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Research Article
Synthesis Optimization of Activated Carbon Driven from Scrap
Tire for Adsorbent Yield and Methylene Blue Removal under
Response Surface Methodology
Estifanos Kassahun ,
1
,
2
Solomon Tibebu ,
3
,
4
,
5
Yobsen Tadesse,
2
and Nigist Awish
6
1
Department of Chemical Engineering, College of Biological and Chemical Engineering,
Addis Ababa Science and Technology University, Addis Ababa 16417, Ethiopia
2
Food and Beverage Industry Research and Development Center, Addis Ababa, Ethiopia
3
Department of Environmental Engineering, College of Biological and Chemical Engineering,
Addis Ababa Science and Technology University, Addis Ababa 16417, Ethiopia
4
Sustainable Energy Center of Excellence, Addis Ababa Science and Technology University, Addis Ababa 16417, Ethiopia
5
Bioprocess and Biotechnology Center of Excellence, Addis Ababa Science and Technology University,
Addis Ababa 16417, Ethiopia
6
Ethiopian Conformity Assessment Enterprise, Addis Ababa, Ethiopia
Correspondence should be addressed to Solomon Tibebu; solomon.tibebu@aastu.edu.et
Received 10 May 2022; Revised 15 June 2022; Accepted 6 August 2022; Published 22 August 2022
Academic Editor: Achraf Ghorbal
Copyright ©2022 Estifanos Kassahun et al. is is an open access article distributed under the Creative Commons Attribution
License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is
properly cited.
is study aimed to investigate the synthesis optimization of activated carbon-driven scrap tires for adsorbent yield and methylene
blue removal under response surface methodology. e scrap tire sample was activated by KOH using ethanol as a solvent. e
optimized activated carbon was characterized using proximate analysis, scanning electron microscope (SEM), X-ray diffraction
(XRD), and Brunauer Emmett Teller (BET) method. e activated carbon was demineralized using 5 M NaOH + 98% H
2
SO
4
(1:1) as a solvent to enhance the surface area. Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich models were used to
check the adsorption isotherm. e adsorption kinetics was checked using pseudo-first-order and pseudo-second-order models.
Weber-Morris intraparticle diffusion model was used to study the diffusion mechanism. e optimum impregnation ratio,
impregnation time, and carbonization temperature for synthesizing the activated carbon were 2 g/g, 12 hr, and700°C, respectively.
e moisture content, volatile matter, ash content, fixed carbon, and bulk density of the activated carbon were 6.13%, 9.42%,
5.34%, 79.11%, and 0.89 mg/L, respectively. e surface area of optimized activated carbon was enhanced by demineralization
process and increased from 53 m
2
/g to 260.26 m
2
/g. Temkin adsorption isotherm with R
2
values of 0.982 and pseudo-second-order
adsorption kinetics with R
2
values of 0.999 best fits the experimental data respectively. Intraparticle diffusion was not the only rate-
controlling step for both optimized and demineralized (NaOH + H
2
SO
4
) activated carbon. It can be concluded that the optimized
and demineralized activated carbon derived from scrap tires has a promising potential to be used as a low-cost adsorbent in
developing countries including Ethiopia. However, further investigation needs to be conducted before scaling up at
industrial level.
1. Introduction
Industries including textile, printing, plastic, cosmetic, pa-
per, and food processing industries use dyes [1, 2]. ere are
over 100,000 different types of commercially available dye
throughout the world. According to Fito et al. [3], 700,000
tons of dyes are globally produced per year. During the
manufacturing process, approximately, 15% of the dyestuff
is lost in industrial wastewater [4]. Wastewater that contains
dyes is characterized by low biodegradability and high
Hindawi
Advances in Materials Science and Engineering
Volume 2022, Article ID 2325213, 13 pages
https://doi.org/10.1155/2022/2325213
organic matter concentration [5]. Discharging untreated
wastewater that is contaminated by dye affects the health of
both terrestrial and aquatic environments including soil, al-
gae, fishes, and other living and non-living components of the
environment [6]. Methylene blue is a cationic soluble dye that
dissociates into cations and chloride ions [7]. It has various
applications in dyeing industries, chemistry, biology, and
medical science [8]. Methylene blue contaminated wastewater
has both acute and chronic effects depending on the rate of
exposure and its level of concentration in the wastewater.
Among such acute and chronic effects allergic, dermatitis, skin
irritation, cancer, and mutation are the major ones [9].
According to Patel et al. [10], photosynthesis can be prohibited
by methylene blue dye that has a concentration of less than
1 mg/l. erefore, treating this wastewater is mandatory to
protect the environment from contamination [11].
Different conventional treatment techniques including
physical, chemical, and biological methods have been used
to treat wastewater containing dye contaminants [12].
However, advanced wastewater treatment technologies are
becoming preferable to effectively and efficiently remove
dye from wastewater [13]. Due to its simplicity of design,
ease of operation, high ability to remove different pollut-
ants, and high efficiency, adsorption is preferred to remove
dye over other advanced wastewater treatment technolo-
gies [14].
Among different adsorbents, activated carbon is widely
used to treat water and wastewater [15]. Moreover, activated
carbon is used in air pollution treatment [16]. Commercial
activated carbon is well known for its high surface area and
adsorption capacity. However, these adsorbents are ex-
pensive; therefore, they are not recommended for devel-
oping countries including Ethiopia [17, 18].
