A facile one-pot hydrothermal process to synthesize sulfonated mesoporous ZrO2

Sulfonated mesoporous ZrO 2 was prepared by a facile one-pot hydrothermal process, using a mixture of ZrOCl 2 ·8H 2 O and sodium dodecyl sulfonate in a NaOH solution, and subsequent calcination of the inorganic/organic intermediate. The influence of NaOH concentration, hydrothermal and calcination temperature on the structural and textural properties of the final products was investigated. Increasing the NaOH concentration gave rise to the transformation from tetragonal to monoclinic and then to tetragonal phase, whereas the increase of hydrothermal temperature led to the tetragonal-to-monoclinic phase transformation. As the NaOH concentration and hydrothermal temperature were increased, a narrow pore size distribution was turned into a multi-modal pore size distribution resulting from regular mesopores and interparticle voids. Accordingly, the incorporated sulfonate anions were oxidized into sulphate anions. After the calcination of 550 °C, the sulfonated products possessed tetragonal crystalline phase with average pore diameter of 4.2 nm and surface area of 108 m 2 g −1 .