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Desalination 263 (2010) 279284

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Desalination
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / d e s a l

Application of polyaniline and polypyrrole composites for paper mill


wastewater treatment
Mohsen Ghorbani a, Hossein Esfandian b, Nastaran Taghipour c, Reza Katal c,
a
b
c

Faculty of Chemical Engineering, Babol University of Technology, Babol, Iran


Faculty of Chemical Engineering, Elm-o-Sanat University, Tehran, Iran
Department of Chemical Engineering, Tarbiat Modares University, Tehran, Iran

a r t i c l e

i n f o

Article history:
Received 3 May 2010
Received in revised form 25 June 2010
Accepted 28 June 2010
Keywords:
Polypyrrole
Polyaniline
Paper mill wastewater
Sawdust
Treatment
Composite

a b s t r a c t
This paper deals with a new application of polyaniline (PAn) and polypyrrole (PPy) synthesized chemically.
Coated on sawdust via cast method the polypyrrole/sawdust (PPy/SD) and polyaniline/sawdust (PAn/SD) were
used as effective adsorbents for the removal of heavy metals, anions, color and COD (chemical oxygen demand)
from mill paper wastewater. The products were investigated in terms of morphology and chemical structure
using scanning electron microscopy and Fourier-transform infrared spectroscopy (FTIR), respectively. It was
found that PPy/SD and PAn/SD are very simple to prepare and can be used as effective adsorbents in the removal
of anions, heavy metals, color and COD from paper mill wastewater.
2010 Elsevier B.V. All rights reserved.

1. Introduction
High consumption of water is one of the most important
environmental concerns in paper industry. In an attempt to overcome
this problem, zero liquid efuent technologies are being developed.
In these technologies circuits are closed and water is continuously
recycled [13]. Such wastewater contains a large amount of pollutants
characterized by biochemical oxygen demand (BOD), chemical oxygen demand (COD), suspended solids (SS), toxicity, and colorants
which cause bacterial and algal slime growths, thermal impacts,
scum formation, color problems, and a loss of both biodiversity and
aesthetic beauty in the environment [4]. The main treatment processes used at pulp and paper mill plants are primary clarication
(sedimentation or otation), secondary treatment (activated sludge
process or anaerobic digestion) and/or tertiary processes (membrane
processes as ultraltration) [5]. Activated sludge plants have been
the most common wastewater treatment process for the removal of
organics in our country; however, there are several problems with the
process. It produces sludges with very variable settlement properties,
it is sensitive to shock loading and toxicity, and its capacity to remove
poorly biodegradable toxic substances is limited [6]. Different type of
catalysts such as Fenton agent and TiO2, have been used to degrade
pollutants from board paper industries and revealed that the Fenton

Corresponding author. Fax: + 98 2182883381.


E-mail address: reza.katal@hotmail.com (R. Katal).
0011-9164/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2010.06.072

reagent gave a higher degree of total COD and BOD depletion compared to TiO2 [7]. In the same year, the occulation performances of
polyacrylamides have been reported for treating pulp and paper mill
wastewater. They revealed that cationic polyacrylamides, like Organopol 5415, with a very high molecular weight and low charge density
achieved a reduction of 95, 98 and 93 % in turbidity, total suspended
solid (TSS) and total COD, respectively, with a sludge 13858947/$
volume index (SVI) of 14 mL/g at the optimum dosage of 5 mg/l [8].
Buzzini and coworkers reported a system based upon precipitation
with a microbial community which provided approximately 8086%
and 7578% total COD removal with and without recirculation of the
efuent, respectively [9].
Since the discovery of conducting polymers three decades ago, a
large volume of research work has been performed associated with
the physics and chemistry of conducting polymers. PPy and PAn is the
most environmentally stable known conducting polymer and also one
of the most commonly investigated conducting polymer due to its
high electrical conductivity and simple preparation [10]. Conducting
polymers found applications in various elds such as microelectronics, composite materials, optics and biosensors [11] and as adsorbent
[12,13]. The ion exchange capacities of conducting Polymers were
well understood and it was found to depend on the polymerization
conditions, the type and size of the dopants incorporated during the
polymerization process as well as on the ions present in the electrolyte solution, the polymer thickness and ageing of the polymer [14].
Review of the literature revealed that PPy synthesized in solutions
with small dopants such as Cl, ClO4, NO3, etc., mainly exhibits

