1.microporous and Mesoporous Materials 131 (2010) 170-176-2-2

Author's personal copy
Microporous and Mesoporous Materials 131 (2010) 170–176
Contents lists available at ScienceDirect
Microporous and Mesoporous Materials

journal homepage: www.elsevier.com/locate/micromeso
In-situ preparation of heteropolytungstic acid on TiMCM-41 nanoporous

framework for photocatalytic degradation of textile dye methyl orange
N. Pugazhenthiran, S. Ramkumar, P. Sathish Kumar, S. Anandan *
Nanomaterials and Solar Energy Conversion Lab, Department of Chemistry, National Institute of Technology, Trichy 620 015, India
a r t i c l e i n f o a b s t r a c t
Article history: Encapsulation of heteropolytungstic acid (HPA) in the TiMCM-41 framework was carried out by an in-situ
Received 13 June 2009 synthesis method in order to improve the catalytic activity because it would provide an effective environ-
Received in revised form 20 August 2009 ment for increasing the number of active surface sites for molecular interaction. Fourier transform infra-
Accepted 16 December 2009
red analysis (FT-IR), 31P NMR analysis, X-ray diffraction (XRD) analysis, adsorption studies, diffused
Available online 24 December 2009
reflectance studies (DRS) and transmission electron microscopy (TEM) studies were employed to charac-
terize the structure and morphology of as synthesized nanoporous materials. The observed 31P NMR peak
Keywords:
at 14.158 ppm indicates unambiguously that the Keggin structure is retained upon in-situ synthesis of
HPA encapsulated TiMCM-41
Nanoporous surfaces
HPA in MCM-41 nanochannels. No obvious extra phases of HPA are seen outside the nanoporous struc-
Methyl orange ture from TEM image confirming that HPA is formed only in the nanoporous framework and there is no
Electron acceptor possibility for leaching out HPA from the nanopores. The modified high surface inorganic substrate was
Photocatalytic degradation chosen as a simple model for the study of reactions involving the much complex commercial products
used for the dyeing of textile fibers. Possibilities to enhance the catalyst performance further by using
electron acceptors are also discussed.
Ó 2009 Elsevier Inc. All rights reserved.
1. Introduction dent from many publications in this area over the last two decades
[12–14]. However, there are certain limitations of using bare TiO2
Synthetic dyes are extensively used in many fields of up to date in photocatalytic reactors, i.e., (i) TiO2 being small size (about
technology, for example, in textile industry, leather tanning indus- 4–30 nm), get itself aggregates rapidly in a suspension loosing its
try, paper production, food technology, etc. [1–10]. Unfortunately, effective surface area as well as the catalytic efficiency and (ii)
the exact amount of dyes produced in the World and exact data on TiO2 being non-porous exhibits low adsorption ability for the pol-
the quantity of dyes discharged to the environment are also not lutants [15], especially for the non-polar organic compounds due
available. Due to large scale production and extensive application, to its polar surface [16,17]. Hence, for photocatalytic decomposi-
synthetic dyes can cause considerable environmental pollution and tion of any target compound, adsorption of it on the TiO2 surface
are serious health-risk factors. A wide range of methods has been is essential prior to the surface reaction. This made many research-
developed for the removal of synthetic dyes from waters and ers to support fine TiO2 on porous adsorbent materials like silica,
wastewaters to decrease their impact on the environment. That alumina, activated carbon, clay, zeolites, MCM-41, etc. in order to
is, the technologies involve adsorption on inorganic or organic attain high specific surface area and also facilitates more effective
matrices, decolorization by photocatalysis, and/or by oxidation adsorption sites than bare TiO2 [15,17–30]. In addition, enhanced
processes, microbiological or enzymatic decomposition etc. [11]. decomposition rate are attributed to the increased condensation
The efficacy of the various methods of dye removal, such as chem- of organic substrates on the supported catalyst by adsorption and
ical precipitation, chemical oxidation, adsorption, along with their the reduced electron–hole recombination process on the surface.
effects on subsequent biological treatment was compared [2]. In order to meet the requirements of future environmental and
Advanced oxidation processes (AOPs) are the effective remedia- energy technologies, new and more efficient materials need to be
tion and treatment methods due to their ability of complete degra- explored and hence we proposed here specific inorganic supported
dation of wide variety of organic pollutants and microbial nanoporous material (i.e., heteropolytungstic acid encapsulated
substances. TiO2 induced photocatalysis is an established AOP for TiMCM-41) for removal of organic pollutants released from textile
the treatment of contaminated air and water streams, which is evi- industries (methyl orange). The reason for choosing heteropolyacid
is that inorganic supports have been preferentially applied in
adsorption studies due to their good mechanical and chemical sta-
* Corresponding author. Tel.: +91 431 2503639; fax: +91 431 2500133.
E-mail addresses: [email protected], [email protected] (S. Anandan). bility, high specific surface area and resistance to microbiological
1387-1811/$ - see front matter Ó 2009 Elsevier Inc. All rights reserved.
doi:10.1016/j.micromeso.2009.12.017

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Microporous and Mesoporous Materials 131 (2010) 170–176

Contents lists available at ScienceDirect

Microporous and Mesoporous Materials

In-situ preparation of heteropolytungstic acid on TiMCM-41 nanoporous

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