Textural and Structural Properties of Mesoporous Silica Synthesized Under Refluxing Conditions

Abstract

Mesoporous silica with pore sizes of 3–6 nm has been synthesized under refluxing and autogenous pressure conditions of hydrothermal synthesis from precursor gels having different alkaline pH. The mesoporous silica prepared is characterized by powder X-ray diffraction, nitrogen adsorption-desorption measurement and scanning electron microscopy. Thermal stability has been tested by XRD analysis of mesoporous silica after thermal treatment at 823 K, 6 h; 1023 K, 1 h and 1223 K, 1 h. The results indicate that the mesoporous silica prepared under refluxing condition from precursor gel of pH 11 has large surface area (ca.1103 m2 g− 1) and pore volume (ca. 0.868 cm3 g− 1) and is thermally stable at 1223 K. The surface area, pore volumes and pore wall thickness increase as the pH of the precursor gel is increased for refluxing condition of synthesis. The comparison of textural properties revealed that the refluxing condition is advantageous over autogenous pressure condition for obtaining mesoporous silica with higher surface area (852 m2 g− 1), pore volume (0.894 cm3 g− 1) and pore diameter > 4 nm with wall thickness of 1.59 nm, when synthesized from precursor gel of pH 9.2. The 29Si NMR spectra showed that a great part of the Si atoms exists as silanol groups. The mesoporous silica made at the lower pH (9.2) under refluxing conditions have more condensed framework. In calcined mesoporous silica, the proportion of partly condensed silica (Q3) is higher than fully condensed silica (Q4).