Banana stem based activated carbon as a low-cost adsorbent for methylene blue removal: Isotherm, kinetics, and reusability
Erni Misran
*, Okta Bani, Elfrida Margaretha Situmeang, Adelina Suciani Purba
Department of Chemical Engineering, Universitas Sumatera Utara, Jl. Almamater Kampus USU, Padang Bulan, Medan 20155, Indonesia
Received 7 April 2021; revised 13 June 2021; accepted 9 July 2021
KEYWORDS Banana stem waste;
H3PO4activator;
Pyrolysis;
Activated carbon;
Cationic dye;
Adsorption
Abstract A low-cost activated carbon from the banana stem (ACBS) was produced to contribute to environmental preservation in removing methylene blue from wastewater. It is originated from abundant agricultural waste and produced at moderate pyrolysis temperature and short pyrolisis time. In the ACBS production, the banana stem was impregnated with H3PO4solution as the acti- vating agent and followed by pyrolysis at 400°C for a rapid time of 15 min. The treatment signif- icantly improved the ACBS surface area to 837.453 m2/g. The influence of the ACBS dose and initial concentration of dye solution at various contact times were investigated in this study. The utilization of ACBS in low doses exhibited high removal efficiency of methylene blue (0.05 to 0.3 g/100 mL). It can remove methylene blue completely in 90 min of adsorption with an initial con- centration of 50 g/mL. High removal efficiencies are still also demonstrated at higher initial concen- trations with 99.762% removal for the initial concentration of 200 g/mL. Equilibrium adsorption data had the best agreement to the Freundlich isotherm model and pseudo-second-order kinetics model. It is predicted that ACBS has a maximum adsorption capacity of 101.01 mg/g. ACBS is an environmentally benign and favorable adsorbent in methylene blue removal and also effective for repeated usage up to 6 consecutive times with no desorption step.
Ó2021 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria University. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).
1. Introduction
Dyes are the most plentiful of water pollutants. One of the remarkable organic dyes is methylene blue that has wide appli-
cation in textile, chemical indicators, dyeing, printing, pesti- cide, coating for paper stock, cosmetics, and pharmaceutical products [1–3]. In medical applications, methylene blue also plays an important role in treating various illnesses and disor- ders[4].
Methylene blue, C16H18ClN3S (Fig. 1), is an important aro- matic compound. However, due to its aromatic ring, methy- lene blue is extremely toxic, carcinogenic and its degradation
* Corresponding author.
E-mail address:[email protected](E. Misran).
Peer review under responsibility of Faculty of Engineering, Alexandria University.
H O S T E D BY
Alexandria University
Alexandria Engineering Journal
www.elsevier.com/locate/aej www.sciencedirect.com
https://doi.org/10.1016/j.aej.2021.07.022
1110-0168Ó2021 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Please cite this article in press as: E. Misran et al., Banana stem based activated carbon as a low-cost adsorbent for methylene blue removal: Isotherm, kinetics, and reusability, Alexandria Eng. J. (2021),https://doi.org/10.1016/j.aej.2021.07.022
Previous studies have suggested various methods for removing dye-stuffs from wastewater. The methods are elec- trochemical degradation [9,10], photocatalytic degradation [11–16], nanofiltration [17], irradiation [18], adsorption [19–
25], and biological treatments[26,27]. To date, the adsorption shows an effective technology in dyes removal, based on its ini- tial and equipment cost, ease of operation, simplicity of design, required land area (only needs half to a quarter compared to a biological system), and the adsorbent regeneration [28]. The ability in preventing the appearance of secondary pollutants via oxidation or degradation of dye material is another advan- tage of adsorption[29,30].
The utilization of activated carbons as adsorbent is widely found in several applications including dye removal consider- ing its porosity and high specific surface area[19]. Various pre- cursors have been used from natural sources such as biomass and biowaste from agricultural, animal, or industrial waste [19–25]. Activated carbon is produced through two main pro- cesses namely carbonization or pyrolysis and activation (phys- ically or chemically). Some efforts are also performed by modifying activated carbon using clay [31], metal [32,33], and metal oxide[16,17,34–38].