280

M. Ghorbani et al. / Desalination 263 (2010) 279284

anion-exchanger behavior due to the high mobility of these ions in


the polymer matrix. While under certain conditions cation exchange
was also found to take place with large dopants like polyvinylsulfonate and polystyrenesulfonate, due to immobility of these ions in the
polymer matrix [14]. adsorption of metal ions by several functionalized polymers based on amines derivatives such as polyacrylonitrile
bers, ethylenediamine, polyacrylamides, poly-4-vinylpyridine, polyethyleneimine, aniline formaldehyde condensate, etc., have been
reported [1520]. Chakraborty and coworkers have investigated one
amine-based polymer, short-chain PAn coated on jute ber for the
removal of chromium in batch mode and Fixed-bed column [21,22] .
polypyrrole was used in the removal of uoride ions from aqueous
solution by conducting PPy [23].
This article reported the removal efciency of heavy metal, anions,
color and COD of paper mill wastewater using PAn/SD and PPy/SD.
2. Materials and methods

Table 1
Textile wastewater characterization.
Compound

Concentration in waste water before removal

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

300
21
155
1.5
33
0.5
0.3612
2700
16

concentration of heavy metals, anions, color and COD was determined.


All the tests were at least carried out twice. Standard deviation for
duplicate experiments in all experiments was less than 3%. Table 1
shows the characteristics of the wastewater (paper mill factory in
Shahi).

2.1. Instrumentation
2.5. Characterization of mamrez tree sawdust
A digital scale FR200, a PH meter, a scanning electron microscope
(SEM) model XL30, a Fourier-transform infrared (FTIR) spectrometer
model shimadzu 4100 have been used in these experiments. Also a
manual Photometer SQ300 Merck as spectrophotometer and Merck
Spectroquant Test Kits were used for the analysis of COD (catolog
2

no.: 114555), NO
(no.: 1.14779),
2 (no.: 100609), NO3 (no.: 100614), S
2
SO
(no.:
114548).
Atomic
absorption
spectrometer
(AAS)
(Model 929,
4
Unicam) was used to analyze the concentration of heavy metal ions.
Conductivity was measured by the four-point method using a current
source.
Keithley 238, a scanner Keithley 706 with switching cards, and
a Solartron-Schlumberger 7081 Precision Voltmeter. The densities of
the samples were determined by the Archimedes method by weighing
the pellets in the air and immersed in decane.
2.2. Preparation of PAn/SD composite
1 g of KIO3 was added to 100 mL of sulfuric acid (1 M) and mixed
by a magnetic stirrer to make a uniform solution. Then, 1 g of SD and
1 mL fresh distilled aniline monomer was added to stirred solution.
The reaction took place for 4 h at room temperature. Finally, the
product was ltered to separate the impurities, and the products
were isolated on lter paper and washed several times with deionized
water and dried at room temperature.
2.3. Preparation of PPy/SD composite

A SEM micrograph of mamrez tree sawdust is shown in Fig. 1.


Mamrez tree sawdust is a heterogeneous material consisting largely of
small spheres, irregular, porous, coke like particles of cell wall of plant
cells. The surface seems to be rough, and protrusions can be seen
throughout the micrograph (Table 2). Pores can be seen however, not
extending into the matrix. The surface roughness is indicative of high
surface area. Characteristics of the adsorbent such as surface area, bulk
density, moisture content, ash content, solubility in water (inorganic
and organic matter) were determined. The results are summarized in
Table 3.
3. Results and discussion
The morphology of sawdust before and after coating with PAn and
PPy is illustrated in Figs. 13. The coating with conducting polymer
produced by surface polymerization is very visible. The coating of SD
has always been found to be uniform by visual inspection, while
coating defects have been suspected in the case of SD at low PAn or
PPy contents. Some PAn precipitate produced by the precipitation
polymerization of aniline in the liquid phase adhered to the PAncoated SD (Figs. 2 and 3) when the polymerization proceeded at a
high (0.2 M) concentration of aniline. The macroscopic particles of
sawdust are not coated only at the surface but the big sizes of sawdust
that constitute their body have also been coated. This means that the
reaction mixture diffuses into particles and all SD inside the particles
become coated with conducting polymer.

