Talanta 83 (2011) 1482–1486
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Talanta
journal homepage: www.elsevier.com/locate/talanta
Synthesis of polypyrrole nanoparticles and its grafting with silica gel for selective
binding of chromium(VI)
P. Mondal, K. Roy, S.P. Bayen, P. Chowdhury
∗
Synthetic Polymer Laboratory, Department of Chemistry, Visva-Bharati Santiniketan 731235, India
article info
Article history:
Received 15 September 2010
Received in revised form
13 November 2010
Accepted 15 November 2010
Available online 23 November 2010
Keywords:
Cr(VI)
Polypyrrole nanoparticles
Functionalizing
Grafting
Metal ion binding
abstract
Polypyrrole nanoparticles of desired structure have been synthesized through simple micelle technique.
It is then grafted with functionalized silica gel to develop a novel organic–inorganic hybrid material.
The role of dimethyl dichloro silane (coupling agent) in grafting is demonstrated. The nanoparticles are
characterized by TEM, SEM and TGA. Grafting reactions are evaluated by spectral (FTIR) analysis and
chemical test. The Cr(VI) binding behavior of the composite is studied in various pH of the medium.
The selectivity in binding Cr(VI) is monitored. The metal ion adsorption capacity and surface area of the
material are found to be 38 mg/g and 235 m
2
/g, respectively.
© 2010 Elsevier B.V. All rights reserved.
1. Introduction
Inherent conducting polymers (polypyrrole, polyaniline and
polythiophene) have attracted a great deal of interest owing to
their remarkable properties, such as redox [1], acid–base [2], ion-
exchange [3] and chemical sensing [4] in addition to its high
conductivity [5]. Bulk polypyrrole is infusible, intractable and insol-
uble in common solvents due to partial cross-linking [6] through
hydrogen bonding. As a result the polymer has poor process abil-
ity and inferior mechanical properties [7]. Various approaches [8]
have been utilized to improve the process ability of polypyrrole
[9–11], including (i) chemical modification of polymer backbone;
(ii) copolymerization of appropriate functional co-monomers; (iii)
use of polymeric or surfactant-type doping anion; and (iv) prepa-
ration of stable colloidal dispersion. Formation of later through
hybridization of polypyrrole with silica deserves special attention
due to its composite nature. The benefit of such composite is the
synergistic combination of properties of both the components. Thus
one can achieve required mechanical strength of silica as well as
high ion exchange properties of polypyrrole [3] in their composite
(organic–inorganic hybrid material based on polypyrrole and sil-
ica). The composite may be helpful in selective binding of chromate
through ion exchange process [12,13]. Two types of polypyrrole
∗
Corresponding author. Tel.: +91 3463 264983; fax: +91 3463 261526.
E-mail address: pranesh 02@yahoo.co.in (P. Chowdhury).
silica composites (PPY–SiO
2
) such as (a) silica rich PPY–SiO
2
nano
composite [8] and (b) polypyrrole rich PPY–SiO
2
hybrid materials
[7] are gaining importance now-a-days due to their various appli-
cations. We have focused on the latter approach in the present
study.
Various authors reported on the preparation of PPY–SiO
2
com-
posites. Armes and co-workers [14–17] have shown that the
polymerization of pyrrole in the presence of ultra fine aqueous silica
sols lead to the formation of unusual “raspberry-shaped” PPY–SiO
2
nano composite which exhibit silica-rich surfaces. Wallace et al.
[18,19] used porous silica gel particles for the preparation of novel
silica rich PPY–SiO
2
composite for chromatographic use. Faverolle
and fellow researchers [20,21] demonstrated that polypyrrole
could be deposited onto E-glass fibers with the help of silane cou-
pling agent. The resulted composite leads to polypyrrole rich over
layers (20–50 nm thickness). Chehimi and his group [7,22] describe
the use of aminopropyl triethoxysilanes (APTS) in the preparation
of polypyrrole-coated silica gel (PPY–APTS–SiO
2
) with the aim of
obtaining a polypyrrole-rich hybrid particles with surface area in
the range162–184 m
2
/g.
In the present work, we demonstrate the role of dimethyl
dichloro silane (DDS) in the preparation of polypyrrole-grafted sil-
ica gel (PPY–DDS–SiO
2
) with a view to obtain polypyrrole-rich
silica particles with surface area greater than 200 m
2
/g. The pro-
cess will be compared to the method published by Chehimi et al.
[7,22] and it will be different from Armes et al. [14–17]. We have
synthesized polypyrrole nanoparticles for grafting onto function-
alized silica gel and studied its chromium(VI) binding ability. A
0039-9140/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.talanta.2010.11.037