Fabrication of Silane Nanocrystalline Cellulose Bio Nanocomposites For The Abatement of Arsenic

International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 6480(Print),
ISSN 0976 6499(Online) Volume 5, Issue 9, September (2014), pp. 70-79 IAEME
70

FABRICATION OF SILANE-NANOCRYSTALLINE CELLULOSE:
BIO-NANOCOMPOSITES FOR THE ABATEMENT OF ARSENIC

Kiran Singh
a
, T. Jai Mangal Sinha
b
, Shalini Srivastava
a

a
Department of Chemistry, Faculty of Science
Dayalbagh Educational Institute, Agra, 282110, India
b
ACS Chemical Innovations, Maharashtra, 4000614, India

ABSTRACT

Arsenic impact on human health has led its minimum contamination limit to be drastically
reduced from 50 to 10 g/L and has resulted in technical and operational impact on water treatment
technologies that have required up-gradation to meet this new standard. The piece of work addresses
synthesis, characterization of nano crystalline cellulose reinforced with silane coupling agents
(3-Aminopropyltrimethoxy silane (APTMS) and 3-Mercaptopropyltrimethoxy silane (MPTMS)
having strong affinity for both the arsenic species. Designed bio-nano composite filled in
polypropylene bags were used for arsenic abatement from water bodies at laboratory batch
conditions. APTMS- NCC and MPTMS- NCC composites exhibited 8.86 and 13.16 mg/g and 9.48
and 8.57 mg/g sorption for As (III) and As (V), respectively. Morphological integrity and
crystallinity of the NCC was maintained after the functionalization as studied by XRD and SEM.
TEM analysis indicated that the dimensions of the NCC was between 5-20 nm. The proposed
biosorbent is suited to be used in the development of an economical pre-treatment step before large
scale chemical treatments for arsenic remediation from water bodies.

Keywords: Arsenic, Functionalization, Bio-Nano Composite, Pre-Treatment Step.

1. INTRODUCTION

Over the past years, intensive research on biosorption of toxic metals/metalloids has
established solid base of knowledge, principles and enormous potential for commercialization
particularly at low level decontamination (Calace et al. 2002). Research towards identifying new
technologies/ reinforcements/ modifications to existing technologies has been conducted for arsenic
removal (Mohan et al. 2007). The highest priority of commercially available remediation technology
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ISSN 0976 - 6480 (Print)
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is the assessment of the commercial potential, practicability of the developed technology,
competition with other technologies, market size, and cost of raw biosorbents (Egila et al. 2011).
Polymer nano-composites have been a subject of increasing interest because of their significant
enhanced mechanical and thermal stability (Alloin et al. 2010, Habibi et al. 2010). Highly ordered
configuration, strength, abundance, stiffness, low weight and biodegradability are some of the special
features of nano-scale cellulose polymers which make them promising candidates for bio-nano
composite production for the removal of cationic metal species (Ning et al. 2011, Mabrouk et al.
2011). However, information on its application towards their suitability for the sorption of anionic
species like arsenic is scanty.
Silane-coupling agents usually improve the degree of cross-linking in the interface region and
are very reactive to hydroxyl groups. Further, hydrolysis-condensation steps of methoxy-silane
groups produce an oligomeric network of polysilsesquioxane (Xie et al. 2010). Therefore, the
hydrocarbon chains of silane are supposed to restrain the swelling of the fiber by creating a cross-
linked network involving covalent bonding between the silane and nanocrystalline cellulose (NCC).
Furthermore, the interconnected pore structure formed by the voids between the NCC and silane
coupling agent would be easily accessible to target arsenic species, improving the decontamination
efficiency. Surface functionalization is also supposed to incorporate cationic amino and thiol groups
responsible for the sorption of anionic arsenic species consequently promoting the sorption capacity
and desirable compatibility with hydrophobic polymer matrices.
In continuation of our work on synthetic and nanotech reinforcements on cellulose for the
decontamination of toxic metals (Srivastava et al. 2005, Goyal and Srivastava 2009, Raj et al. 2010,
Singh et al. 2014), the present communication highlights the use of silane coupling agents
(3-Aminopropyltrimethoxy silane and 3-Mercaptopropyltrimethoxy silane) for arsenic (arsenite and
arsenate) biosorption as one of the operational parameter in the development of innovative
economically sustainable water treatment.

