Synthesis and characterization of hierarchical titanium-containing silicas using different size templates

  • Aleksey Fedosov
  • Marina Fedosova
  • Irina Postnikova
  • Sergey Orekhov
  • Aleksey Gushchin
  • Denis Ryabinin
  • Ilya ChuzhaykinEmail author
Regular Article


The development of hierarchical catalytic heterogeneous catalytic systems with a controlled micro/mesopore ratio is an important issue in catalysis. The main purpose of the paper is to the establish influence of the size of the template molecule on the main characteristics of hierarchical titanium-containing silicas (H-TS). The H-TS were successfully synthesized by a bi-template method using tetrapropylammonium hydroxide (TPAG) as permanent template of MFI topology and tetramethylammonium bromide (TMAB), tetraethylammonium bromide (TEAB), tetrabutylammonium hydroxide (TBAG), dodecyltrimethylammonium bromide (DTMAB), cetyltrimethylammonium bromide (CTAB), didecyldimethylammonium chloride (DDAC), tetradecylbenzyldimethylammonium bromide (TBDAB) as variable structure-directing agent (SDA) of a different size. The structure and morphology were characterized by X-ray diffraction, a Fourier transform infrared spectroscopy, a Raman spectroscopy, a scanning electron microscopy and low-temperature nitrogen adsorption-desorption. The catalytic properties of the prepared titanium-containing micro-mesoporous silicas for hydroxylation of phenol with \(\hbox {H}_{2}\hbox {O}_{2}\) have been evaluated, and their activities have been compared with those of TS-1 with only micropores. The findings of the research illustrate that with an increase in the molecule volume of the structure-directing agent, there is a decrease in the proportion of the crystalline phase and in the degree of the inclusion of \(\hbox {Ti}^{4+}\) atoms in the structure of the zeolite material. Increase in the volume of the structure-directing agent leads to the decrease of the crystallinity of the samples and decrease in the specific surface area of the material and in the specific volume of micropores. The result of this research will be used to create a theoretical model of controlled micro-/mesoporous ratio in silicas and it may open new perspectives for their potential application in selective oxidation reactions involving large molecules.

Graphic Abstract

SYNOPSIS Synthesis and characterization of hierarchical titanium-containing silicas produced by a bi-template method are reported. The findings of the research illustrate that the size of the template influences the main textural properties of titanium-containing silicas.


Hierarchical silica titanium silicalite bi-template synthesis mixed templates 



The study was financially supported by The Ministry of Education and Science of the Russian Federation (State assignment No. 10.2326.2017/PP).

The SEM study was carried out on the equipment of the Collective Usage Center “New Materials and Resource-saving Technologies” (Lobachevsky State University of Nizhny Novgorod).

The Raman spectroscopy was carried out in the Laboratory of Functional Nanomaterials (Lobachevsky State University of Nizhny Novgorod).

Supplementary material

12039_2019_1652_MOESM1_ESM.pdf (1009 kb)
Supplementary material 1 (pdf 1008 KB)


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Copyright information

© Indian Academy of Sciences 2019

Authors and Affiliations

  • Aleksey Fedosov
    • 1
  • Marina Fedosova
    • 1
  • Irina Postnikova
    • 1
  • Sergey Orekhov
    • 1
  • Aleksey Gushchin
    • 2
  • Denis Ryabinin
    • 3
  • Ilya Chuzhaykin
    • 1
    • 2
    Email author
  1. 1.Nizhny Novgorod State Technical University n.a. R.E. AlekseevDzerzhinskRussia
  2. 2.Lobachevsky State University of Nizhny Novgorod, National Research UniversityNizhny NovgorodRussia
  3. 3.University of AlbertaEdmontonCanada

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