AbstractIn this study, metal organic framework/activated carbon catalysts (X–MOF/AC, where X=Sn or Cu) were synthesized using a facile method and used for the acetylene hydrochlorination reaction. The prepared catalysts were characterized using Fouriertransform infrared spectroscopy (FTIR), X‐ray diffraction analysis(XRD), nitrogen adsorption‐desorption analysis, thermo‐gravimetric analysis (TGA), acetylene temperature‐programmed desorption experiments (C2H2‐TPD), hydrogen temperature‐programmed reduction experiments (H2‐TPR), X‐ray photoelectron spectroscopy (XPS) and scanning electron microscopy‐energy dispersive spectroscopy (SEM‐EDS). Compared with Cu–MOF/AC, Sn‐MOF/AC behaved the highest acetylene conversion of 93.5% under the conditions of 200 °C and an acetylene gas space velocity of 30 h−1. Furthermore, XRD, TGA and SEM‐EDS results showed that Sn‐MOF and Cu–MOF possesse different morphology and thermalstability, respectively. Additionally, C2H2‐TPD and TGA results indicated that Sn‐MOF/AC displays the higher acetylene adsorption and the better anti‐coking ability as compare to Cu–MOF/AC.