The production of activated carbon from natural precur- sors is very attractive considering its availability and simple procedure. One of the promising activated carbon precursors is banana stem waste that exists abundantly especially in Indonesia. Banana stem is a lignocellulosic material that com- prises cellulose, hemicellulose, and lignin of 43.3%, 20.6%, and 27.8% respectively[20]. Banana production in Indonesia was 7.28 million tons in 2019 with increasing growth of 0.22% compared to 2018[39]. Banana harvesting leaves a huge amount of waste, with the largest portion is the banana stem (60%), whereas 30% is fruit and the rest is leaf from the total production[40].
To the best of our knowledge, the utilization of activated carbon from the banana stem (ACBS) that is produced via pyrolysis at moderate temperature and short pyrolysis time to remove methylene blue solution has not been reported yet. In previous studies, pyrolysis was always performed in high temperature and longer time: 400–500 °C[25], 600 °C for 1 h [19], 700 °C for 1 h [23], and 400–900 °C for 30–
120 min with the best result was achieved with condition of 900°C for 30 min[21].
In this study, the properties of methylene blue removal using ACBS in various adsorbent doses and initial concentra- tions of methylene blue solution for a serial contact time were investigated. The adsorption parameters of isotherm and kinetics models were also presented. The reusability of the ACBS by applying it in sequential methylene blue removal
dered. The powders that pass through the 32 mesh sieve was impregnated overnight with H3PO4 solution. Pyrolysis was conducted in a reactor with nitrogen (N2) flow at 400°C for 15 min. The ACBS was washed up until the pH solution was neutral. Finally, the dried ACBS was placed in a vacuum des- iccator until it was characterized or used in adsorption. The schematic route of the ACBS preparation is shown inFig. 2.
2.2. Characterization of activated carbon
The surface image of the ACBS morphology was detected by SEM (scanning electron microscopy) (JED-2300, JEOL). The FTIR (Fourier transform infrared spectroscopy) (Prestige 21 Shimadzu, Japan) was applied to investigate the presence of functional groups in the ACBS. The BET (Brunauer- Emmett-Teller) surface area was examined using BET surface analyzer (Quantachrome Instruments version 11.03) through the adsorption/desorption isotherms of N2 conducted at 77 K. The morphology, functional groups, and BET surface area of dried BS powder and ACBS after the adsorption pro- cess were also examined as a comparison.
2.3. Methylene blue adsorption
The experiments were conducted in batch mode using 100 mL methylene blue solution at neutral pH. Our previous study on pH influence found that the best performance of the ACBS in removing methylene blue was at pH = 7 and room tempera- ture [43]. The influences of adsorbent dose m (0.05, 0.1, 0.2, 0.3 g in 100 mL dye solution), initial concentration C0 (25, 50, 100, 150, 200 mg/L), and contact timet(2 – 90 min) were investigated. After adding a certain dosage of adsorbent, the mixture with knownC0was shaken at 100 rpm for a certaint.
The influence of adsorbent doses was examined by adding a series of different dosesmof ACBS into methylene blue solu- tion withC0of 50 mg/L for a contact time of 90 min. To study the initial concentration effect, methylene blue solution with a series of initial concentrationsC0was contacted with 0.2 g of ACBS for 90 min. To study the adsorption kinetics, 0.2 g of ACBS was mixed with methylene blue solution at C0 of 50 mg/L. Sampling was carried out at certain time intervals in 2–90 min.
The methylene blue concentration at a certain contact time (Ct) was determined using a UV–VIS spectrophotometer (Shi- madzu 1800, Japan). Eqs.(1) and (2)were used to calculate the removal efficiency (R) of methylene blue and adsorption capacity (qt, mg/g) respectively:
R¼C0 -Ct
C0 ð1Þ
qt¼C0 -Ct
m V ð2Þ
C0andCtare the concentration of methylene blue at initial and at a contact time oft(mg/L) respectively;Vis the solution volume (L), andmis the weight of ACBS (g).
