This article systematically presented analysis results of factors affecting the preparation of nano-ZIF-8 in methanol for high yield. Samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET) adsorption, and thermogravimetry-differential thermal analysis (TG/DTA). Synthesized nano-ZIF-8 had advantages over commercial ZIF-8 (Basolite((R)) Z1200 from Sigma-Aldrich) such as a higher surface area, consisting of not only micropores like Basolite((R)) Z1200 but also subordinate mesopores, formed by an assembly of nano-ZIF-8 crystals, which was 30nm. Specifically, for the first time, nano-ZIF-8 was prepared in methanol with the yield of 61.2%.