Pol. J. Environ. Stud. Vol. 28, No.

4 (2019), 2311-2319
DOI: 10.15244/pjoes/91076 ONLINE PUBLICATION DATE: 2019-01-18

Original Research
Synthesizing and Characterizing Sawdust
Biochar/Fe3O4 Nanocomposites and its Potential
Application in Textile Wastewater Treatment

Farah Nadeem, Nadia Jamil*, Amna Moazzam, Sajid Rashid Ahmad,

Ambreen Lateef, Anam Khalid, Abdul Qadir, Azhar Ali, Soniya Munir

College of Earth and Environmental Sciences, University of the Punjab, Lahore, Pakistan

Received: 5 January 2018

Accepted: 15 May 2018

Abstract

The present research deals with the synthesis and viability of Sawdust biochar/Fe3O4 nanocomposite
toward textile waste water treatment. The structure, functionality, and morphology of the nanocomposite
were determined by FT-IR, powder XRD, and SEM. Removal of the textile dye Reactive Blue 21 (RB21)
was almost 75% under optimum conditions. The value of Langmuir dimensionless separation factor
R L indicated a favorable adsorption (0<R L<1). Langmuir constant (K L, i.e., 0.15) symbolizes that there
is high affinity of the adsorbent for the adsorbate. The value of Freundlich constant was found to be
2.78 (n>1), hence denoting favorable sorption. The negative values for free energy indicated a spontaneous
reaction. Positive value for enthalpy suggested the endothermic nature of adsorption. The kinetic data
showed a pseudo first-order kinetic model. The calculated value of qt agreed with the experimental
value of qt at equilibrium. The results depicted that sawdust biochar/Fe3O4 nanocomposites are efficient
adsorbents for removing RB21 and has potential application in treatment of textile wastewater.

Keywords: textile wastewater, nanocomposites, adsorption, biochar

Introduction advanced oxidation [7], and phyto-catalytic degradation

[8]. Biodegradation of dyes is difficult because of their
Azo and reactive dyes are mostly used in various stable and complex chemical structure. Therefore, the
industries like textile, leather, paper, food, plastic, adsorption process has been adopted for removal of dyes
and printing of color products [1-3]. Dyes are toxic due to its simplicity, flexibility, ease of operation, and
for humans as well as the environment, and must be cost effectiveness [9].
treated before their discharge to reduce environmental Various adsorbents have been utilized for dye
pollution [4]. Several methods for removing dyes include removal, such as alumina, rice husk, banana peels,
membrane filtration [5], coagulation/flocculation [6], orange peels, coconut shells, peanut shells, and various
clays, etc. [10]. Among these, carbon-based materials
are more efficient adsorbents, comprising large numbers
of pores and high surface area for adsorption of dyes,
but due to their high preparation cost they can’t be used
*e-mail: [email protected]
2312 Nadeem F., et al.