2. EXPERIMENTAL

2.1. Reagents and chemicals
All chemicals were of analytical grade. Stock solutions of arsenic containing 1,000 mg/L
As(III) and As(V) were prepared by dissolving NaAsO
2
and Na
2
HAsO
4
7H
2
O in double distilled
water and stored in darkness at 4 C.

2.2. Preparation of Nanocrystalline cellulose
NCC was prepared by sulfuric acid hydrolysis of microcrystalline cellulose (MCC)
(Ioelovich, 2012). MCC (50.0 g oven dried weight) was mixed with H
2
SO
4
solution (62 %, w/v) with
continuous stirring at 45 C for 40 min. Hydrolysis reaction was stopped by adding excess (10 fold)
of distilled water followed by the removal of acidic solution by successive centrifugation at 12,000
rpm for 10 min. until the supernatant became turbid. The sediment was collected and washed against
distilled water until the pH of the solution became neutral. After washing, the content was sonicated
for 30 min. The cloudy supernatant, containing NCC, was collected and the remaining sediment was
again mixed with water, sonicated and centrifuged to obtain additional NCC, this procedure was
repeated till the supernatant was clear.

2.3 Preparation of NCC-Silane composite
3-Aminopropyltrimethoxy silane (APTMS) was pre-hydrolyzed for 2 h under stirring in
ethanol-distilled water solution (100 ml; 80/20 v/v) (Xie et al. 2009). NCC was dried under vacuum
at 60 C for 24 h. The treatment of NCC (10.0 g) with APTMS (100 ml) was performed and the
resulting suspension was maintained for 2 h under stirring and then removed from the solutions and
72

dried at room temperature for 24 h. The dried sample was heated at 110 C for 2 h to promote actual
coupling. At the end of the reaction, NCC was centrifuged at 1400 rpm for 2 min. The concentration
of the silane coupling agent was varied from 0.0-3.0%. pH was adjusted to 4.55.0 by adding acetic
acid. The same procedure was followed for 3-Mercaptopropyltrimethoxy silane (MPTMS).

2.4. Characterization of NCC and NCC-silane composite
NCC and NCC-silane composites were dried at 105 C for 6 h and cooled to room
temperature for analysis. The dimensions of the NCC were measured by transmission electronic
microscopy (TEM-JEOL 2100F) operated at 80 kV. NCC suspension at 4% (w/v) was mildly ultra
sonicated in a water bath sonicator for 30 min, and 1 mL of the solution was dropped on a 300 mesh
copper grid coated with Formvar polymer. After 2 min, the excessive water was drained with a
Whatman paper no. 2, and the grid was inverted and allowed to touch a drop of uranyl acetate 2%
(w/v) for 5 min. The process was repeated three times, and the grid was air-dried at room
temperature for 24 h. The average crystallite size and crystallinity pattern of NCC-silane composites
were recorded using glancing angle X-ray diffractometer (Bruker AXS D8 Advance, Germany) with
Cu K radiation at 40 kV and 30 mA. Scattered radiation was detected in the range 2 = 5-40
o
, at a
speed of 2
o
/min. The morphological characteristics were evaluated using Scanning Electron
Micrograph Zeiss EVO40 at bar length equivalent to 10 m at working voltage 15 kV with 500X
magnification. FTIR analysis in solid phase in KBr was performed using a Shimadzu 8400 Fourier
Transform Infrared spectroscope. Absorption mode FT-IR spectra were recorded in 600-4,000 cm
-1

range and scanned for 64 times.

