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Preparation of mesoporous titanosilicate molecular sieves with a cage type 3D porous structure for cyclohexene epoxidation
Journal article   Peer reviewed

Preparation of mesoporous titanosilicate molecular sieves with a cage type 3D porous structure for cyclohexene epoxidation

C Anand, P Srinivasu, G P Mane, S N Talapaneni, D S Dhawale, Mohammad A Wahab, S V Priya, S Varghese, Y Sugi and A Vinu
Microporous and Mesoporous Materials, Vol.160, pp.159-166
2012
DOI: https://doi.org/10.1016/j.micromeso.2012.05.014
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https://doi.org/10.1016/j.micromeso.2012.05.014View
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Abstract

mesoporous nanoporous catalysis zeolite epoxidation
We report on the preparation of mesoporous titanosilicate with a 3D porous structure and Fm3m symmetry using Pluronic F127 as structure directing agent and titanium isopropoxide as a titanium source. The amount of titanium in the silica framework of the materials is controlled by a simple adjustment of the molar water to hydrochloric acid (nH2O/nHCl) ratio. The materials with different nSi/nTi ratios are also prepared by varying the amount of titanium source in the synthesis gel at an optimized nH2O/nHCl of 463. The structural order, the textural parameters, morphology, the nature and co-ordination of Ti species, and the amount of Ti content in the samples are analyzed by various techniques including X-ray diffraction (XRD), N2 adsorption, high resolution scanning electron microscopy (HRSEM), UV-vis diffused reflectance spectroscopy (UV-vis DRS), and inductively coupled plasma emission spectroscopy (ICP), respectively. All the materials prepared with various nSi/nTi ratios exhibit well-ordered porous structure and possess high BET surface areas (673-941 m2 g-1) and large pore volumes (0.46-0.71 cm 3 g-1). The pore diameter of the samples also increases with increasing the Ti content in the samples. UV-vis results confirm that most of the Ti atoms are in the tetrahedral co-ordination. Finally, the materials are subjected to cyclohexene epoxidation using TBHP/H2O2 as oxidant and acetonitrile as solvent in order to investigate their catalytic activity. Ti-KIT-5 samples display a high catalytic activity with TBHP as oxidant and remain inactive when H2O2 was used. The amount of Ti plays a crucial role in controlling the catalytic activity of the samples. Of the catalysts studied, Ti-KIT-5(5) where the number in the parenthesis indicates the Si/Ti ratio shows the best activity, affording a high conversion to cyclohexene. Among the catalysts studied, Ti-KIT-5-5 exhibited better catalytic activity with respect to reaction time, reaction temperature, conversion and epoxide selectivity. © 2012 Elsevier Inc. All rights reserved.

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