In the present work, zinc titanates (ZTO) as photocatalysts were synthesized, characterized, and evaluated aiming to study their photocatalytic properties for hydrogen production under visible-light irradiation and employing MeOH (methanol) and TEOA (Triethanolamine) as sacrificial agents. ZTO were synthesized by modified Pechini method. Characterization of materials consisted in TGA, XRD, TEM, EELS, BET, and UV–Vis. Surface interaction studies consisted of FT-IR spectroscopy and determination of MeOH and TEOA adsorption–desorption capacities on the ZTO by TGA. Zinc titanates were evaluated as photocatalyst for H₂ production using an artificial visible light and monitored by GC. TGA results led to establish calcination temperatures of 550 °C (Zn₂Ti₃O₈) and 700 °C (ZnTiO₃) to reach their crystalline phases. XRD analysis of sample cds-ZTO found cubic Zn₂Ti₃O₈ and traces of the ZnO crystalline phase, while p-ZTO exhibited a mixture of cubic and hexagonal ZnTiO₃ crystalline phases. Surface area for cds-ZTO was 88 m²/g, while ZnTiO₃ had 13 m²/g. Photocatalytic H₂ production for cds-ZTO and p-ZTO using TEOA as sacrificial agent showed the highest photocatalytic activities generating 548 and 441 µmolH₂/h.g_cat. TEOA adsorption–desorption capacity was found superior on cds-ZTO and p-ZTO than that for MeOH on both samples.