2.4. Isotherm study
Batch experimental adsorption data at various C0 were uti- lized to investigate the isotherm parameters of the Langmuir and Freundlich model. The mathematical equation in non- linear form and linearized form are described in Eqs.(3) and (4)for Langmuir model:
qe¼ qmKLCe 1þKLCe
ð3Þ
Ce
qe ¼ 1
qmCeþ 1
KLqm ð4Þ
Meanwhile, the mathematical equation in non-linear form and linearized form are described in Eqs.(5) and (6)for Fre- undlich model:
qe¼KFCe1=n ð5Þ
log qe¼logKFþ1 nlogC
e ð6Þ
For the Eqs. (3)–(6),qe is the amount of methylene blue adsorbed per unit mass of ACBS at equilibrium (mg/g);qmis the maximum amount of methylene blue adsorbed per unit mass of adsorbent at complete monolayer on the surface- bound (mg/g); Ce is the concentration of methylene blue in solution at equilibrium (mg/L);KL is a constant concerning the affinity of the binding sites (L/mg); KF is a Freundlich adsorption constant concerning the adsorption capacity of the ACBS ((mg/g) (L/mg)1/n); and 1/n is the intensity of adsorption.
2.5. Kinetics study
Adsorption data at various t were employed to predict the kinetics parameter by applying pseudo-first-order (PFO) and
pseudo-second-order (PSO) kinetics model. The linearized forms of the models are described in Eqs. (7) and (8) respectively:
logðqeqtÞ¼logqe K1t
2:303 ð7Þ
t qt¼ 1
K2q2eþ 1
qmt ð8Þ
where K1 is the PFO and K2 is the PSO adsorption rate constant.
2.6. Reusability
To examine the reusability of ACBS, a set of adsorption exper- iments was conducted using the same ACBS repeatedly. Ini- tially, we prepared some solutions of methylene blue (100 mL each) withC0of 50 mg/L and 0.2 g of ACBS. The first solution was mixed with the ACBS for 90 min and then the solution was filtered. The methylene blue concentration in the filtrate was examined using a UV–VIS spectrophotometer, then the removal efficiency was obtained by applying Eq.(1).
Whereas the residue, the ACBS that has adsorbed methylene blue in the first solution, was further mixed with the second solution of methylene blue as prepared previously. The residue of ACBS was utilized directly, without the desorption step.
The same process was repeated until eight times of consecutive use.
3. Results and discussion
3.1. Characteristics of ACBS 3.1.1. Morphology
The surface morphology of BS powder, ACBS before adsorp- tion, and ACBS after adsorption were acquired using SEM (Fig. 3). The surface image of BS powder is uniform with no pore (Fig. 3a). The activation and pyrolysis process has suc- cessfully promoted the porous structure in ACBS that gave a great contribution to its surface area. As inFig. 3b, a signifi- cant increase in pore numbers is detected on the adsorbent sur- faces before adsorption. The pores are heterogeneous in sizes and shapes with a rough surface. This surface morphology gives a great advantage because it is able to furnish more sites for adsorbates binding. Furthermore, the adsorbent surface Fig. 2 The schematic route of the ACBS preparation.
has changed significantly after the methylene blue adsorption (Fig. 3c). It is observed that the pores have diminished because of the adsorption process.
3.1.2. Functional group
The FTIR results show the presence of some functional groups of the BS powder and ACBS before and after adsorption (Fig. 4). For BS powder (Fig. 4a), the presence of –OH (3371.57 cm1), C-H (2927.94 cm1), C = O (1624.06 cm1), C = C (1373.32 cm1), C-N (1323.17 cm1), and C-O (1246.02 and 1049.28 cm1) are observed. While for ACBS before adsorption (Fig. 4b), absorbed wave numbers that cause the peaks of the formed functional groups were also shifted, hence the presence of O-H (3437.15 cm1), C = O (1593.20 cm1), and C-O (1195.87 cm1) groups is notable.
