Preparation and Investigation of Thermolysis of l-Aspartic Acid-Intercalated Layered Double Hydroxide

l -Aspartic acid ( l -Asp) has been intercalated into magnesium−aluminum layered double hydroxides by coprecipitation. The structure and composition of the intercalated material have been studied by X-ray diffraction, inductively coupled plasma emission spectroscopy, and elemental analysis. A schematic model of the intercalated structure has been proposed. Furthermore, the thermal decomposition of the hybrid material has been characterized by in situ powder X-ray diffraction, in situ Fourier transform infrared spectroscopy, thermogravimetry, differential thermal analysis, 13 C solid-state magic-angle spinning nuclear magnetic resonance, temperature-programmed decomposition, and gas chromatography−mass spectrometry. The thermolysis of l -Asp LDH is quite different from that of the pristine l -Asp studied as a reference sample and is characterized by three steps: the first from room temperature to 150 °C is attributed to the loss of both adsorbed and interlayer water, accompanied by the destruction of the hydrogen bonding network and a decrease in basal spacing; the second step (250∼350 °C) involves the polymerization and deamination of l -Asp ions in the interlayer of LDH and dehydroxylation of the brucite-like layers; the third step in the temperature region of 350∼450 °C corresponds to dehydroxylation of the brucite-like layers as well as further decomposition of interlayer materials.