Abstract: A Cu-Al-hydrotalcite-like compound (Cu-Al-HTLc) was assembled via Glycerol-Hydrothermal technique using CuSO4?5H2O, AlCl3?6H2O and Na2CO3 as raw material. A Cu-Al-HTLc with a well-defined shape, distinct intercalated structure, regular quality, and good dispersing capability could be obtained under the following conditions: verdigris was obtained firstly, a hydrothermal reaction started when combining the verdigris and AlCl3?6H2O solution. The influence of different conditions on the characteristics of the sample was investigated in this paper. Hydrotalcite samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller N2 surface area measurements.