This indicates that the activator has broken the hydrocarbon bond thus causing the change in activated carbon. Moreover, the peak of aliphatic C-H disappeared in ACBS that might be caused by the pyrolysis process as found in[44,45]. Here, the presence of O-H and C = O groups on ACBS is an advan- tage. Those groups conduce the acidic and basic characteristics to ACBS thus enable it to adsorb cationic and anionic dye molecule[46].
Furthermore, the FTIR spectrum for ACBS after adsorp- tion shows some functional groups originated from methylene blue (Fig. 4c). Some new peaks indicated the form of N-H (975.98 cm1), C-S (725.23 cm1), and C = C
(1597.06 cm1) that are chromophores of methylene blue.
The existence of these functional groups could be used as evi- dence that methylene blue dye was adsorbed onto ACBS. A decrease in peak heights and a shift of peak position also approves that the adsorbent and the adsorbate had a strong interaction.
3.1.3. Surface area
BET measurement results (Table 1) show the characteristics of BS powder and ACBS. The surface area increased significantly in ACBS compared to BS powder. The activation and pyroly- sis process has successfully removed the ash and impurities in BS thus enlarging the pores in ACBS. Pyrolysis causes the loss of volatile components which promotes pore formation. More- over, the destruction of aliphatic groups may also increase sur- face area[47], as observed from the FTIR result in this study.
The high surface area of ACBS will provide sufficient active sites for dye adsorption. However, the surface area of ACBS decreases after adsorption because the dye molecules are adsorbed on the ACBS surface thus covered the pores. Hence, the pore volume also decreases.
Fig. 5represents the pore size distribution profiles based on Barrett-Joyner-Halenda (BJH) model. The radius of the pore is 75.61 nm, 2.14 nm, and 3.86 nm for BS powder, ACBS before adsorption, and ACBS after adsorption, respectively. The decrease of the pore radius is in accordance with the increase surface area of the produced ACBS from the activation and Fig. 3 SEM visualization of (a) banana stem powder, (b) activated carbon from the banana stem before adsorption, and (c) activated carbon from banana stem after adsorption.
pyrolysis step. Meanwhile, after the adsorption, the pore size increases due to the pore being filled by dye molecules.
3.2. Performance of banana stem activated carbon 3.2.1. Effect of adsorbent dose
The effect of adsorbent doses (0.05 to 0.3 g in 100 mL dye solu- tion) was studied usingC0of 50 mg/L at various adsorption contact times (Fig. 6). The more adsorbent dose the higher the removal efficiency and adsorption capacity as contact time increases. The removal efficiency of methylene blue onto ACBS is very high in a short contact time.
The removal is very fast at the beginning (for about 10 min) and afterward gradually decreases until the equilibrium is attained. The very rapid removal of the methylene blue at the beginning is probably attributed to the great number of vacant sites available. The usage of 0.1 g adsorbent can achieve 95.26% removal in 10 min. At 90 min of adsorption, the
methylene blue can be removed perfectly for all adsorbent doses under study.
3.2.2. Effect of initial concentration
ACBS shows high removal efficiency in adsorption of methy- lene blue dye at the varied initial concentrations (25–200 mg/
L), viz. minimal 99.76%. The removal efficiency decreases with the increasing concentration of the dye solution. The highest capacity of 99.76 mg/g is acquired at 200 mg/L of dye solution.
These results are illustrated inFig. 7and will be used to get the suitable isotherm adsorption model.
3.3. Isotherm model
The Langmuir and Freundlich models were utilized to study isotherm adsorption. The comparison of both model parame- ters is presented inTable 2. In deciding which model could best explain the adsorption at equilibrium, so the values of correla- tion coefficient (R2) and root-mean-square-errors (RMSE) can be used as the indicators [48]. Both models show a high R2. However, R2 is not adequate to depict the applicability of the models to the experimental data. Hence, a comparison between the calculated adsorption capacities at equilibrium (qe) from the applied models and the experimental values is exhibited. As a result, the Freundlich isotherm model is the more appropriate model for this study since it demonstrates better agreement with the experimental data (Fig. 8). The Fig. 4 FTIR spectra of (a) banana stem powder, (b) activated carbon from the banana stem before adsorption, and (c) activated carbon from banana stem after adsorption.
