ZnS-Bipy hybrid photocatalysts were easily synthesized using microwave irradiation. Their structural, optical and morphological properties were characterized by FTIR spectroscopy, powder X-ray diffraction (PXRD), UV-vis spectroscopy, nitrogen physisorption, Scanning electron microscopy (SEM), X-Ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). These materials were tested as photocatalysts in the hydrogen evolution reaction (HER) using water as raw material and methanol as sacrificial molecule under UV light irradiation. The obtainment of an optimal material able to carry out this photocatalytic reaction was studied through the reaction time and finally an optimized ZnS-Bipy hybrid material with the suitable combination of crystalline, optical and textural features was obtained. This photocatalyst presented an optimal performace in the generation of H-2 (20,000 mu mol per gram of catalyst) and was perfectly active after 5 cycles of catalytic runs.