A series of trinuclear acetato complex of Fe(Ill) intercalated TiP was successfully prepared by ion exchange process by varying the wt% of Fe(Ill), activated at various temperatures and characterized by various techniques. The PXRD and FTIR analyses reveal that the pillaring has been taken place in the interlayer of the layered materials. All the catalysts were found to be mesoporous in nature. The number of reducing sites was found to be higher than that of oxidizing sites. With increase in the calcination temperature of 5 wt% Fe(III)/TiP, surface area and surface oxygen increase up to 300 degrees C, thereafter exhibits a slow decrease up to 500 degrees C. But the oxidizing and reducing properties go on decreasing with activation temperature. Catalytic decomposition of acetone, methanol, diethyl ether and 2-propanol as probe molecules was studied to find out the suitability of the material for VOCs decomposition reactions. Fe(Ill) pillared TiP (5 wt%) with high iron content, surface area and surface oxygen shows higher catalytic activity towards the complete decomposition of VOCs. Titanium phosphate pillared with 5 wt% Fe(III), calcined at 300 degrees C showed complete decomposition of VOCs in the range of 180-350 degrees C. The catalytic activity of these materials is comparable with other reported catalysts. (c) 2007 Elsevier B.V. All rights reserved.