The zirconium phosphate α-Zr(HPO4)2·H2O (α-ZrP) with layered structure has been synthesized by refluxing method. Power X-ray diffraction (XRD), vibrational spectroscopy (FT-IR, FT-Raman), thermal analysis (TG-DSC), transition electron spectroscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometer (EDS) was respectively used for structure characterization of the compound α-ZrP. The result of intercalation reactions with tetramethylammonium bromide and cetyltrimethylammonium bromide showed interlayer distances increase of ~ 0.46 nm and ~ 1.68 nm, respectively. The BET surface area of α-ZrP is 12.29 m2·g-1. The cyclic voltammetry behaviors of the compound on Au electrode showed a typical reversible process. Moreover, the strong fluorescent property of the α-ZrP was measured. The maximum emission peaks occurred at ca. 390 nm upon excitation at ca. 288 nm.