To resolve this challenge, research is being conducted by
different scholars in investigating eco-friendly and low-cost
precursors for activated carbon [19, 20]. Peanut shell,
sawdust, bagasse, and bamboo are some of the activated
carbon precursors that have been studied previously [21, 22].
Around 1.5 billion scrap tires per year are disposed of in
the environment [23]. According to Ali et al. [24], in the
coming years, it is expected that 20 million additional scrap
tires will be disposed of per year. Big cities are the main
disposal sites for scrap tires [2]. e main contributors to the
increment of scrap tires are trucks, vehicles, motorcycles,
and bicycles [25]. In developing countries such as Ethiopia,
the amount of scrap tires is expected to increase along with
the increase of vehicles [26]. According to Alamrew [27],
annually, 40,175 tons of scrap tires are generated in Ethiopia.
Scrap tires are causing adverse environmental impacts [28].
Energy recovery through combustion and disposal in
landfills are the two common methods that are being used to
manage this waste [29]. However, these methods have both
environmental and health impacts.
e release of chemicals into the atmosphere is the
main health concern that results from combustion [30].
When they are dumped in landfills, they can also cause a
negative impact on hygiene by being a breeding ground
for mosquitoes and insects [24]. Due to the leaching of
trace metals, sulfur, and zinc, scrap tires can also
contaminate the soil [31]. Scrap tires are not easily bio-
degradable in landfills. e volume that they occupy is also
a major problem in landfills [32].
Instead of landfilling, recycling scrap tires have its own
economic advantage. Scrap tires can be used as part of
construction material due to their physical characteristics
[33]. Ground scrap tires are used for roofing materials,
sports tracks, and noise pollution barriers [32]. According to
Dick et al. [34], pyrolysis is the most recommended method
of recycling waste tires. e three valuable products of waste
tires that are processed through pyrolysis are pyro-oil, pyro-
gas, and pyro-char [35]. Due to its high carbon content,
surface area, and porosity, pyro-char (activated carbon
derived from the waste tire) can be used as an adsorbent for
removing different pollutants from wastewater [24, 36–38].
Increasing the surface area of the activated carbon, which
is derived from scrap tires, is the major problem that is faced
during the preparation process [24]. Demineralization en-
hances the adsorption capacity of the adsorbent by removing
inorganic minerals from the given adsorbent through a
process called leaching [39]. is process increases the
availability of the pours by removing the impurities (inor-
ganic minerals) that blocked the pour structure, which in
turn increases the surface area, micro, and mesopore volume
[39]. Some of the inorganic minerals that are found in waste
tires are iron, silicon dioxide, zinc, calcium, potassium,
magnesium, chromium, manganese, sodium, nickel, and lead
[40]. Moreover, demineralization lowers the ash content and
increases the yield of the activated carbon [41]. Response
surface methodology is one of the most efficient methods that
is used to study and optimize experimental variables [42, 43].
It is used to study and optimize experimental variables. is
methodology has an advantage in terms of evaluating the
controlling effect of each parameter and their interaction by
reducing the number of experiments [44].
Previously, research has been studied regarding the use
of activated carbon derived from scrap tires for the removal
of methylene blue dye from wastewater [2, 38, 45]. However,
it is noted that no research is carried out regarding the
synthesis optimization of activated carbon derived from
scrap tires under response surface methodology. Teng et al.
[46] studied the effect of impregnation ratio, pyrolysis
temperature, and holding time on surface area and yield of
activated carbon derived from scrap tires. However, it is
noted that no research is carried out regarding the de-
mineralization of activated carbon derived from scrap tires
using NaOH + H
2
SO
4
(1 :1) as a demineralizing solvent for
surface area enhancement. erefore, this study aimed to
optimize the synthesis of activated carbon driven from scrap
tires in terms of yield and methylene blue removal.
2. Materials and Methods
2.1. Pretreatment of Scrap Tire. e scrap tires were collected
from a local market, which is located in Addis Ketema sub-
city, Addis Ababa, Ethiopia. ese tires were washed several
times with detergent and tap water to remove dirt and dried
at an ambient temperature 25±1°C. e cleaned tires were
then cut into small pieces by sharp knives. e size of the
2Advances in Materials Science and Engineering
tires was further decreased by a high-speed multifunction
miller (Model HC-700) and sieved to a size of 0.2 mm. e
scrap tires were then washed several times with distilled
water and dried in an oven (Model BOV-T50F) for 5 h at
60°C [47, 48].
2.2. Aqueous Solution Preparation. An aqueous solution of
1 g/L was prepared by adding 1g of methylene blue
(C
16
H
18
N
3
SCl, molecular weight: 319.85g/mol) in a 1 L
volumetric flask. en, distilled water was filled to the mark
of 1 L, and dissolution is performed using a magnetic stirrer.
By using the concept of the dilution process, a different
working solution was prepared.