5 g FeCl4 was added to 100 mL of water and then a uniform solution was resulted using magnetic mixer. Then, 1 g of SD and 1 mL fresh
distilled pyrrole monomer was added to stirred solution. The reaction
was carried out for 4 h at room temperature. Finally, the product was
ltered to separate the impurities, the products were isolated on lter
paper and washed several times with deionized water and dried at
room temperature.
In order to remove any dissolvable color materials in SD, PAn/SD
and PPy/SD, they were washed with acetone and sodium hydroxide
(0.3 M) until the washing liquid was colorless.
The composite has been grinded before use and their size were
between 1 and 2 mm.
2.4. Removal technique
Adsorption experiments were performed by agitating 0.5 g of sorbent with 50 mL of paper mill wastewater at 30 0.5 C in magnetic
mixer. The rotating speed was 700 rpm throughout the study. At the
end of predetermined time intervals, the sorbent was ltered and the

Fig. 1. SEM image of SD.

M. Ghorbani et al. / Desalination 263 (2010) 279284

281

Table 2
Various physical parameters for the adsorbent (mamrez tree sawdust).
Parameters

Values

Particle size (mm)


Surface area (m2/g)
Bulk density (g/cm3)
Moisture contents (%)
Water soluble components (inorganic matter) (%)
Insoluble components (organic matter) (%)

35
620
1.25
5.75
16.45
76.25

Table 3
Conductivity and density of sawdust, conducting polymers, and their composites at
20 C.
Compound
SD
PAn/SD
PPy/SD
PAn
PPy

Conductivity (S cm 1)
1.4 10
0.30
0.16
2.1
0.9

14

Density (g cm 3)
1.25
1.30
1.34
1.38
1.45

Fig. 4. SEM image of PAn/SD with more zoom.

Figs. 4 and 5, show with more Zoom Polymer coat is on the


sawdust. As can be seen, PPy and PAn, has been formed. In general,
increasing the amount of additives in the reaction, such as sawdust,
inuences the physical properties of composites.

Fig. 5. SEM image of PPy/SD with more zoom.

Fig. 2. SEM image of PAn/SD.

Fig. 3. SEM image of PPy/SD.

The structure of products was determined by FTIR spectrum which


has been done to identify the characteristics of the peaks of diagram
for the related products.
FTIR spectra in the 2500500 cm 1 region, for the products are
shown in Figs. 6 and 7. As can be seen, the peak 1502 cm- 1 has been
assigned to the C = C stretching vibration of the quinoid ring, the
peak at 1402 cm 1 is assigned to the stretching vibration of C = C of
the benzenoid ring and 1296 cm 1 correspondence to CN stretching
vibration.

Fig. 6. FTIR spectra of PAn/SD.

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M. Ghorbani et al. / Desalination 263 (2010) 279284

Fig. 7. FTIR spectra of PPy/SD.

For studying affects SD on conductive polymer properties, conductivities and densities of composites, SD, PAn and PPy were measured
(Table 3). PAn and PPy have identical densities therefore composites

