Materials Chemistry and Physics, Vol.113, No.2-3, 773-779, 2009
Facile synthesis and morphology control of zeolite MCM-22 via a two-step sol-gel route with tetraethyl orthosilicate as silica source
MCM-22 zeolite was synthesized via a two-step sol-gel route (low pH sol-gel reaction followed by high pH crystallization) under static hydrothermal conditions using tetraethyl orthosilicate (TEOS) as silica source. Various parameters that significantly influence the synthesis results during both the hydrolysis reaction of TEOS in acid media and the hydrothermal reaction in base media were investigated in detail. The produced samples were characterized by XRD, ICP, and SEM techniques. It is found that pure MCM-22 with high crystallinity can be obtained via the novel two-step sol-gel route in a broad window of reaction conditions. The increase of temperature and pH value for the hydrolysis of TEOS favors the shortening of crystallization time and decreasing of MCM-22 particle size. Moreover, by adjusting the hydrothermal reaction parameters, such as increasing the crystallization temperature, increasing the alkalinity of the synthesis gel mixture, and decreasing the SiO2/Al2O3 ratio, the crystallization is accelerated substantially. Also, rose-like or lamellar-like morphologies of MCM-22 particles with different sizes can be achieved by changing these reaction parameters. Using this two-step sol-gel route, MCM-22 is able to be well produced in a wide range of the SiO2/Al2O3 ratio from 20 to 100. (C) 2008 Elsevier B.V. All rights reserved.