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In this study, a new process to synthesize Calgary framework 20 (CALF-20), a zinc-based metal-organic framework (MOF), in a H 2 O/methanol solution was developed, exhibiting a high CO 2 adsorption capacity. Generally, CALF-20 was synthesized by a solvothermal method, requiring the consumption of considerable thermal energy. On the other hand, the proposed synthetic process required only 6 min to crystallize CALF-20 in a H 2 O/methanol mixed solution at room temperature (298 K) and normal pressure (101.3 kPa). In addition, CALF-20 was obtained in 93.3 % yield using zinc and oxalate sources under an aging time of 120 min. As-synthesized CALF-20 exhibited a Brunauer–Emmett–Teller surface area of 520 m2 g−1, a micropore volume of 0.19 cm3 g−1, a CO 2 uptake of 3.84 mmol g−1 at 298 K, and a P CO 2 of 100 kPa; these values were similar to those obtained for CALF-20 synthesized by the solvothermal method using high thermal energy. Furthermore, CALF-20 was crystallized without washing using H 2 O. The key factor for the crystallization of the CALF-20 structure in this process was the deprotonation of 1,2,4-triazole, which was caused by the acetate anion derived from zinc acetate as the starting metal source. [Display omitted] • Calgary framework 20 (CALF-20) was successfully synthesized in methanol aqueous solution under room temperature and normal pressure. • The fabrication of CALF-20 structure started after 6 min from the beginning of aging process. • Acetic ion derived from zinc acetate played a role in the deprotonation of 1,2,4-triazole. • CALF-20 structure was fabricated without activation process with solvents. • The micropores for gas adsorption were produced due to the Zn-oxalate-1,2,4-triazole three-dimensional networks. [ABSTRACT FROM AUTHOR]