on a large scale [11, 12]. Plenty of research has been was taken in a separating funnel and added dropwise
done on materials that can be used as raw materials for into the suspension of iron salts and SDB with
preparing low-cost charcoal [13], such as rice husk [14], continuous stirring. After dropping NaOH solution, the
seed shell [15], sawdust [16], coconut shell [17], pine suspension was filtered and washed with a mixture of
cone [18], and wheat husk [19]. ethanol and water to clear all impurities and by products.
These either have low adsorption capacity when The residue was dried in an oven (Memmert D-91126
applied for actual wastewater or are ineffective SchwabachFRG) at 150ºC for 2 hours.
for removing dyes. To enhance their effectiveness,
charcoal is incorporated with different nano-materials Characterization Techniques
for synthesizing nanocomposites [20]. Magnetic
nanoparticles have seemed to show promising results The residual dye concentrations in aqueous solutions
with dyes. They can degrade and adsorb dyes from were determined by a UV-Vis spectrophotometer
wastewater over a wide range of temperatures and (752N, HEB, China). The prepared nanocomposite was
pH values [11]. Charcoal with magnetic nanoparticles characterized by Fourier transform infrared spectroscopy
has been found to be more effective than other (FT-IR) to obtain information about the functional
nanocomposites [21]. Simply put, it can be separated by groups using a Fourier transform infrared spectrometer
external magnetic field from solution for reuse [22]. (Perkin Elmer spectrum RXI), scanning the sample
The current study is an attempt to synthesize in the wavelength range of 4000-700 cm-1. A powder
Fe2O3/sawdust charcoal nanocomposite adsorbent for x-ray diffraction (XRD) study was conducted using
removing dyes from simulated textile effluent to reduce a PANalyticalX’Pert Pro difffractometer. Diffraction
the environmental impacts of water pollution. Reactive data was attained by exposing samples to Cu-Kα x-ray
blue 21 is a commonly used dye in textile industries and radiation of wavelength (λ) 1.5418 Å. The sample
renders a strong color to the textile effluent. The use of was scanned for 20-80o2θ with step size of 0.05o2θ at
such nanocomposites can be employed in industries as 0.5 seconds per step size. Phase identification was
it will be a significant way forward for reducing water carried out by means of MATCH! software in
pollution and water waste caused by the textile industry. conjunction with the Crystallography Open Database.
The surface morphology of the sample can was
determined by scanning electron microscopy (Jeol
Materials and Methods JSM6480LV).

Synthesizing Sawdust Biochar (SDB) Batch Adsorption Studies: Kinetics,

Thermodynamics, and Isotherms
The sawdust was subjected to carbonization
under anoxic conditions using a charcolator operated The experiments of adsorption were carried out in
at atmospheric pressure. The sample at ambient 500 ml conical flask containing 30 ml of RB21 dye
temperature was placed in an aluminum container and solution and 0.25 g of Fe3O4/SDB nanocomposite, with
heated at 300ºC for three hours. A 1 mm hole was constant stirring at shaking speed of 200 rmp at different
drilled in the lid of the aluminum container so that temperatures(10ºC, 30ºC, 50ºC, and 70ºC) in different
steam and gas could escape to avoid any explosion time intervals (15, 30, 45, 60, 75, 90, and 105 minutes).
during heating. After the carbonization was over, Then the content of the experiment was filtered by
the container was left to cool for 30 minutes [23]. Whatmann filter paper No. 41 to measure the Reactive
The prepared charcoal was soaked in distilled water Blue 21 (RB21) dye concentration in each sample using
for 2 hours and then boiled for one hour. It was then UV-Visible Spectrophotometer (752N, HEB, China)
filtered, dried, ground to fine powder, and passed at λmax = 621 nm by plotting the calibration curve. To
through a 60 mesh/inch sieve. The sieved sawdust study the effects of optimum parameter, experiments
biochar was stored in Ziploc polyethylene bags at room were carried out for different nanocomposite doses of
temperature until further experimentation. 0.1, 0.15, 0.2, 0.25, 0.3, and 0.35 g/L at initial pH of
3, 5, 7, 9, and 11, and RB21 concentrations of 30, 60,
Synthesizing Fe3O4/SDB Nanocomposite 90, 120, 150, and 180 mg/L. Dye uptake efficiency was
calculated using Eq. 1:
The Fe3O4/SDB nanocomposite was synthesized
by an in situ chemical co-precipitation method [24] q (mg/g) = (Ci-Ce) x V/M (1)
in which SDB was used as support material. 20 g of
SDB was added to 400 ml distilled water in a 1000 ml …where q is the dye uptake by adsorbent (mg/g), and Ci
conical flask and stirred for 1 hr on a magnetic stirrer and Ce are initial and final concentrations of RB21 dye,
(MSH-20A WiseStir). In a separate beaker, 5.5602g of respectively. V is dye solution volume (1000 ml) and M
ferric sulphate (FeSO4.7H20) and 10.812g ferric chloride is the mass of adsorbent used (grams).
(FeCl3.6H2O) were dissolved in 200 ml distilled water The residual dye concentration in synthetic
and added in SDB suspension.100 ml of 0.8 M NaOH wastewater was calculated using Eq. 2:
Synthesizing and Characterizing Sawdust... 2313