2.5. Batch experiments for sorption and desorption studies
Batch experiments using standard practices were performed as functions of contact time (10-
50 min), volume of test solution (100-300 ml), pH (1-10) and arsenic ion concentration (0.01-50
mg/L), shaking rate 250 rpm at room temperature in clean air-conditioned environmental laboratory.
Non-woven polypropylene filter bags were prepared containing different amount (0.1 - 1.0 g) of
adsorbent dose. The solutions of As (III) and As (V) were taken into separate erlenmeyer flasks.
After proper pH adjustments, a filter bag containing adsorbent of known quantity was dipped into
arsenic bearing suspension and kept under stirring until the equilibrium conditions were reached.
After shaking, suspension was allowed to settle down. Arsenic treated filter bag was taken out and
filtrate was collected and subjected for arsenic ions estimation using ICP OES Perkin Elmer
Optima 8x00.
Percent arsenic sorption was computed using the equation: % Sorption

100],
where, C
and C
are the initial and final concentrations of arsenic ions in solution. All the
investigations were carried out in triplicate to confirm reproducibility of the experimental results.
The reproducibility and relative deviation are considered at 0.5% and 2.5%, respectively. The
adsorption capacity Q
(mg/g) was calculated from the following equation: Q
V
,
where
C
and C
represent the initial and final concentrations of the arsenic solutions, respectively. V and m
are the solution volumes and adsorbent dose.

2.6. Statistical and Error analysis
Batch experiments were conducted in triplicate (N=3) and data represents the mean value.
Mean values, correlation coefficients, and standard deviations were computerized. For inter-group
mean value differences, each parameter was subjected to the Students t-test for significance level
(p < 0.05). For nonlinear fitting of kinetic data, the Standard Error (SE) analysis is used to evaluate
the applicability of the model. The SE is calculated as SE
where,
and

International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976
ISSN 0976 6499(Online) Volume 5, Issue 9, September (2014), pp.
are the experimental and model calculation values, respectively; N is the number of the experimental
points. For the confirmation of the best fit for the adsorption system, it is necessary to analyze the
data using SE by combining the values of correlation coeffic

3. RESULTS AND DISCUSSION

Applied synthetic strategy is based on the fact that, arsenic forms bond with organic sulphur,
nitrogen and carbon. As (III) shows high affinity towards sulphur and sulphydryl groups, while As
(V) with reduced nitrogen groups (Kumaresan et al. 2001).
NCC to introduce positively charged
(III), respectively, have been carried out.

3.1. Structural confirmation of preparation of NCC and
NCC was obtained in 6070 % yield and
composites in 82-84 % yield. The degree of substitution
taken as an evidence for the success of
Silanes withamino andthiol
OH groups in a controlled aqueous
silanes is illustrated in Fig. 1. The Si
undergoes hydrolysis of alkoxy group
susceptible for auto-condensation, forming
of oligomeric network on the NCC surface

Fig. 1: Synthetic strategy used for the preparation of APTMS

In FTIR spectra of NCC, a
presence of free and hydrogen bonded
1429 cm
1
, 1152 cm
1
, 1001 cm
1

vibrations, COC anti symmetric stretching vibration,
linkages, respectively.

International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976
6499(Online) Volume 5, Issue 9, September (2014), pp. 70-79 IAEME
73
experimental and model calculation values, respectively; N is the number of the experimental
data using SE by combining the values of correlation coefficient (R
2
).
3. RESULTS AND DISCUSSION
nitrogen groups (Kumaresan et al. 2001). Therefore, synthetic modifications
to introduce positively charged amino and thiol groups having affinity for As (V) and As
(III), respectively, have been carried out.
Structural confirmation of preparation of NCC and NCC-Silane composite
70 % yield and was silynated to obtain APTMS and MPTMS
. The degree of substitution (DS) is in the range of 1.4
the success of silanization onto NCC.
thiol groups were chosen, having substantial reactivity toward
in a controlled aqueous environment. The expected reaction between
The SiOC bond of silane being unstable in the presence of moisture
hydrolysis of alkoxy groups, forming silanol (SiOH) groups. Silanol groups
forming SiOSi linkage ultimately resulting into the fabrication
the NCC surface (Gousse et al. 2002).
Synthetic strategy used for the preparation of APTMS-NCC and MPTMS-NCC composites
In FTIR spectra of NCC, a broad band (Fig. 2) at around 3324 cm
1
is attributed to the
presence of free and hydrogen bonded OH stretching vibrations. The peaks at 2891 cm
and 896 cm
1
corresponds to the CH stretching
ric stretching vibration, CO stretching vibration and glycosidic
experimental and model calculation values, respectively; N is the number of the experimental
Therefore, synthetic modifications onto
thiol groups having affinity for As (V) and As
Silane composites
APTMS and MPTMS-NCC
(DS) is in the range of 1.4-3.2. DS was
substantial reactivity toward
between NCC chains and
stable in the presence of moisture
ilanol groups are
resulting into the fabrication

