Changes in the Surface Area of Silica-supported 12-Molybdophosphoric Acid in Relation to the Degree of Loading and the Calcination Temperature

Abstract

A technical silica gel (Grace-113) was impregnated with 12-molybdophosphoric solution to attain loadings of 0.72–13.4 wt.%. The air-dried solids were then calcined for 3 h at 400, 600 and 800°C, respectively, followed by determination of their N2 adsorption isotherms. The silica gel was thermally stable and suffered about 15% loss in area at 800°C. The impregnated silicas showed considerable decrease in surface area as a function of their heteropoly acid content. Two processes are suggested as taking part in the modification of pore structure: (1) diffusion of the aqueous heteropoly acid solution and its subsequent deposition; and (2) dissolution of silica gel in the acidic aqueous solution followed by interaction with HPMo to form either molybdosilicate or P–Si exchange products. Correlation with the previously studied catalytic conversion of isopropanol indicated that the activity was independent of the surface area. Catalytic dehydration on the 600°C and 800°C products seems to be associated with silicate, molybdate or MoO3 surface species rather than being due to surface acidity or the extent of the surface area.