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® Z1200 from Sigma‐Aldrich) such as a higher surface area, consisting of not only micropores like Basolite® Z1200 but also subordinate mesopores, formed by an assembly of nano‐ZIF‐8 crystals, which was 30 nm. Specifically, for the first time, nano‐ZIF‐8 was prepared in methanol with the yield of 61.2 %.