A mechanochemical method is developed in preparing magnesium-aluminum-layered double hydroxides (MgAl-LDHs). This approach includes activation process and diffusion process. In order to verify the LDHs structure and study the reaction kinetics, X-ray diffraction (XRD) patterns, inductively coupled plasma(ICP) and physical adsorption instrument were characterized. The results show that activation time can change the surface of particles and affect the reaction grade. During the diffusion process, reaction time is the most important factor. The reaction energy (ΔQ) was calculated that is 6kJ/mol.