R(%) = (Ci-Ce) / Ci x 100 (2) appearing at 1119 cm-1 and 1380 cm-1 were due to the
C-H bending and C-O stretching of the phenolic and
…where R is the residual dye concentration as methyl groups, respectively. Carbonyl vibrational
a percentage, and Ci and Ce are initial and final stretching can be observed at 1901cm-1. The peaks at
concentrations of BR21 dye, respectively. 2005 cm-1 and 2325 cm-1 correspond to C=O bond and
Isotherm models, including Langmuir and O=C=O stretching, respectively. The peak at 3218 cm-1
Freundlich models, were used to calculate equilibrium is attributed to O-H stretching, which could also be due
adsorption and to study surface properties and to the moisture content in the adsorbent [27].
attraction of adsorbent toward the dye molecules [25]. The powder XRD pattern of nanocomposite
The thermodynamic parameters were determined, and (Fig. 2a), indicates two distinct peaks depicting the
in order to explain the mechanism of adsorption of presence of carbon between 2θ values of 22° and 26°,
the solute on the adsorbent, the adsorption constants and of magnetite peak 36° as matched by the pattern
were calculated by pseudo first- and second-order [96-900-6922]. The nanocomposite was amorphous in
mechanisms [26]. nature, which depicts no or very little crystallinity. The
SEM image of Fe3O4/SDB nanocomposite in Fig. 2b)
(A and B) shows white color particles on SDB surface,
Results and Discussion which confirms the presence of Fe3O4.

Characterization of Fe3O4/SDB Nanocomposite Adsorption Capacity of Fe3O4/SDB Nanocomposite

Toward Adsorption Capacity of Reactive Blue 21
The FT-IR spectra of synthesized nanocomposite
shown in Fig. 1a) represents the peak at 799 cm-1, The present study investigated the adsorption of
which contributes to the Fe-O bond while other peaks RB21 on Fe3O4/SDB nanocomposite as a function
of shaking speed, shaking time, adsorbent dose, pH,

Fig. 1 a) FTIR spectra of Fe3O4/SDB nanocomposite; b) Comparison of FTIR spectra of Fe3O4/SDB nanocomposite before and after
adsorption of RB 21dye.
2314 Nadeem F., et al.

Fig. 2 a) Powder XRD pattern of Fe3O4/SDB nanocomposite along with COD reference pattern; b) SEM images of Fe3O4/SDB
nanocomposite at 10µm (A) and 50µm (B) resolution showing white color particles on charcoal surface.

temperature, and effect of initial dye concentration. there is sufficient speed, the sites on the surface of the
There was an increase in removal efficiency of adsorbent will be available to the dye [28]. However,
RB21 with the increase in shaking speed, as shown in after a certain speed (200 rpm in this case) there is a
Fig. 3a). However, removal efficiency decreased when reduction in the adsorption, and desorption begins.
the shaking speed was increased past 200 rpm. The This could be because there is more than the required
increase in adsorption with increase in agitation speed increase in the kinetic energy of the molecules of the
could be due to an increase in the mobility of the adsorbent as well as the dye, and they start hitting each
adsorption system. Resistance among the particles other with greater force, which results in detachment of
decreases and the adsorbate is moved toward the some dye molecules from the surface of the adsorbent
adsorbent. When the shaking speed is less, the adsorbent [29].
gets collected and does not spread, so a less active site The results in Fig. 3b) show an increase in removal
will be available for the adsorbate to adhere. When efficiency of RB21 with the increase in shaking time,
Synthesizing and Characterizing Sawdust... 2315

