For the homogeneous precipitation of hydrotalcite-like compounds (layered double hydroxides; LDHs), HMT (hexamethylenetetramine) was used and the conditions for obtaining the LDHs were investigated. The well-crystallized 1-5 mum LDHs were obtained in a pressure vessel after a 1-day treatment at 140 degreesC. The resulting LDHs contained a carbonate anion, which was successfully deintercalated using an NaCl-HCI mixed solution without any morphological change.