and ZnFe 2 O 4 samples, respectively. e composite overcomes the disadvantages of the traditional sintering, showing a very high desulfurization performance. e breakthrough time was 147 min, and the sulfur adsorption capacity could reach 23.67% in the desulfurization performance test.