Using Mg(NO3)2?6H2O as the magnesium source and Al(NO3)3?9H2O as the aluminum source, a highly dispersed magnesium-aluminum layered double hydroxide MgAl-LDH was prepared by hydrothermal method and calcined to generate MgAl-LDO. The product was characterized and analyzed by Field emission scanning electron microscope (FE-SEM), X-ray diffraction (XRD), transmission electron microscope (TEM), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron analysis (XPS), nitrogen adsorption-desorption method, and its adsorption mechanism was discussed. The results show that the adsorption process of the two products is basically the same as the Langmuir adsorption model. Among them, the specific surface area of MgAl-LDO is larger and the adsorption performance is better. The maximum adsorption capacity of methyl orange can reach 925.9 mg?g-1. Adsorption mechanisms include chemical interaction, hydrogen bonding, electrostatic interaction, and surface complexation.