Dicalcium phosphate dihydrate (DCPD) nanoparticles, also known as brushite, are considered an important bioceramic compound. In this study, brushite was prepared from Moroccan phosphogypsum (PG) using a new sol-gel method. A two-step technique undergoes the synthesis of brushite, the preparation of anhydrite from PG followed by adding phosphoric acid in the presence of sodium hydroxide. The morphology, the chemical composition, and the crystallites size were obtained using Scanning Electron Microscopy (SEM-EDAX), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR), respectively. According to the Debye-Scherrer equation, these characterization methods indicated that the synthesized brushite was highly pure according to the Ca/P ratio of 1.14 and an average crystallites size estimated at 66 nm. These results proved that the brushite was successfully synthesized from Moroccan phosphogypsum.