NCC composites
is attributed to the
OH stretching vibrations. The peaks at 2891 cm
1
,
CH stretching, CH
2
bending
CO stretching vibration and glycosidic
74

Fig. 2: FT-IR spectrum of MPTMS-NCC, APTMS-NCC composites and NCC

Silane (APTMS and MPTMS) modified NCC shows an increase in the relative intensity of
the band at 1,076 cm
-1
, which may be related to the SiOSi group stretching, which in turn may
indicate the formation of the polysilsesquioxane network. On the other hand, the absorption band in
the 960 cm
-1
region, attributed to SiOC symmetric stretching, was reduced in the modified NCC,
suggesting condensation of the silanol groups. The existence of siloxane is further confirmed by the
band at 838 cm
-1
attributed to Si -CH
2
group. The strong characteristic band at 1207 cm
-1
region
75

could be related Si O-Si. Moreover, a SiCH
3
band at 1265 cm
-1
also appeared clearly due to the
formation of polysiloxane network (Abdelmouleh et al 2002, Abdelmouleh et al. 2004). A deformed
amine band was observed at 1146 and 1465 cm
-1
in APTMS-NCC composite confirming the
presence of CH
2
N
+
H (CH
3
)
2
and aliphatic CN vibration, respectively. Band at 2548 cm
-1
confirms the presence of SH group in MPTMS-NCC composite.
NCC suspension had shape of dispersed triangular crystals depicted in the TEM image
(Fig. 3). On average, the NCC are 24 nm long (ranging from 10 to 30), 4 nm wide (ranging from 4 to
8), and have an aspect ratio (L/D) of 6 (ranging from 5 to 20). High resolution TEM lattice image of
NCC depicts the well spaced lattice fringes in a single crystal structure of NCC with high crystalline
quality. The crystal plane spacing of NCC is about 0.128 nm, which corresponds to (002) crystal
plane of face centered NCC single crystal.

Figure 3: TEM image of NCC at 20 nm magnification and at high resolution of 1nm

XRD analysis shows that the acid treatment results into narrowing and higher crystallinity
level of hydrolyzed cellulose (Fig. 4). Presence of three strong peaks at 2= 14.84, 22.76 and 34.98
are the characteristics of cellulose I (Klemm et al. 2005). Crystallinity index was calculated from the
ratio of the peak heights corresponding to crystalline and amorphous regions with an error of 0.3 %.
The observed slight decrease in crystallinity index reduction may be ascribed to the incorporation of
silane groups onto the NCC surface. X-ray crystallinity index of NCC, APTMS-NCC and MPTMS-
NCC composite were calculated using equation: CI
100, and found to be 92.56, 68.26

and 62.74 respectively. The average crystallite size was estimated from the full width at half-
maximum intensity (FWHM) of the reflection using Debye-Scherrer equation:
cos
, where is the breadth of the peak of a specific phase (2=22.56), K;

constant that varies with the method of taking the breadth (K = 0.94), ; the wavelength of incident
X-rays ( = 0.15418 nm), ; the center angle of the peak, and L; the crystallite length. The average
crystallite size was found to be 6, 118 and 122 nm for NCC, APTMS-NCC and MPTMS-NCC
composite respectively.