densities are equal. PA/SD, PPy/SD composites have much higher conductivities than conductivity of SD.
Experiments were done using PA/SD, PP/SD during 25 min with 5minute intervals. As can be seen (Tables 4 and 5) increasing the time
(5 to 20 min) removal efciency increased but after 20 min it increased
not signicantly.
For studying effect of SD size on removal efciency, SD indifferent
sizes (2050 m, 100150 m, 12 mm, 2030 mm) was coated with
polymer and applied for wastewater treatment. Amount of adsorbent
was 0.5 g, wastewater volume was 50 mL and the treatment process
was in 20 min. The results are indicated in Tables 6 and 7. As can be
seen decreasing SD size of 2030 mm to 12 mm removal efciency
increased but decreasing more, removal efciency decreased. The
reason could be for small size SD, polymer diffuses into SD so is not
coated on SD surface that made removal efciency decreased.
In Table 8, the removal efciency of wastewater is shown using
PAn, PPy and SD. As can be seen in Table 8, SD has low efciency in
the removal of anions and COD, but its performance to remove metals
and color is considerable. PPy and PAn have noticeable efciency
in the removal of metals, anions, color and COD. However, in all
experiments, the removal efciency of PPy and PAn are lower than
composites. Therefore it can be concluded that SD in the composites
does not play signicant role in the anions and COD removal but the

Table 4
Analyze of mill paper waste water after removal using PPy/SD in different time of reaction.
Compound

Removal efciency after


5 min of reaction (%)

Removal efciency after


10 min of reaction (%)

Removal efciency after


15 min of reaction (%)

Removal efciency after


20 min of reaction (%)

Removal efciency after


25 min of reaction (%)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

52.4
50.15
55.35
60.46
56.65
60.11
62.55
38.72
61.28

68.4
65.5
70.64
72.5
67.14
71.5
74.58
52.47
73.65

78.54
75.82
81.43
85.27
77.41
84.72
86.68
61.44
82.38

84.5
83.67
87.45
94.2
87.1
92.17
93.22
65.41
89.55

84.82
84.1
88.32
94.54
87.85
92.25
94.05
65.55
90.1

Table 5
Analyze of mill paper waste water after removal using PAn/SD in different time of reaction.
Compound

Removal efciency after


5 min of reaction (%)

Removal efciency after


10 min of reaction (%)

Removal efciency after


15 min of reaction (%)

Removal efciency after


20 min of reaction (%)

Removal efciency after


25 min of reaction (%)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

45.41
45.78
47.65
53.25
44.85
56.7
55.42
31.24
52.45

62.5
58.74
64.25
67.42
62.34
67.86
69.56
42.52
70.75

74.15
72.51
79.45
80.34
73.68
80.38
79.35
53.25
79.21

80.1
81.3
79.8
85.6
82.7
86.72
84.44
58.71
84.15

80.65
82.04
80.42
86.4
83.84
88.2
85.65
59.34
85.04

Table 6
Wastewater treatment using PPy/SD with different particle size.
Compound

Particle size between


10 and 15 m

Particle size between


1 and 2 mm

Particle size between


100 and 150 m

Particle size between


20 and 50 m

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

81.75
79.25
83.42
89.5
82.68
85.4
85.52
57.32
84.31

84.5
83.67
87.45
94.2
87.1
92.17
93.22
65.41
89.55

72.3
74.25
74.84
80.16
70.64
83.67
83.45
51.22
80.86

61.93
57.25
55.45
75.23
53.22
80.24
75.32
34.54
76.78

M. Ghorbani et al. / Desalination 263 (2010) 279284


Table 7
Wastewater treatment using PAn/SD with different particle size.

Table 9
The removal efciency of PAn, SD and PPy, SD (not in composite form).

Compound

Particle size Particle size Particle size Particle size


between 10 between 1 between 100 between 20
and 15 m and 2 mm and 150 m and 50 m

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

66.74
73.35
77.21
81.65
76.72
82.68
79.78
50.45
78.35

80.1
81.3
79.8
85.6
82.7
86.72
84.44
58.71
84.15

66.56
70.12
68.23
78.45
63.75
81.25
80.56
45.75
77.64

283

58.45
51.51
50.46
74.87
48.53
77.86
72.37
30.25
76.78

Table 8
The analyze of wastewater after treatment using PAn, PPy and SD.