but after 90 minutes there was no further improvement that the more the adsorbent, the more the number of
in adsorption capacity. This behavior of the adsorbent sites present for adsorption. The adsorption sites do not
and dye could mean that high adsorption in the saturate the adsorption system, hence increasing the dye
beginning could be due to the large number of sorption uptake with an increase in adsorbent dose [31].
sites present at the earlier stage. A high concentration The effect of pH on adsorption of RB21 is shown in
gradient between dye in solution and dye present on the Fig. 3d), where the results depict maximum adsorption
surface of the adsorbent is developed. As the contact at neutral pH. The adsorption decreased in acidic and
time increases, the number of active sites also decreases basic conditions. Similar results were obtained by some
because they have been occupied by the adsorbate. researchers [32] when using activated carbon to remove
When an optimum time is reached and maximum azo dyes. Highly acidic conditions led to an increase
sites have been utilized, no further change in removal in amount of H+ ions, and the surface of the charcoal
efficiency is observed [30]. composite obtains a positive charge by absorbing those
We observed that removal efficiency of RB21 ions. The dye ions and the hydrogen ions hence get into
increased continuously with the increase in adsorbent a competition for the surface of the adsorbent, resulting
dose as in Fig. 3c). This could be justified by the fact in low adsorption of dyes due only to iron oxide

Fig. 3. Effects of: a) shaking speed on adsorption of RB21 on Fe3O4/SDB nanocomposite, b) shaking time on adsorption of RB21 on
Fe3O4/SDB nanocomposite, c) adsorbent dose on adsorption of RB21 on Fe3O4/SDB nanocomposite, d) different pH on adsorption of
RB21 on Fe3O4/SDB nanocomposite, e) varying temperature on adsorption of RB21 on Fe3O4/SDB nanocomposite, and f) initial dye
concentration on adsorption of RB21 on Fe3O4/SDB nanocomposite.
2316 Nadeem F., et al.

nanoparticles. An increase in pH results in an increase with high coefficient of correlation (R 2) value revealed
in the negatively charged sites, and hence adsorption that the adsorption process obeyed the Freundlich
takes place only at the charcoal surface. So at neutral isotherm model. The Freundlich constants were
pH maximum adsorption took place [33]. determined from the slope and intercept of the linear
The RB21 dye showed an increase in adsorption plot. The values of Freundlich constants, i.e., 1/n, n
with the increase in temperature of the dye solution (adsorption intensity), Kf (adsorption capacity), and R 2
in Fig. 3e). The increase in adsorption along with are given in Table 1.
temperature could be due to enhanced penetration of the
dye. This also symbolizes that the adsorption of the dye Thermodynamic Models
was endothermic. A study by a group of researchers [34]
also describes how such an increase in adsorption could The thermodynamic parameters were determined
be because of the creation of more active sites due to using the following Eqs. 5 and 6 [39] (ΔH° and ΔS°
heat energy. A decrease in removal efficiency was noted were determined from the slope and intercept of the
with the increase in initial RB21 dye concentration, as linear Van’t Hoff plot of lnKeq versus 1/T):
shown in Fig. 3f). The adsorbent has a specific number of
active sites for adsorption. Once the adsorbent becomes ΔG° = -RTlnK (5)
saturated, no further adsorption takes place. In the case
of low dye concentrations, the numbers of binding sites and lnKeq = ΔS°/R - ΔH°/RT (6)
increase, but with increasing dye concentration those
sites fall short and hence adsorption capacity decreases … where ΔHº is enthalpy of adsorption, ΔSº is entropy
[35]. change, ΔGº is Gibbs free energy change, R is the gas
constant, T is absolute temperature, ln is the natural
Adsorption Isotherm Models logarithm, and Keq is the equilibrium constant.
Fig. 4d) shows the linear plots of lnKeq against 1/T.
The Langmuir model [36] was calculated by Eq. 3: The thermodynamic parameters for adsorption of RB
21 on Fe3O4/SDB nanocomposite are given in Table
Ce/ qe = 1/qmax.Ce + 1/KL.qmax (3) 2. The value of Keq increased with temperature while
Gibbs free energy (ΔG°) decreased with increasing
…where qmax is the maximum amount of dye adsorbed temperature. The values obtained for ΔH° and ΔS°
per unit mass of adsorbent, and K L is the Langmuir were positive for adsorption. The negative values for
Constant. A linear plot of Ce/qe against Ce was plotted free energy indicated a spontaneous reaction. Positive
and the values of qmax and K L were obtained using the value for enthalpy suggests the endothermic nature
slope and intercepts of the plot.
The graph of specific sorption (Ce/qe) was plotted
against equilibrium concentration for RB 21 in
Fig. 4a). The linear plot for batch data with high
coefficient of correlation (R 2) value for the dye revealed
that the adsorption process obeyed the Langmuir
isotherm model. The values of Langmuir constants,
i.e., K L, R L, qmax, and R 2 are given in Table 1 for RB 21.
Fig. 4b) shows variation of separation factor R L with
initial dye concentrations for RB 21. We observed
from the graph that the separation factor decreases
and nears zero with the increase in dye concentration.
The value of Langmuir dimensionless separation
factor R L indicated favorable adsorption (0< R L<1) [37]
with a value of 0.04. We used the following equation for
the Freundlich model [38]:

