Layered hydroxide zinc benzoate compounds with structure of layered basic metal salt (LBMS) were prepared by a hydrothermal reaction in a temperature range of 110–180 °C. The structure, chemical composition, and exfoliation reaction in alcohol solvents of the layered compounds were investigated by using XRD, TG-DTA, SEM, and TEM. Two kinds of layered phases with a basal spacing of 1.93 and 1.47 nm were obtained by the hydrothermal reaction. The chemical formulas for the 1.93 and 1.47 nm layered phases can be written as Zn(OH)1.66(C6H5COO)0.34·0.24H2O and Zn(OH)1.14(C6H5COO)0.86, respectively. The 1.93 and 1.47 nm layered phases show plate-like and fibrous particle morphology, respectively. Both of the layered phases can be exfoliated in alcohol solvents. The exfoliated nanosheets of the 1.93 nm layered phase can be curled into the nanotubes of Zn(OH)2. Nanobelt-like and nanoflower-like particles of Zn(OH)2 were formed by exfoliating the 1.47 nm layered phase.
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