A new photocatalyst, few-layer MoS 2 grown in MgAl-LDH interlayers (MoS 2 /MgAl-LDH), was prepared by a facile two-step hydrothermal synthesis. The structural and photocatalytic properties of the obtained material were characterized by several techniques including powder X-ray diffraction (XRD), Raman spectroscopy, field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), photoluminescence spectroscopy (PL) and UV-vis absorption spectroscopy. The MoS 2 /MgAl-LDH composite showed excellent photocatalytic performance for methyl orange (MO) degradation at low concentrations (50 mg L À1 and 100 mg L À1 ). Furthermore, even for a MO solution concentration as high as 200 mg L À1 , this composite also presented high degradation efficiency (>84%) and mineralization efficiency (>73%) at 120 min. The results show that the MoS 2 /MgAl-LDH composite has great potential for application in wastewater treatment.