2.3. Scrap Tire-Driven Activated Carbon (STAC) Synthesis
Optimization. e chemical activation process was con-
ducted in the presence of ethanol as a solvent. irty grams of
the pretreated scrap tire sample was impregnated with KOH
at various impregnation ratios (0–2 g/g) and impregnation
time (12–36 hr). e impregnated sample was dried in an
oven at 105°C. e sample was then pyrolyzed in a muffle
furnace (Model Naberthrem F 330) in an inert environment,
which is created by N
2
gas. Pyrolysis was carried out at
different carbonization temperatures (700–900°C) for 2 hr
[49]. After the activated sample was cooled, it was washed
with 0.1 N HCl in 150 ml solution for 30 min. en, the
activated sample was washed several times with distilled water
until the pH of the supernatant is 7. e activated sample was
then dried in an oven at 105°C for 24 hr.
e synthesis process of the activated carbon was op-
timized by central composite design (CCD) using Minitab
software Version 20.1.3 under response surface methodol-
ogy (RSM). Impregnation ratio, impregnation time, and
carbonization temperature were factors. ese factors were
fixed based on literature values. SCAC Yield and methylene
blue (MB) removal efficiency were response variables.
According to the RSM of CCD, 20 experiments were
conducted at different combinations of the three variables.
e number of experiments was calculated using.
N�2F+2F +x0,(1)
where Nis the number of experimental runs, Frepresents
the factor number, and xo is the number of replicates at the
central point. In this study, Nis 20, Fis 3 and xo is 6.
Of the 20 experiments, 5 experiments were replicated at
center points to evaluate the error. Based on a set of ex-
periments, the range of the variables, step size, and the
central value were chosen as shown in Table 1.
e center points are used to determine the experimental
error and the reproducibility of the data. e axial points are
located at (±α, 0, 0), (0, ±α, 0), and (0, 0, α). α�1.0 (face-
centered) is the distance of the axial point from the center and
makes the design rotatable. e experimental sequence was
randomized to minimize the effect of the uncontrolled factor.
e experimental results were fitted using a polynomial
quadratic equation to correlate the response variables. e
general form of the polynomial quadratic equation shown in
equation (2) was used to develop a model that predicts
(estimates) the STAC yield and MB removal percentage at
the designed variable combination. e model is also used to
predict the individual and interaction effects of different
parameters.
R�βo+
k
i�1
βixi +
k
i�1
βii(xi)2+
k−1
i�1
k
j�i+1
βijxixjε,(2)
where, R�predicted response, β0�constant coefficient,
βi�linear effect coefficients, βii �quadratic effect coefficients,
βiij �interaction effect coefficients, xi �independent variables.
e STAC yield was calculated by equation (3).
Yield �Wac
Wo∗100,(3)
where: Wo(g) is dry weight of the pretreated scrap tire and
Wac (g) is the dry weight of produced STAC.
To determine MB removal, 200 ml of 20 solutions, which
have the same value of pH and initial MB concentration,
were prepared in a 250 ml Erlenmeyer flask. e pH, initial
concentration, adsorbent dose, and contact time were taken
constant for all experiments at 9, 20 mg/L, 0.5 g, and 45 min,
respectively [50]. e adsorption experiment was conducted
at room temperature and at a mixing speed of 125 rpm [3].
e adsorbent was separated from the solution using
Whatman filter paper 42. e final MB concentration was
determined using a UV-visible spectrophotometer (JASCO
V-770) at a wavelength of 668 nm [6].
MB removal efficiency was calculated by equation (4).
Re �Co −Ce
Co
∗100,(4)
where: Re (%) is removal efficiency, Co (mg L
−1
) is the initial
concentration of MB, and Ce (mg L
−1
) is the final MB
concentration.
e optimized STAC is used in characterization, de-
mineralization, isotherm, and kinetics study.
2.4. Characterization of the Activated Carbon. e moisture
content (MC), volatile matter (VM), ash content (AC), and
fixed carbon (FC) of the optimized STAC were determined
according to ASTM standards (D 2866–2869) [18]. e bulk
density of the STAC was determined by the water dis-
placement method.
SEM (Model FEI Inspect F50) was used to determine the
surface morphology of the pretreated sample, before activation
and after adsorption. Standard procedures were followed in
preparing the sample and operating the equipment [51, 52].
Table 1: Selected optimization variables.
Variables (factors) Code
Coded variable
levels
−1 0 1
Carbonization temperature (℃) T 700 800 900
Impregnation ratio (g/g) IR 0 1 2
Impregnation time (hrs.) IT 12 24 36
Advances in Materials Science and Engineering 3
XRD (Model Olympus BTXH) was used at a diffraction
angle of 2ø from 10 to 80°to determine the crystalline and
amorphous nature of the sample after activation and after
adsorption. e XRD was operated at 15 mA and a scanning
rate of 4.2°C/min. e results were analyzed using origin
software Version 9.55 [18].
BETsurface area analyzer (Horiba, SA-9600) was used to
determine the surface area of optimized STAC. e sample
was analyzed by taking 0.4 g of STAC in three vacuum tubes
for 2 h at 100°C [53].
