We report a “delayed neutralization” process for the preparation of highly‐ordered aluminosilicate MCM‐41 molecular sieves with high thermal and hydrothermal stability, and sharp pore size distribution. However, the structural order and pore size are dependent on the carbon chain length. In the mixture surfactant systems, the pore size of the MCM‐41 materials could be fine‐tuned. The pore size can be extended from 2.5 to 4.5 nm by adding a suitable amount of hydrocarbons. The tubular morphology of the MCM‐41 material of 0.3 to 10 micrometers diameter, where the wall consists of coaxial cylindrical pores of nanometers MCM‐41, can be obtained by careful control of the surfactant‐water content and the rate of condensation of silica. An optimum condition for automatic synthesis of the hierarchical TWT structure has been accomplished. The addition of 1‐alkanols as cosurfactant would not only improve the order of the MCM‐41 hexagonal structure but also promote the formation of micrometer‐sized hierarchical materials, for example: tubules‐within‐tubule and uniform‐sized hollow spheres of diameter 5.0 ± 1.0 μm. However, the inside of the micron spheres has intricate structures possessing various topological genus ranks. The MCM‐41 is a good supporter for Molybdenum oxide catalysts. The rate of deactivation in the catalytic reaction of ethyl‐benzene dehydrogenation to styrene increases in the order: MT < MP < SiO2. The physically mixed samples have higher catalytic activity than impregnated ones.
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