logqe = 1 / nlogCe + log Kf (4)

…where Kf is the Freundlich constant. A linear plot of

log qe against log Ce was plotted and the values of n and
Kf were obtained using the slope and intercepts of the Fig. 4. a) Linear plot of Langmuir isotherm for adsorption of
plot. RB21 on Fe3O4/SDB nanocomposite, b) variation of separation
The linear plot of log of amount adsorbed per amount factor (RL) as a function of initial concentration of RB21, c)
of adsorbent at the equilibrium (log qe) is plotted against linear plot of Freundlich isotherm for adsorption of RB21 on
the logarithm of equilibrium concentration (log Ce) Fe3O4/SDB nanocomposite, and d) graph of lnKeq versus 1/T for
for RB 21 in Fig. 4c). The linear plot for batch data adsorption of RB21.
Synthesizing and Characterizing Sawdust... 2317

Table 1. Adsorption isotherm parameters for RB21 onto Fe3O4/

SDB nanocomposite (bold values are experimental finding
results).
Parameters Value
Model
qmax,exp (mg/g) 25.334
qmax,cal (mg/g) 27.77778
KL (L/mg) 0.150627
Langmuir
RL 0.042383
R2 0.775
N 2.785515
Freundlich Kf 6.251727
R2 0.972

Table 2. Thermodynamic parameters (ΔH°, ΔG°, ΔS°) for the

adsorption of Reactive Blue 21.
Temperature ΔG° ΔH° ΔS°
Keq
(°C) (Jmol-) (Jmol-) (Jmol-K-)
10 510.5637 -14679.1
26 594.0709 -15885.3
30 1291.795 -18055.5 49.027658 221.73 Fig. 5. a) Pseudo first-order sorption kinetics of RB21 on
Fe3O4/SDB nanocomposite, and b) pseudo second-order
50 6378.947 -23537.3 sorption kinetics of RB21 on Fe3O4/SDB nanocomposite.
70 13313.51 -27093.1

Table 3. Kinetic model parameters for the adsorption of RB21

onto Fe3O4/SDB nanocomposite (bold values are experimental
of the adsorption. Also, ΔH° was found to be greater finding results).
than 40 KJ/mol, symbolizing the chemisorption of RB
21 on the adsorbent. Positive values for ΔS° indicated an Parameters Value
Model
increase in randomness during the adsorption process qmax,exp (mg/g) 24.534
[40]. qmax,cal (mg/g) 23.71374
Pseudo-first order K1 (min-1) 0.06445
Kinetic Models
R 2
0.947
The following Eq.7 was used for the pseudo first- qmax,cal (mg/g 27.02703
order mechanism: Pseudo-second
K2 0.00423
order
log (q-qe) = log q – k1t/2.303 (7) R2 0.996