2.5. Demineralization. e optimized STAC was deminer-
alized for enhancing the surface area. e demineralization
process was conducted using a solvent that is prepared by 5M
NaOH + 98% H
2
SO
4
(1:1). 20 g of optimized STAC followed
by 1 L distilled water was added to 16 ml of the demineralization
solvent in Erlenmeyer flask. e mixture was mixed using a hot
plate stirrer (Model P40-HS) at a temperature, mixing speed,
and mixing time of 100°C, 400 rpm, and 3 hr, respectively. en
the demineralized STAC was separated from the solution using
Whatman filter paper 42. e separated demineralized STAC
was then washed thoroughly with distilled water and dried in an
oven at 110°C for 24 hr [39, 54]. e surface area of the
demineralized STAC was analyzed by BET method.
2.6. Adsorption Isotherm. e adsorption isotherm was
studied at room temperature by preparing 200 mL of dif-
ferent initial MB concentrations (100, 120, 140, 150, 170, and
190 mg/L) in a 250 mL Erlenmeyer flask [3]. e pH, ad-
sorbent dose, contact time, and mixing speed were taken
constant at 9, 0.5 g, 45 min, and 125 rpm, respectively.
Langmuir adsorption isotherm assumes monolayer ad-
sorption of adsorbate on the adsorbent surface and ad-
sorption energy is fixed at all points [55]. e linearized form
of Langmuir isotherm model is shown in equation (5).
Ce
qe
�1
qmKl
+Ce
qm
,(5)
qe �co −ce
m×v, (6)
where q
e
and q
m
are the adsorbed amount at equilibrium and
Langmuir maximum adsorption, respectively (mg g
−1
), K
l
is
the constants of Langmuir (L mg
−1
), Vis the adsorbate
volume (L), and mis the mass of adsorbent (g).
R
L
is a dimensionless factor that predicts the appro-
priateness of the adsorption by the constants obtained from
the Langmuir model and calculated using R
L
.
RL�1
1+Kl Co
.(7)
If R
L
>1, the used adsorbent is not appropriate for the
adsorption of the adsorbate. If R
L
�0, adsorption on the
adsorbent will be reversed. If R
L
�1, the isotherm is of linear
type, and if 0 <R
L
<1, the utilized adsorbent is appropriate.
Freundlich isotherm assumes a heterogeneous adsorp-
tion process [56]. e linearized form of Freundlich iso-
therm model is shown in equation (8).
logqe�logKf+1
nlogCe,(8)
where: q
e
is the Equilibrium loading (mg g
−1
), C
e
is the
Equilibrium concentration (mg L
−1
), K
f
is adsorption ca-
pacity ((mg g
−1
) (L mg
−1
)
1/n
), and nis the adsorption in-
tensity. e value of the Freundlich constant (n) should lie in
the range of 1–10 for favorable adsorption, the higher nvalue
the better the adsorption.
Temkin adsorption isotherm assumes that the heat of
adsorption for all molecules decreases with the coverage of
the adsorbent surface [57, 58]. According to Togue Kamga
[59], this model is only valid for a range of intermediate ion
concentrations. e linearized form of Temkin adsorption
isotherm is given by
qe �Rt
b
lnKT +RT
b
lnCe
,(9)
where: bis Temkin constant which is related to the heat
of sorption (J mol
−1
) and KT is Temkin isotherm constant
(L g
−1
).
Dubinin-Radushkevich isotherm is an empirical iso-
therm model that expresses the distribution of Gaussian
energy onto heterogeneous surfaces with an adsorption
mechanism [44]. Since this model does not predict Henry’s
law at low temperatures, it is only suitable for an inter-
mediate range of adsorbate concentration [60]. According to
Boubaker et al. [44], the model states that the adsorption
potential is variable and the free adsorption enthalpy was
related to the degree of pores filling. is model determines
whether the pollutant uptake mechanism is physical or
chemical [42, 61]. e linearized form of Dubinin-
Radushkevich isotherm adsorption isotherm is given by
equation (10).
lnqe �lnqDR max −βϵ2,(10)
ϵ�R∗T∗ln 1+1
Ce
,(11)
where: lnqDRmax is the maximum adsorption capacity of
Dubinin-Radushkevich isotherm (mg g
−1
), βis Dubinin-
Radushkevich constant (mol
2
kJ
−2
), ϵis Polanyi potential, R
is universal gas constant (8.31 Jmol
−1
K
−1
), and Tis absolute
temperature (K).
2.7. Adsorption Kinetics and Intraparticle Diffusion. e
adsorption kinetics and intraparticle diffusion were studied
in 200 ml solution at a fixed value of pH 9, adsorbent dose of
0.5 g, and mixing speed of 125 rpm. e experiments were
carried out at room temperature and at different contact
times (25, 50, 100, 200, 250, and 300 min) in a 250 mL
Erlenmeyer flask [62]. In the solid-solution interface, the
adsorbate removal rate is expressed by adsorption kinetics.
e experimental data were fitted on pseudo-first-order and
pseudo-second-order adsorption kinetics models [63]. e
4Advances in Materials Science and Engineering
integral form of pseudo-first-order and pseudo-second-or-
der equations are expressed in equations (12) and (13),
respectively.
log q−qt
�logqe−K1t
2.303 ,(12)
t
qt
�1
K2q2
e
+t
qe
,(13)
qt �co −ct
m×v, (14)
where qe and qt (both in mg g
−1
) are the amounts of MB
adsorbed at equilibrium and at time t, respectively; K1
(min
−1
) is the rate constant of pseudo-first-order; K2
(g mg
−1
min
−1
) is the rate constant of pseudo-second-order,
V(L) is the volume of the solution, m(g) is the mass of
adsorbent, and t(min) is contact time.
