Abstract: The Ni/SiO₂ catalysts were prepared by ammonia evaporation method, with nickel nitrate as Ni source and silica sol as the SiO₂ source, for synthesis of 2-MTHF from 2-MF hydrogenation. The catalytic performance of catalysts prepared at different calcination temperatures were tested on a fixed-bed reactor. XRD, N₂ adsorption-desorption, H₂-TPR, NH₃-TPD, XPS and TG were employed to characterize the structure and surface properties of these catalysts. The effect of calcination temperature on the structure, surface property and catalytic performance of catalysts were investigated. The result indicated that all the catalysts had a phyllosilicate structure after calcination, and maintained the structure after reduction. Ni particles dispersed well with smaller size and strong metal support interaction showed high activity. The surface acidity of catalysts was influenced by the calcination temperature. The maximum catalytic activity and selectivity were obtained on the catalyst calcined by at 500 ℃, which exhibited a 2-MF conversion of 100% and the 2-MTHF selectivity of 93.5% at the optimized condition, due to smaller particle size and suitable surface acidity.