Table 1 Pore characteristics based on BET analysis.
Material Surface area (m2/g) Pore Volume (cc/g)
Banana stem powder 10.483 0.023
ACBS before adsorption 837.453 0.437
ACBS after adsorption 828.110 0.423
SSE and RMSE values of the Freundlich model are lower than that of the Langmuir model. Thence, the interaction between the adsorbed molecules and ACBS is carried on multilayer adsorption over a heterogeneous surface as assumed by the Freundlich model[44]. This result is also mentioned in previ- ous works[44,49]. Both studies concluded that the Freundlich model describes the methylene blue removal better than the Langmuir model.
The constant n in the Freundlich model identifies the adsorption intensity. Its classification is:n> 1 (physical pro- cess);n< 1 (chemical process);n= 1 (linear). In adsorption, n> 1 is the most common condition and annvalue between 1 and 10 indicates the desired adsorption[50]. Likewise, the1/
n= 0.1 to 0.5 (adsorption process is excellent):1/n= 0.5 to 1 (process is easy to adsorb): 1/n 1 (process is difficult to adsorb)[25]. In this study, the value ofnis 6.25 which exhibits that methylene blue removal is a physical process and included in good adsorption. Whereas,1/nvalue is 0.16 which confirms that the dye adsorption onto ACBS was favorable and showed excellent performance at various conditions under study.
Theqmin the Langmuir model is the maximum amount of adsorbate per unit mass of adsorbent. Adsorption capacity is a key parameter to appraise the adsorption influence of adsor- bents [3]. The maximum adsorption capacity of ACBS is 101.01 mg/g.Table 3presents a comparison of the maximum adsorption capacity values of various adsorbents. The list reveals that ACBS is a promising adsorbent for methylene blue.
3.4. Kinetics model
To get an appropriate kinetics model, it is necessary to analyze the concentration of dye solution at various contact times. The parameters of PFO and PSO kinetics models are summarized inTable 4. The values ofR2, SSE, and RMSE are also the indi- cators in deciding the most accurate model that describes the kinetics process of adsorption [48]. From the table, the PSO kinetics model described the data well with higherR2than that of the PFO kinetics model. Based on the SSE and RMSE, the PSO kinetics model also shows excellent agreement with the experimental data (Fig. 9). Moreover, the adsorption rate con- stant K2 is higher than K1 indicating that methylene blue removal was faster (K2 = 0.41 g/mg.min) as (K1 = 0.013/
min). These results confirm the adsorption rate-determining step is the diffusion of methylene blue onto the pores of the ACBS and chemisorptions. Some studies also demonstrates that methylene blue adsorption obeys the PSO kinetics model [8,28,44,49,60,61].
3.5. Reusability and potential application
The result reveals that the ACBS shows excellent performance until the fourth consecutive use with a high removal efficiency of 99.712%. The removal efficiency decreased slightly until the sixth consecutive use (96.479%) and decreased dramatically at (a)
(b)
(c) 0.00
0.10 0.20 0.30 0.40 0.50 0.60
0 20 40 60 80 100 120 140
dV(log r) [cc/g]
Pore radius (nm)
0.00 0.10 0.20 0.30 0.40 0.50 0.60
0 20 40 60 80 100 120 140
dV(log r) [cc/g]
Pore radius (nm)
Fig. 5 Pore size distribution of (a) banana stem powder, (b) activated carbon from the banana stem before adsorption, and (c) activated carbon from the banana stem after adsorption.
Fig. 6 Removal efficiency of methylene blue onto ACBS (initial concentration = 50 mg/L, dye solution volume = 100 mL, ambient temperature, contact time = 90 min) at various adsor- bent doses.
the eighth consecutive use (45.051%). This reusability profile can be found out inFig. 10. Other studies always performed desorption step in each cycle of their reusability test, which uses methanol[8], HNO3[49], or NaOH[60,62]as elution sol- vent. Since ACBS exhibits high removal efficiency without des- orption step in reusability tests, so there is no doubt that ACBS is a promising adsorbent for methylene blue adsorption.