Weber-Morris intraparticle diffusion model was used to
study the diffusion mechanism of MB [63]. e model
equation is expressed in equation (16).
qt �kid ∗t0.5+c, (15)
where k
id
(mg. g
−1
min
0.5
) is the intraparticle diffusion rate
constant and cis a constant number.
3. Results and Discussion
3.1. Synthesis Optimization of Activated Carbon. e syn-
thesis of STAC was optimized by using the impregnation
ratio (IR), impregnation time (IT), and carbonization
temperatures (T) as a factor. STAC yield and MB removal
efficiency were response variables as shown in Table 2.
e maximum STAC yield (68.35%) was obtained at an
impregnation ratio of 2 g/g, impregnation time of 12 hr, and
carbonization temperature of 700°C. e MB removal effi-
ciency at these factors was 89.96%. e maximum MB removal
efficiency (90.48%) was obtained at impregnation ratio, im-
pregnation time, and carbonization temperature of 0 g/g,
12 hr, and 900°C, respectively. e STAC yield at these factors
was 45.33%. e minimum STAC yield (34.03%) was obtained
at impregnation ratio, impregnation time, and carbonization
temperature of 0 g/g, 36 hr, and 900°C, respectively. e
minimum MB removal efficiency (89.18%) was obtained at
impregnation ratio, impregnation time, and carbonization
temperature of 2 g/g, 36 hr, and 800°C, respectively.
e factor values that give relatively both maximum
STAC yield and MB removal are considered optimum factor
values that are used to synthesize STAC. erefore, an
impregnation ratio of 2 g/g, impregnation time of 12hr, and
carbonization temperature of 700 C was taken as optimum
factor values for synthesizing STAC. According to Teng et al.
[46], a higher value of yield is obtained at carbonization
temperature, impregnation ratio, and carbonization time of
500 C, 4, and 1 hr, respectively. Moreover, the maximum
value of BET surface area was obtained at a carbonization
temperature of 700 C, impregnation ratio of 4, and car-
bonization time of 1 hr. e maximum MB removal
efficiency was compared with previous studies as shown in
Table 3.
e effect of carbonization temperature, impregnation
time, and impregnation ratio on STAC yield and MB re-
moval is presented in Figure 1.
As shown in Figures 1(a)–1(c), the STAC yield decreases
with the increment of carbonization temperature. is might
be due to a higher degradation of rubber and other tire
components at an enhanced temperature, which results in
loss of weight [72]. STAC yield decreased with the increment
of Impregnation time. is might be due to the collapse of
pores and a decrease in surface area [73]. Increasing the
impregnation ratio has facilitated the increment of the yield
due to the addition of extra mass to the precursor [74].
As shown in Figures 1(d)–1(f), MB removal decreased as
carbonization temperature increased. is might be due to the
collapse of pores and carbon matrix at high temperatures [75].
MB removal increased with the increment of impregnation
ratio. is might be due to the increment of surface area by
chemical activation [46]. As the impregnation time increased,
the MB removal efficiency decreased continuously. is might
be due to the shrinkage of char structure, widening and
combining of some micropores into mesopores, which de-
creased the adsorption capability of the adsorbent [73].
Due to the sorption capacity and pore structure of the
activated carbon, the MB molecules can be adsorbed on the
surface of the adsorbent [76]. According to Gao et al. [77],
the presence of the micropores present in the activated
carbon and the attraction of the Vander Waals forces are the
main adsorption mechanisms of pollutants.
3.2. ANOVA and Development of Regression Model Equation.
e regression coefficient for STAC yield (R
2
�0.957) and
MB removal (R
2
�0.992) indicates that the quadratic re-
gression model best fits the experimental data for both
Table 2: Optimization of STAC synthesis.
IR (g/g) IT (hr.) T (C°) Yield (%) MB removal (%)
1 24 900 39.98 90.23
0 24 900 34.03 90.21
1 24 700 49.91 89.92
0 12 900 45.56 89.85
1 12 700 54.66 89.56
0 12 900 45.33 90.48
1 24 800 46.68 89.47
0 36 900 44.66 90.46
2 36 800 59.19 89.18
2 12 700 68.35 89.96
1 36 800 52.31 89.41
0 24 800 43.66 89.79
1 24 800 46.67 89.51
1 24 800 43.68 89.53
2 24 800 49.24 89.48
1 24 800 43.69 89.55
1 24 800 48.69 89.58
2 12 700 35.33 90.25
1 36 800 49.67 89.63
2 36 700 38.66 90.31
Advances in Materials Science and Engineering 5
response variables. e Predicted R
2
value of the STAC
yield is 0.872, which is in reasonable agreement with the
adjusted R
2
value of 0.919. For MB removal, the predicted
R
2
value is 0.972 and the adjusted R
2
value is 0.984. is
indicates that the predicted and adjusted value is in sat-
isfactory agreement.
e implication and suitability of the models for both STAC
yield and MB removal were also tested by analysis of variance
(ANOVA) as shown in Table 4. e mean squares were cal-
culated by dividing the sum of the squares of each of the various
sources and the mode and the error variance were calculated by
the respective degrees of freedom. e F-value is the ratio of the
Table 3: Comparison of MB removal efficiency of STAC with other researches.
