Titanium phosphate containing long chain surfactants can be synthesized either by batch using the inorganic ion-exchanger gamma-titanium phosphate and surfactant solutions or via sol-gel by direct intercalation. The resulting content of the surfactants after being exchanged depends on the length of the chain and is greater in the case of the material obtained by direct intercalation. All of the material obtained has a layered structure and an increased interlayer distance. The longer the chain is the greater the increase in distance. The layered structure is maintained up to 300 degrees C. The pyrophosphate formation occurs at 900 degrees C in the case of material by direct intercalation, whereas in the case of batch material it occurs at a higher temperature. The surfactant loss occurs in three or more distinct stages. As far as the batch material is concerned the last loss occurs at a high temperature of similar to 800 degrees C. Thermal treatment is carried out in air or nitrogen atmosphere for the better characterization of the processes. (c) 2006 Elsevier Ltd. All rights reserved.