The adsorbent reusability is an important feature for deter- mining its commercial viability for industrial application. The availability of abundant banana stems as activated carbon pre- cursor is another main factor in ensuring the continuity of ACBS production. Besides, a simple method is used in its pro- duction. In the next step, another study will be conducted to predict the required adsorbent amount at a target removal effi- ciency and the actual initial concentration of industrial waste containing methylene blue using the adsorption isotherm equa- tions combined with the mass balance equation. Hence, the utilization of ACBS in the industrial application can be realized.
4. Conclusions
Activated carbon developed by lignocellulosic waste: banana stem shows promising performance for methylene blue removal. It has a high surface area and pore volume that pro- vides sufficient active sites for dye molecules. The porous struc- ture of ACBS is confirmed by SEM images. Batch mode experiments were performed to examine the influences of Fig. 7 Effect of initial concentration on removal efficiency of methylene blue and adsorption capacity (adsorbent dose = 0.2 g in 100 mL solution, ambient temperature, contact time = 90 min).
Table 2 Langmuir and Freundlich isotherm parameters of methylene blue adsorption onto ACBS.
Isotherm Model Parameter Value R2 SSE RMSE
Langmuir qm(mg/g)
KL(L/mg)
101.01 123.75
0.9980 961.774 15.506
Freundlich KF(mg/g).(L/mg)1/n n
111.20 6.25
0.9977 47.479 3.445
0 20 40 60 80 100 120
0 0.1 0.2 0.3 0.4 0.5
qe (mg/g)
Ce (mg/L)
Experiment Langmuir Freundlich
Fig. 8 Isotherm Model.
Table 3 The maximum adsorption capacity of the various adsorbents.
Adsorbent Source qm(mg/
g)
Ref Olive stone activated carbon 4.8–12.4 [21]
Wood waste activated carbon 4.94 [22]
Hickory biochars 12–16 [51]
Municipal solid wastes activated biochar 21.83 [52]
Biochar from liquefaction of rice husk 32.5–
67.6
[53]
Apricot stone activated carbon 36.68 [23]
Oxidized multiwalled carbon nanotube (OMWCNT)
46.36 [54]
Nano-magnetite-heulandite cross-linked chitosan
45 [55]
Ficus caricabast activated carbon 47.62 [24]
Alumina-zirconia (Al2O3–ZrO2) composite 53.44 [56]
Carbon nanotubes 64.7 [57]
Microwave-assisted corncob activated carbon
82.71 [25]
Weeds activated biochar 92.59 [58]
ZnO-nano rods-activated carbon 89.29 [59]
Banana stem activated carbon 101.01 This work
adsorption variables. The usage of a low adsorbent dose (0.05 to 0.3 g adsorbent in 100 mL with the initial concentration of 50 g/mL) can remove methylene blue with high efficiencies.
The usage of 0.1 g adsorbent can achieve 95.26% removal in 10 min. At 90 min of adsorption, the methylene blue can be removed perfectly for all adsorbent doses under study. High removal efficiencies are still also demonstrated at higher initial concentrations with 99.762% removal for the initial concentra- tion of 200 g/mL. The adsorption process obeys the Freundlich isotherm model and shows wonderful intensity since the1/n value is 0.16. It is predicted that ACBS has a maximum adsorption capacity of 101.01 mg/g obtained from the Lang- muir model which is higher than some other adsorbents. The adsorption rate-determining step is the diffusion of methylene blue molecules onto the ACBS since the kinetic behavior is described better by the pseudo-second-order kinetic model.
Furthermore, the ACBS can be used effectively in a sequential adsorption process with removal efficiency above 96% without
sor for activated carbon preparation that exhibits superior per- formance in methylene blue adsorption. Hence, ACBS definitely becomes an alternative promising adsorbent.
Declaration of Competing Interest
The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Acknowledgment
We thank Lembaga Penelitian of Universitas Sumatera Utara for the TALENTA Research Grant, Fiscal Year of 2017, Con- tract No. 5338/UN5.1.R/PPM/2017, 22ndMay 2017.
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