Adsorbent Removal efficiency (%) Reference
STAC 90.48 is study
Ficus carica bast 85.00 Pathania et al. [64]
Eucalyptus leaves 86.66 Ghosh et al. [65]
Jackfruit leaf powder 85.00 Ahmed et al. [66]
Black tea wastes 75.00 Ullah et al. [67]
TiO
2
/montmorillonite-albumin nanocomposite 84.45 Varmazyar et al. [68]
Parthenium hysterophorus 94.00 Fito et al. [3]
Corn husk 97.30 Khodaie et al. [69]
Rice husk biochar 98.90 Ahmad et al. [70]
Cotton stem biochar 96.28 Wang and Liu [71]
0
10
20
30
40
50
60
70
80
0123
STAC Yield (%)
IR (g/g)
(a)
0
10
20
30
40
50
60
70
80
0 10203040
STAC Yield (%)
IT (hr)
(b)
0
10
20
30
40
50
60
70
80
500 600 700 800 900 1000
STAC Yield (%)
T (C°)
(c)
89
89.2
89.4
89.6
89.8
90
90.2
90.4
90.6
0 0.5 1 1.5 2 2.5
MB (%)
IR (g/g)
(d)
89
89.2
89.4
89.6
89.8
90
90.2
90.4
90.6
0 10203040
MB (%)
IT (hr)
(e)
T (C°)
89
89.2
89.4
89.6
89.8
90
90.2
90.4
90.6
500 600 700 800 900 1000
MB (%)
(f)
Figure 1: Effect of individual factors on STAC yield (a–c) and MB removal (d–f ).
6Advances in Materials Science and Engineering
mean square contributing to regression to the mean square
contributing to error. e greater the F-value, the more is the
significance of the corresponding variable to cause an effect.
As shown in Table 4, the model F-value of 25.18 for
STAC yield and 137.97 for MB removal implies that this
model was significant. e lack of fit F-value of 0.62 for
STAC yield and 0.47 for MB removal implies that the lack of
fit is not significant relative to the pure error. e signifi-
cance of the model is also tested by Pvalue. If the Pvalues of
the model terms are less than 0.05, they are statistically
significant. e ANOVA of the quadratic model for STAC
yield indicates that T, IT, IR, T
2
, IT
2
, and T ∗IR are sta-
tistically significant (P<0.05) but IR
2
, T ∗IT, and IT ∗IR are
not statistically significant (P>0.05). For MB removal, the
model indicates that T, IT, IR, T
2
, IT
2
and T ∗IR, IR
2
, and
IT ∗IR are statistically significant (P<0.05) but T ∗IT is not
statistically significant (P<0.05). e regression model
equation was developed by removing the insignificant model
terms. e model equation that is developed by three factors
or twenty experiments for STAC yield and MB removal is
described in equations (16) and (17), respectively.
Yield(%) � −149.5+0.553T −2.937IT +72.06IR
−0.000356T2+0.03461IT2−0.08051T∗IR,
(16)
MBR(%) � 126.77 −0.08868T −0.0958IT −1.833IR
+0.000052T2−0.000461IT2+0.0836IR2
+0.002250T∗IR −0.01312IT∗IR,
(17)
where: T is Carbonization temperature, IR is Impregnation
ratio, IT is Impregnation time, T ∗IR is the interaction effect
of time and impregnation ratio, IT ∗IR is the interaction
effect of impregnation time and impregnation ratio, MBR is
Methylene blue removal (%) and Y is STAC yield (%).
3.3. e Interaction Effect of Factors on STAC Yield and MB
Removal. Out of the three interaction effects, only one
interaction (T ∗IR) is statistically significant (P<0.05)
for STAC yield and two interactions (T ∗IR and IT ∗IR)
are statistically significant (P<0.05) for MB removal as
shown in Table 4. e three-dimensional response surface
plot of the statistically significant (P<0.05) interaction
effects on STAC yield and MB removal is presented in
Figure 2.
3.4. Characteristics of Optimized Activated Carbon
3.4.1. Proximate Analysis. e MC, VM, AC, FC, and bulk
density of the STAC were 6.13%, 9.42%, 5.34%, 79.11%, and
0.89 mg/L, respectively. e low value of MC, VM, AC, and
the higher value of FC indicates that the STAC has a good
adsorbent characteristic [78].
3.4.2. Scanning Electron Microscope (SEM). e surface
morphology of scrap tires before activation (raw), after
activation, and after adsorption are presented in Figure 3. In
all three SEM micrograph images, a magnification of 10 µm
was used. Compared to the raw scrap tire, the activated scrap
tire shows a highly porous morphological structure with
heterogeneous, irregular, and small pores of various shapes
and sizes. e internal structure of the STAC was irregular
with many gullies and openings. is might be due to the
chemical and thermal activation of the scrap tire [53]. After
adsorption, the number of pours decreased. is might be
due to the adsorption of MB on the internal and external
pore structure of the STAC [79].