Compound

Removal efciency
(%) using PAn
and SD (not in the
composite form)

Removal efciency
(%) using PPy and
SD (not in the
composite form)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

67.52
78.68
76.5
73.7
79.3
75.42
71.51
52.4
70.14

75.8
81.24
84.3
82.5
83.25
80.04
78.7
62.74
80.12

Table 10
Desorption data using H2SO4, NaOH and distillated water.

Compound

Removal
efciency
of PAn (%)

Removal
efciency
of PPy (%)

Removal
efciency
of SD (%)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

63.5
78.2
72.27
69.43
81.7
72.54
57.41
57.45
64.38

74.73
84.16
85.24
76.23
84.11
72.45
61.37
64.52
78.65

56.34
7.45
11.24
71.76
9.8
78.41
71.12
3.07
74.75

role of SD in the removal of the metals and color is considerable, and it


causes an increase in the removal efciency of the composites.
Fig. 8 shows decolorization of paper mill wastewater .As illustrated,
the color of wastewater is decreased after treatment by composites,
and clear liquid was obtained. This gure indicates the high efciency
of PAn/SD and PPy/SD in the wastewater decolorization.
The results of application of PAn, SD and PPy, SD (not in the composite form) are shown in the Table 9. As can be seen, removal efciency
of composites are higher than PAn, SD and PPy, SD (not in the composite
form).
Heavy metals, color, COD and anions desorption from the PAn/SD
and PPy/SD were investigated using solutions of the following three
materials: 1 M H2SO4, distillated water and 1 M NaOH. As can be seen
in Table 10, anions desorption efciencies using NaOH, was more than
desorption efciencies using deionized water and H2SO4. Color and
COD desorption efciencies using distilled water was more than two
others. Metals (Fe, Mg and Cu) desorption efciencies using H2SO4
was higher and for Zn desorption efciency using NaOH was more
than others.

Compound

Desorption
efciency
using
NaOH (%)

Desorption
efciency
using
H2SO4 (%)

Desorption
efciency using
distillated
water (%)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

32.5
93.74
92.25
24.27
88.54
25.45
38.24
42.86
92.5

85.52
18.14
25.78
88.2
14.74
87.94
48.56
58.3
47.8

51.35
38.74
44.58
42.5
57.2
52.46
82.45
88.74
61.5

Removal efciency of anions, color, COD and heavy metals using


regenerated adsorbents is shown in Table 11. The adsorbents were
washed by H2SO4, NaOH and deionized water respectively. As shown
in Table 11, there is a little difference between regenerated and fresh
composites in the removal efciency.

4. Conclusion
The composite of conducting polymer showed considerable potential in the removal of heavy metals, color and anions from paper mill
wastewater and have the ability to remove COD; but the removal
efciency of COD is lower than removal efciency of anions, metals and
color. Composites regeneration operation is performed using NaOH,
deionized water and H2SO4. After regeneration, composites were used
for wastewater treatment. Ability of these composites has no considerable difference, with the fresh composites for removing color, COD,
anions and heavy metals. Also, the efciency of these composites are
higher than PAn PPy and SD to treat the wastewater.

Table 11
Analyze of mill paper waste water before and after removal by regenerated PPy/SD and
PAn/SD.

Fig. 8. (a) Wastewater, wastewater after treated with (b) PPy/SD, (c) PAn/SD.

Compound

Removal efciency
of PAn/SD (%)

Removal efciency
of PPy/SD (%)

Mg (mg/l)
S 2 (mg/l)
2
SO
(mg/l)
4
Fe (mg/l)
1
1
Total N (NO
3 , NO2 ) (mg/l)
Cu (mg/l)
Color (adsorbance, at 600 nm)
COD (mg/l)
Zn (mg/l)

77.85
79.01
76.1
81.08
82.7
83.14
83.33
52.71
84.73

82.71
83.22
84.35
90.05
86.43
86.54
91.86
59.43
87.42

284

M. Ghorbani et al. / Desalination 263 (2010) 279284

Acknowledgements
The research upon which this paper is based was supported by
a grant from the Khosro Katal. Saied Farhadi at Tarbiat Modares
University is acknowledged for his assistance with experimental design
and analysis.
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