A novel synthesis of Mg-Al-CO3 layered double hydroxide (LDH) through chemical precipitation and hydrothermal methods has been investigated in this paper. The advantages of this method are using magnesite as magnesium source and no CO2 released in the process of preparation. Mg-Al-CO3 LDH (ZY) prepared under the optimized condition (the molar ratio of magnesite and Al(NO3)(3 center dot)9H(2)O was 2.5:1; the aging time and temperature were 16 h and 100 degrees C, respectively) was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), thermo-gravimetric and differential thermal analyser (TG-DTA) and scanning electron microscope (SEM). The crystal morphology of the prepared LDH displays platelet-like structure with a hexagonal shape, which is agreed with the LDH produced by industrial chemicals. Through elemental analysis and inductively coupled plasma-atomic emission spectrometry (ICP-AES), the chemical formula of ZY is determined as Mg0.70Al0.35(OH)(2)(CO3)(0.15)center dot 0.6H(2)O. (C) 2012 Elsevier Ltd. All rights reserved.