3.4.3. X-Ray Diffraction (XRD). e X-ray diffraction of
scrap tires after activation and after adsorption is presented
in Figure 4. e large hill of A, from 2θ�19.56°to 36.56°
corresponding to side spacing 4.5347 ˚
A to 2.4558 ˚
A indicated
the existence of amorphous carbon together with other
crystalline compounds. ese crystalline compounds were
found to be ZnO (zincite) and β-ZnS (wurtzite). Similar
results were reported by Ilnicka et al. [80]; L´
opez et al. [81];
Undri et al. [82]. ZnO (zincite) is the major component of
the scrap tire. However, according to Amirza et al. [83],
Table 4: Response surface quadratic model of ANOVA for MB removal.
Source
STAC yield MB removal
dfSum of
squares Mean square F-value Pvalue dfSum of
squares Mean square F-value Pvalue
Model 9 1131.76 125.751 25.18 0.001 9 2.82914 0.314348 137.97 0.001
T-carbonization temperature 1 382.91 382.913 76.68 0.001 1 0.13225 0.132250 58.05 0.001
IT-impregnation time 1 41.53 41.534 8.32 0.016 1 0.02809 0.028090 12.33 0.006
IR-impregnation ratio 1 79.92 79.919 16.00 0.003 1 0.32761 0.327610 143.79 0.001
T
2
1 34.76 34.763 6.96 0.025 1 0.75404 0.754036 330.96 0.001
IT
2
1 68.33 68.326 13.68 0.004 1 0.01211 0.012111 5.32 0.044
IR
2
1 11.56 11.562 2.32 0.159 1 0.01924 0.019236 8.44 0.016
T∗IT 1 23.22 23.222 4.65 0.056 1 0.28880 0.288800 126.76 0.056
T∗IR 1 518.58 518.581 103.85 0.001 1 0.40500 0.405000 177.76 0.001
IT ∗IR 1 1.04 1.044 0.21 0.657 1 0.19845 0.198450 87.10 0.001
Lack-of-fit 5 19.18 3.836 0.62 0.691 5 0.00723 0.001447 0.4e 0.790
Pure error 5 30.75 6.151 5 0.01555 0.003110
Total 19 1181.69 19 2.85192
Advances in Materials Science and Engineering 7
70
55
40
700 800
T (C°) 900 0
1
IR (g/g)
2
Yield (%)
(a)
90.5
90
89.5
700 800
T (C°)
900 0
1
IR (g/g)
2
MB (%)
(b)
012
IR (g/g) 30
20
IT (hr)
10
96
91
86
MB (%)
(c)
Figure 2: 3D plot of statistically significant interactions (the interaction effect of T and IR on STAC yield (a); Tand IR on MB removal
(b); and IR and IT on MB removal (c)).
(a) (b) (c)
Figure 3: SEM image scrap tire for raw (a), after activation (b), and after adsorption (c).
0 10203040
2 eta (deg)
50 60 70 80 90
Intensity of scarp tire aer activation
Intensity of activated scrap tire aer activation
Figure 4: XRD analysis of scrap tire after activation (black color) and after adsorption (green color).
8Advances in Materials Science and Engineering
while carbonization, the ZnO reacted with sulfur com-
pounds existing in the furnace, creating zinc sulfide in the
crystalline form of β-ZnS (wurtzite). Ali and Alrafai [84] also
reported the conversion of ZnO into ZnS due to desulfur-
ization reaction and the volatilization process.
e peaks labeled as B, C, and D at peak positions of
2θ�29.76°, 49.58°, and 54.56°corresponding to side spacing
2.9996 ˚
A, 1.8371 ˚
A, and 1.6806 ˚
Ashowed the presence of ZnS.
Different peaks labeled at E, F, G, and H with different peak
positions of 2θ�31.34°, 34.1 , 40.86, and 47.3 , corresponding
to side spacing 2.8519 ˚
A, 2.6271 ˚
A, 2.2067 ˚
A, and 1.9202 ˚
A,
respectively. e presence of crystalline structure is indicated
by these high-intensity peaks [85]. On the other hand, similar
peaks were observed by MB adsorbed STAC samples, with the
exception of increased intensity and full width half maximum
(FWHM) values. As 2θvalues increased in the spectra pattern,
the peak intensity decreased, which indicates the presence of
an amorphous carbon arrangement [18].
3.5. Surface Area Study of Optimized and Demineralized
Activated Carbon. A demineralization experiment was
conducted to enhance the surface area of the optimized
STAC. In this study, inorganic minerals such as ZnO were
removed from the pores and polymeric resins of rubber,
which could lead to enhancement of the surface area. e
surface area of optimized STAC was 54.93 m
2
/g. A surface
area of 88 m
2
/g was reported by Jankovsk´
a et al. [86] for
activated carbon driven from scrap tires. e surface area of
optimized STAC that is demineralized by NaOH + H
2
SO
4
was 260.26 m
2
/g. is indicates that the surface area of op-
timized STAC increased due to the demineralization process
[39]. A higher surface area value of 493 m
2
/g was reported by
Ali et al. [24] for activated carbon derived from scrap tires.