76

Fig. 4: XRD spectrum of NCC, APTMS-NCC and MPTMS-NCC composite

SEM images (Fig. 5) of NCC, APTMS-NCC and APTMS-NCC composite indicate that the
surface morphology of NCC looks smooth and triangular. However, after silanization, the shape of
the NCC is slightly deformed, losing their original triangular shapes in both silane modifications.
SEM image also points out that silane-NCC composites are rougher than NCC, which might be due
to the heterogeneous reaction on the surface of NCC. After the silanization reaction, obvious coating
layers are observed confirming the immobilization of the silane groups on the surface of NCC. NCC
appeared to be agglomerated before functionalization and was separated from each other after
silanization, reason being the incorporation of relatively hydrophobic groups on the surface.

Fig.5: SEM image of NCC, APTMS-NCC and MPTMS-NCC composites

002
101
021
040
77

3.2. Sorption Experiments
A series of batch experiments on sorption of As (III) and As (V) led to the standardization of
the optimum conditions for APTMS-NCC (88.60 and 95.60 %) and MPTMS-NCC composites
(94.40 and 85.70 %), respectively at arsenic ion concentration (25 mg/L), contact time (40 min),
volume (200 mL) and pH 7.5 for As (III) and 2.5 for As (V).
Fig. 6 shows the dependence of sorption behavior of arsenic species on pH at adsorbent dose
(0.5g). The observed varying trends of sorption with lowering and rise in pH explains highly pH
dependent nature of aqueous arsenic chemistry. Adsorption of As (III) shows gradually increasing
trend, attaining maximum adsorption (APTMS-NCC composite-88.60 and MPTMS- NCC
composites-94.40 %) at pH 7.5. The trivalent arsenic species exists in a non-ionic form (H
3
AsO
3
) in
the pH range 27 and in the anionic (H
2
AsO
3
-1
and HAsO
3
-2
) form (Ghimire et al. 2002) in the pH
range 710. Optimum sorption of arsenite species in the pH range 710 can be assigned to the
availability of the negatively charged As (III) species interacting with the positively charge silane-
NCC composite, having isoelectric points in the pH range 4.08.0. Maximum adsorption of As (V)
on (APTMS-NCC and MPTMS- NCC composites is found 95.60% and 85.70 % respectively at pH
2.5, while remains constant in the pH range of 310. The pentavalent arsenic species exists in the
monovalent (H
3
AsO
4
-1
) and divalent anions (H
2
AsO
4
2-
) in the pH range 25. Maximum sorption of
As (V) on cationic adsorbent observed at pH 2.5 can be easily ascribed to its interaction with the
anionic (H
2
AsO
4
-1
and HAsO
4
-2
) species, occurring predominantly in this pH range. The preference
of APTMS-NCC composite for As (V) and MPTMS-NCC composite for As (III) sorption depends
on the relative affinity of As (V) towards reduced nitrogen groups, while that of As (III) for thiol
groups.

Fig. 6: Effect of pH on As (III and V) sorption onto
a). APTMS-NCC and b). MPTMS-NCC composites

4. CONCLUSIONS

This study demonstrated that silane coupling agents are promising candidates for efficient
removal of arsenic from water bodies due to their high compatibility with NCC for water treatment.
The incorporation of positively charged amino and thiol groups in NCC significantly enhanced
binding capacity of negatively charged arsenic species. Such need based tailored cellulosic bio-nano
composites with enhanced sorption efficiency and environmental stability are important for the
development of simple and cost effective pretreatment step before large scale chemical treatments
for the removal of arsenic from water bodies.

78

ACKNOWLEDGEMENT

Authors are thankful to Prof. P.K. Kalra, Director, Dayalbagh Educational Institute,
Dayalbagh, Agra and Prof. Sahab Dass, Head, Department of Chemistry, for providing necessary
research facilities. Kiran Singh is grateful to UGC-BSR, fellowship (New Delhi), for rendering
financial assistance.

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International Journal of Advanced Research in Engineering and Technology (IJARET), ISSN 0976 6480(Print),

(mg/g) was calculated from the following equation: Q

100, and found to be 92.56, 68.26

, where is the breadth of the peak of a specific phase (2=22.56), K;

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