A series of iron and manganese mixed oxide pillared clay with varying manganese to iron ratio has been successfully synthesized. Prepared materials were characterized by low angle XRD, TG/DTA, hydrogen TPR and nitrogen adsorption desorption experiment. All the materials were found to be thermally stable up to 500°C having basal spacing ≥16.5Ǻ. Surface area and pore volume increases with the increase in the metal uptake irrespective of manganese to iron ratio. Catalytic decomposition of acetone and trichloroethylene was studied to find out the suitability of the material for VOC decomposition reaction. Catalyst (S-16/4) having high manganese content acts as better catalyst for the acetone decomposition reaction. Time on stream experiment justifies the stability of the prepared catalyst at least for 20h with minor change in the activity. However, in case of trichloroethylene (TCE) decomposition catalyst (S-8/12) with higher iron content shows better activity. Quick deactivation of the catalyst for TCE decomposition is noticed for all the prepared materials.