3.6. Adsorption Mechanism
3.6.1. Adsorption Isotherm. Langmuir, Freundlich, Temkin,
and Dubinin-Radushkevich adsorption isotherm models
were used to study the adsorption mechanism. Regression
coefficient (R
2
) was used to indicate the isotherm model that
best fits with experimental data. For both optimized and
demineralized STAC, Temkin adsorption isotherm model
with R
2
values of 0.974 and 0.982 best describes the ad-
sorption mechanism as shown in Table 5. is indicates that
the heat of adsorption of all molecules in the layer reduces
linearly [87]. is results from the increase of surface
Table 5: Adsorption isotherm.
Isotherm model Optimized Demineralized
Langmuir
R
2
0.957 0.946
q
m
(mg g
−1
) 73.53 92.59
K
l
(L mg
−1
) 0.130 0.1314
Equation Y�0.0136X+ 0.1043 Y�0.0108X+ 0.0822
Freundlich
R
2
0.956 0.965
N1.675 1.5731
K
f
((mg g
−1
) (L mg
−1
)
1/n
) 10.277 14.692
Equation Y�0.5967X+ 1.0119 Y�0.6357X+ 1.1671
Temkin
R
2
0.974 0.982
b(J mol
−1
) 16.427 19.862
K
T
(L g
−1
) 1.265 1.834
Equation Y�16.43X+ 3.89 Y�19.86X+ 12.05
Dubinin-Radushkevich
R
2
0.972 0.947
qDRmax (mg g
−1
) 99.48 134.29
β(mol
2
kJ
−2
) 1 ∗10
−6
2∗10
−6
Equation Y� −1∗10
−6
X+ 4.60 Y� −2∗10
−6
X+ 4.90
Table 6: Adsorption kinetics and intraparticle diffusion.
Kinetics model Optimized Demineralized
Pseudo-first-order
R
2
0.987 0.842
q
e
(mg g
−1
) 0.016 0.001
K
1
(min
−1
)−0.051 −0.017
Equation Y�0.024X−1.85 Y�0.042X−3.20
Pseudo-second-order
R
2
0.996 0.999
q
e
(mg g
−1
) 11.166 12.976
K
2
( g mg
−1
min
−1
)−0.027 −0.397
Equation Y�13.659X−3.0697 Y�12.715X+ 0.0931
Intraparticle diffusion
R
2
0.912 0.898
C13.017 13.679
K
ID
(mg g
−1
min
0.5
)−0.105 −0.105
Equation Y� −0.105X+ 13.017 Y� −0.105X+ 13.679
Advances in Materials Science and Engineering 9
coverage [57]. Temkin adsorption isotherm also indicates that
up to maximum binding energy, the adsorption is charac-
terized by a uniform distribution of binding energies [61, 88].
3.6.2. Adsorption Kinetics and Intraparticle Diffusion.
e adsorption kinetics of the adsorption process was ex-
amined by pseudo-first-order and pseudo-second-order
models. For both optimized and demineralized STAC,
pseudo-second-order adsorption kinetics model with R
2
values of 0.996, and 0.999 best fits with the experimental data
as shown in Table 6. is indicates that the adsorption
process is controlled by chemical reactions [89]. e dif-
fusion mechanism was studied by the intraparticle diffusion
model. From the linear regression equation, it can be noted
that values of C of both the optimized and demineralized
STAC are not equal to zero. is indicates that intraparticle
diffusion was not the only rate-controlling step [90].
4. Conclusion
e STAC synthesis was optimized using central composite
design under response surface methodology. Impregnation
ratio of 2 g/g, impregnation time of 12 hr, and carbonization
temperature of 700°C was taken as optimum factor values for
synthesizing STAC. e regression coefficient for STAC yield
and MB removal with R
2
values of 0.957 and 0.992 indicates
that the quadratic regression model best fits the experimental
data for both response variables. From ANOVA, it can be
noted that the interaction effect of carbonization temperature
and impregnation ratio on STAC yield is the only significant
(P<0.05) interaction. Moreover, for MB removal, the inter-
action effect of carbonization temperature and impregnation
ratio and the interaction effect of impregnation time and
impregnation ratio is the only significant (P<0.05) interac-
tions. e proximate analysis indicates that the STAC has a
good adsorbent characteristic. e surface area of optimized
STAC was enhanced from 54.93 m
2
/g to 260.26 m
2
/g by the
demineralization process using NaOH + H
2
SO
4
at (1 :1) as a
solvent. Temkin adsorption isotherm with R
2
values of 0.974
and 0.982 best fits with the experimental data for both opti-
mized and demineralized STAC respectively. is indicates
that the heat of adsorption of all molecules in the layer reduces
linearly with coverage. For both optimized and demineralized
STAC, pseudo-second-order adsorption kinetics with R
2
value
of 0.996 and 0.999 best fits the experimental data, respectively.
is indicates that the adsorption process is controlled by
chemical reactions. From the intraparticle diffusion model, it
can be noted that intraparticle diffusion was not the only rate-
controlling step for both optimized and demineralized STAC.
Generally, it can be concluded that the optimized STAC that is
demineralized by NaOH + H
2
SO
4
solvent has a promising
potential to be used as a low-cost adsorbent in developing
countries including Ethiopia. However, further investigation
needs to be conducted before scaling up at the industrial level.
Data Availability
All the data used to support the findings of this study are
included in the article.
Conflicts of Interest
e authors declare that they have no conflicts of interest.
Acknowledgments
is study was financially supported by Addis Ababa Science
and Technology University.
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