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A metal-free covalent triazine framework (CTF) was synthesized from 2,4,6-tricyano-1,3,5-triazine (TCT) through open-system and liquid-phase synthesis using trifluoromethanesulfonic acid as both a catalyst and a solvent (TCT-CTF). In conventional closed-system methods, metal ions used as catalysts remained even after purification, and large quantities could not be synthesized. The proposed method solved these problems and synthesized higher-quality TCT-CTF with a layered structure and a composition with a C/N ratio of 1, which is close to the ideal value.