The organic-inorganic layered compound zinc hydroxide-benzoic acid with basal spacing of 1.92 nm was synthesized hydrothermally using amorphous Zn(OH)2 and benzoic acid at the reaction temperature of 90~130 ℃, the molar ratio of C6H5COOH/Zn(Containing 6 mmol of Zn) of 0.4~0.6, 20 mL H2O and the reaction time of 6 h. The character, structure, particle morphology and chemical composition of the layered compound were characterized by means of XRD, TG-DTA, SEM, TEM and elemental analysis. The results indicate that the layered compound is of plate-like morphology and that with the temperature raising of hydrothermal synthesis, the particle of plate-like piece becomes smaller. The chemical formula of the layered compound could be written as Zn(OH)2-y·(C6H5COO)y·0.3H2O, 0.36≤y≤0.54.