In this study, the hydrothermal method was used to synthesize MIL-101(Cr), and activated carbon (AC) with different content was incorporated in to MIL-101(Cr), thereby obtaining AC-MIL-101(Cr) composite material with a huge specific surface area. The physical properties of MIL-101(Cr) and AC-MIL-101(Cr) were characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), nitrogen adsorption and desorption and specific surface area testing, and ethanol vapor adsorption performance testing. The results show that with the increase of activated carbon content, the thermal stability of AC-MIL-101(Cr) is improved. Compared with the pure sample, the BET specific surface area and pore volume of AC-MIL-101(Cr) have increased. In the relative pressure range of 0–0.4, the saturated adsorption capacity of AC-MIL-101(Cr) to ethanol vapor decreases slightly. It is lower than MIL-101(Cr), but its adsorption rate is improved. Therefore, AC-MIL-101(Cr)/ethanol vapor has a good application prospect in adsorption refrigeration systems. The exploration of AC-MIL-101(Cr) composite materials in this paper provides a reference for the future application of carbon-based/MOFS composite adsorbent/ethanol vapor working fluid in adsorption refrigeration.