…where q is the amount of dye adsorbed at equilibrium

(mg/g), qe is the amount of dye adsorbed at time t (mg/g),
K 2 is the equilibrium rate constant of pseudo first-order
and K1 is the equilibrium rate constant of pseudo first-
sorption min- 1, and h = k 2q2 – where h is the initial
order sorption (min- 1).
sorption rate and mg g- 1min- 1. A linear plot of log t/qe
A linear plot of log (q-qe) was plotted against time
was plotted against time (t). The values of rate constant
(t). The values of rate constant (K1), coefficient of
(K 2), coefficient of correlation (R 2), and qcalculated were
correlation (R 2), and qcalculated were found using slope and
found using slope and intercept of the graph.
intercept of the graph.
The adsorption rates were calculated using
The following equation was used for the pseudo
pseudo first-order and pseudo second-order kinetics
second order mechanism:
models. The log(q/qe) plotted against time is shown
in Fig. 7a). The linear plot and high coefficient of
t/q = 1/k2qe2 + t/q (8) correlation (0.947) confirms the application of first-order
kinetics. Fig. 7b) shows the plot of t/qe against time.
… where q is the amount of dye adsorbed at equilibrium The linear plot and high coefficient of correlation (0.996)
(mg/g), qe is the amount of dye adsorbed at time t (mg/g), confirms the application of second-order kinetics as
2318 Nadeem F., et al.

well. The value of calculated dye uptake at equilibrium solution on dead floating aquatic macrophyte: effect of pH,
for first-order kinetics is very close to the experimental temperature, and pretreatment. Water Air Soil Pollut. 223
value as opposed to the calculated value of second-order (7), 4369, 2012.
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KIM W., LEE S. The removal of hexavalent chromium
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from aqueous solutions using modified holly sawdust:
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Adsorption Mechanism 4. MAKARCHUK O.V., DONTSOVA T.A., ASTRELIN I.M.
Magnetic nanocomposites as efficient sorption materials
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peaks has increased, indicating a decrease in intensity. on chemical coagulation/flocculation technologies for
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8. PATIL B.N., NAIK D.B., SHRIVASTAVA V.S.
Conclusions Photocatalytic degradation of hazardous Ponceau-S dye
from industrial wastewater using nanosized niobium
It may be concluded that the proposed method pentoxide with carbon. Desalination. 269 (1), 276, 2011.
is a simple and cost-effective way to synthesize 9. FARROKHI M., HOSSEINI S.C., YANG J.K.,
Fe3O4/SDB nanocomposite for the efficient removal SHIRZAD-SIBONI M. Application of ZnO–Fe3O4
of RB21 from textile effluent. 75% color removal was Nanocomposite on the removal of azo dye from aqueous
attained at 90 minutes shaking with adsorbent dose solutions: kinetics and equilibrium studies. Water Air Soil
of 0.25 g and initial dye concentration of 150 mg/L. Pollut. 225 (9), 2113, 2014.
The shaking speed was set at 200 rpm for 30 minutes 10. JAIN R., SHARMA N., RADHAPYARI K.
Electrochemical treatment of pharmaceutical azo dye
at 30ºC and neutral pH. The pseudo first-order and
amaranth from wastewater. J. Appl. Electrochem. 39 (5),
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adsorption process was chemisorption. The negative of basic dye using activated carbon prepared from oil palm
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Fe3O4/SDB nanocomposites can be used for the efficient 13. GUPTA V.K. Application of low-cost adsorbents for
removal of RB21 from wastewater. This research is a dye removal – A review, Journal of Environmental
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Conflict of Interest 2006.
15. THINAKARAN N., PANNEERSELVAM P.,
BASKARALINGAM P., ELANGO D., SIVANESAN S.
The authors declare no conflict of interest. Equilibrium and kinetic studies on the removal of acid
red 114 from aqueous solutions using activated carbons
prepared from seed shells, J Hazard Mater. 158 (1), 142,
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