A rare earth metal-organic framework Yb-BTC was prepared from Yb(NO3)3•5H2O and 1,3,5-benzenetricarboxylic acid (H3BTC) by the solvothermal method and characterized through X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 absorption-desorption isotherm (BET) and Fourier transform infrared spectroscopy (FTIR). The results showed that Yb-BTC was a typical microporous material with specific surface area of 560 m2/g and pore size of 1.84 nm, and Yb-BTC had uniform particle size, its size was about 2 μm. The activity of Yb-BTC for preparation of polycarnonate diol (PCDL) via the transesterification between diphenyl carbonate (DPC) and 1,5-pentanediol (PDO) was investigated, and was compared with those of catalysts reported such as triethylamine, zinc acetate, tetra-n-butyl titanate and titanium oxide bis(2,4-pentanedionate). The results exhibited that the catalytic activity of Yb-BTC was equivalent to that of titanium catalyst. When the molar ratio of PDO to DPC was 1.2, the amount of Yb-BTC was 0.05% ( the amount accounting for mass percent of DPC), the time of atmospheric transesterification at 180~185 ℃ was 2 h, the time of vacuum polycondensation at 160 ℃ was 4 h, and PCDL with the number-average relative molecular mass of 2300 g/mol and the hydroxyl value of 49.3 mg KOH/g were obtained.