| Summary: | The application of hybrid photocatalysts made of carbon nitride and lead-free perovskites, namely DMASnBr<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> and PEA<sub>2</sub>SnBr<sub>4</sub>/g-C<sub>3</sub>N<sub>4</sub>, for the H<sub>2</sub> evolution from saccharides aqueous solution is described. The novel composites were tested and compared in terms of hydrogen evolution rate (HER) under simulated solar light, using Pt as a reference co-catalyst, and glucose as a representative sacrificial biomass. The conditions were optimized to maximize H<sub>2</sub> generation by a design of experiments involving catalyst amount, glucose concentration and Pt loading. For both materials, such parameters affected significantly H<sub>2</sub> photogeneration, with the best performance observed using 0.5 g L<sup>−1</sup> catalyst, 0.2 M glucose and 0.5 wt% Pt. Under optimized conditions, DMASnBr<sub>3</sub>/g-C<sub>3</sub>N<sub>4</sub> showed a 5-fold higher HER compared to PEA<sub>2</sub>SnBr<sub>4</sub>/g-C<sub>3</sub>N<sub>4</sub>, i.e., 925 µmoles g<sup>−1</sup> h<sup>−1</sup> and 190 µmoles g<sup>−1</sup> h<sup>−1</sup>, respectively (RSD ≤ 11%, <i>n</i> = 4). The former composite, which affords an HER 15-fold higher in aqueous glucose than in neat water, provided H<sub>2</sub> also with no metal co-catalyst (around 140 µmoles g<sup>−1</sup> h<sup>−1</sup>), and it was reusable for at least three photoreactions. Encouraging results were also collected by explorative tests on raw starch solution (around 150 µmoles g<sup>−1</sup> h<sup>−1</sup>).
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