| Summary: | Two-dimensional graphitic carbon nitrides (2D g-C<sub>3</sub>N<sub>4</sub>) are promising photocatalysts for water splitting to hydrogen due to their non-toxicity and high stability. However, the bulk g-C<sub>3</sub>N<sub>4</sub> has some intrinsic drawbacks, such as rapid electron–hole recombination and low charge-carrier mobility, resulting in poor photocatalytic activity. Here, 2,4-diamine-6-phenyl-1,3,5-triazine was employed as a precursor to regulating the assembly of melamine and cyanuric acid in water. The resulting g-C<sub>3</sub>N<sub>4</sub> not only improved the visible light absorption and electron–hole separation but also provided more catalytic sites for enhanced photocatalytic hydrogen evolution. The modified g-C<sub>3</sub>N<sub>4</sub> (CNP10-H) showed a hydrogen-releasing rate of 2184 μmol·g<sup>−1</sup>·h<sup>−1</sup>, much higher than the bulk g-C<sub>3</sub>N<sub>4</sub>.
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