Vol.:(0123456789) 1 3
Journal of Porous Materials
https://doi.org/10.1007/s10934-019-00803-0
Iron oxide impregnated mesoporous MCM‑41: synthesis,
characterization and adsorption studies
Jyoti Prakash Dhal
1,2
· Tapan Dash
3
· Garudadhwaj Hota
2
© Springer Science+Business Media, LLC, part of Springer Nature 2019
Abstract
Mesoporous MCM-41 and MCM-41 impregnated with structural iron (Fe–MCM-41) were prepared by a facile surfactant
based wet chemical method using tetraethyl orthosilicate, cetyl trimethyl ammonium bromide in the presence of ammonium
hydroxide and FeSO
4
·7H
2
O as impregnated reagent. The prepared mesoporous materials were characterized by small and
wide angle X-ray difraction (XRD), XPS, FESEM, HRTEM, FTIR and N
2
gas adsorption/desorption isotherm techniques.
The results indicate the formation of high surface area (1266 m
2
/g) porous structure with particle size in the range of
200–400 nm for MCM-41. In case of Fe–MCM-41 the surface area decreases (880 m
2
/g) substantially with formation of
iron oxide nanoparticles in the frame work of MCM-41. The obtained mesoporous materials were used as adsorbents for the
removal of methylene blue from aqueous media. The percentage removal of the dye was found to be 99.9% for Fe–MCM-
41 and 94.5% for MCM-41, respectively, by using 20 mL of dye solution with initial concentration of 100 mg/L and 0.05 g
of each adsorbent. The maximum adsorption capacity of Fe–MCM-41 was found to be 194 mg/g and for MCM-41, it was
149.5 mg/g. This result suggests that the prepared Fe–MCM-41 is an efective adsorbent for decontamination of Methylene
blue from aqueous media.
Keywords Mesoporous materials · MCM-41 · Fe–MCM-41 · Adsorption · Methylene blue
1 Introduction
Mesoporous materials such as MCM-41, MCM-48, and
SBAs have been the subject of intensive research in the feld
of adsorption and heterogeneous catalysis because of their
high surface area, high pore volume, favorable and control-
lable pore uniformity, high hydrophobicity and relatively
high thermal stability [1–3]. MCM-41 (Mobil composite
material number 41, frst discovered in 1992) consists of
hexagonal array of uniformly sized one-dimensional pore
geometry with a pore diameter of 2 to 10 nm [4]. Due to its
excellent removal capacity, mesoporous MCM-41 has been
used for adsorption of various contaminants from aqueous
media. For the improvement of the adsorption capacity and
selectivity of adsorption, modifcation of MCM-41 is very
helpful [5]. Particularly, incorporation of heteroatoms such
as Fe, Al, Cr and so on into the primarily inert frameworks
make the structure more potential for the application in
the feld of catalysis and adsorption [6, 7]. Due to its high
surface area of around 1000 m
2
/g, porosity and amorphous
structure, there is a possibility of impregnation of transition
metal ion inside the mesoporous framework by substitution
of Si atoms in regular tetrahedral positions [8, 9].
Amongst the various heteroatoms, iron atom incorporated
into the silica framework results the generation of strong
acid sites; as a result Fe-containing mesoporous silicates
have shown improved performance towards catalytic activ-
ity and adsorption. Very recently several attempts have
been made in which iron-containing mesoporous materials
MCM-41(Fe
3+
) have been extensively studied because of
its considerable interest for various applications, especially
* Jyoti Prakash Dhal
jyoti84.chem@gmail.com
* Garudadhwaj Hota
garud@nitrkl.ac.in
1
Department of Chemistry, College of Engineering
and Technology (A Constituent and Autonomous College
of Biju Patnaik University of Technology, Orissa),
Bhubaneswar, India
2
Department of Chemistry, National Institute of Technology,
Rourkela, Odisha 769008, India
3
Centurion University of Technology and Management,
Odisha, India