Abstract: A new Mo-Sn catalyst prepared by hydrothermal method was used for the synthesis of dimethoxymethane (DMM) from methanol oxidation. The catalyst with low Mo content can achieve low-temperature oxidation of methanol to DMM with high selectivity. The influence of Mo content on the structure and the catalytic performance of the catalyst was investigated. It was found that Mo1Sn10 catalyst showed the best catalytic performance under the conditions of 140 °C and atmospheric pressure, the methanol conversion was 14.2%, and the selectivity of DMM reached 88.9% without the formation of CO_x during the reaction process. The catalysts were characterized by XRD, Raman, FT-IR, XPS, NH₃-TPD and H₂-TPR. The results showed that the catalysts with different Mo content had obvious differences in structure and performance. Lower Mo content was more conducive to the formation of Mo⁵⁺ and MoO_x, and the resulting changes in acidity and redox properties were the important reasons for the excellent performance of the catalysts.