Sodium-cerium molybdate - NaCe(MoO4)2 - crystals were synthesized by the conventional hydrothermal method at 150 °C without using organic additives or surfactants. This material was characterized by X-ray diffraction (XRD), Raman and Fourier-transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), UV–vis diffuse reflectance and zeta potential. The XRD pattern showed that the NaCe(MoO4)2 crystallizes in a scheelite-type tetragonal structure without secondary phases, as well as Raman and FT-IR spectroscopy confirm the formation of the NaCe(MoO4)2 tetragonal. SEM images show that the obtained samples have a truncated octahedral morphology with an average side length of ∼1.2 μm and high uniformity. The removal and degradation of Remazol Brilliant Blue (RB) and Methylene Blue (MB) dyes under visible light irradiation were analyzed, showing that the NaCe(MoO4)2 microcrystals exhibit favorable performance for the removal and/or degradation of these dyes, especially in the MB case.