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Inorganic Chemistry Communications: Rasha A. Al-Husseiny, Shahlaa E. Ebrahim
Inorganic Chemistry Communications: Rasha A. Al-Husseiny, Shahlaa E. Ebrahim
Short communication
A R T I C L E I N F O A B S T R A C T
Keywords: In this work magnetite/geopolymer composite (MGP) was synthesized using a chemical co-precipitation tech
Geopolymer nique. The synthesized materials were characterized using several techniques such as: “X-ray diffraction (XRD),
Methylene blue Fourier- transform infrared spectroscopy (FTIR), vibrating sample- magnetometer (VSM), field-emission scanning
Fe3O4
electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), Brunauer–Emmett–Teller (BET) and
Adsorption capacity
Barrentt-Joyner-Halenda(BJH)” to analysis the structure and morphology of the geopolymer and the obtained
Kaolin
Artificial neural network composite. The analysis indicated that metal oxide predominantly appeared at the shape of the spinel structure of
magnetite, and that the presence of nano-magnetite had a substantial impact on the surface area and pore
structure of the geopolymer. Methylene blue adsorption on the MGC was investigated. The specific surface area
of the geopolymer and Fe3O4/geopolymer composite was determined to be 26.604 m2/g and 69.04 m2/g,
respectively. It was revealed that a mixture of Fe3O4 and geopolymer with percent 10% magnetite to geopolymer
had high adsorption performance on MB, with a removal rate of over 95%, which was much greater than that of
separate mesoporous geopolymers. The synthesized nanocomposites as promising adsorbents have a potential
application in the removal of dyes from aqueous solution. Langmuir and Frendulich isotherm models were used
to analyze the equilibrium data, the Frendulich model revealing a strong correlation coefficient. The kinetic
process’s results were in accordance with the pseudo-second-order model. Fluidization of mass was used to
demonstrate dye breakthrough curves under the influence of various operating conditions, and the actual results
fitted with the predicted data produced using an artificial neural network(ANN).
1. Introduction environment have been developed and evaluated in recent years, such as
coagulation [4], advanced oxidation [5], ultrafiltration [6],ion-ex
The release of many dyes and pigments into the aquatic environment change [7], electrochemical treatment [8], photocatalytic degradation
as a result of rapid industrial expansion has made wastewater treatment [9], and adsorption [10,11]. Adsorption is a popular approach among
a difficult issue in environmental sciences. Water pollution produced by physicochemical processes because of its low cost, simple design, and
dyes has developed as a result of their widespread usage in fields such as reusability [12].As a result, dye removal has been explored using ab
textiles, leather, chemicals, petroleum products, paper, cotton, wool, sorbents with various geometries and chemical compositions [13]. The
plastic, and pharmaceuticals, attracting the attention of the scientific study is concentrating on less expensive and “greener” options. Geo
community [1,2,3]. Methylene blue (MB) is a basic dyestuff widely polymers have gotten a lot of attention because of their numerous
utilized in different sectors and is one of the most frequently used in interesting characteristics, including ionic exchange, and the environ
dustrial dyes. As a result, for both environmental protection and the mentally friendly aspect of their manufacturing method [14]. Geo
reuse of these unconventional waters necessitate the treatment of water polymers are networks or chains of mineral molecules linked by
polluted by these compounds. Various strategies for recovering haz covalent connections. It is made by reacting an alkaline liquid with a
ardous chemicals from effluent before releasing them into the aquatic geologically derived substance such as kaolin (metakaoline) [14,15],
* Corresponding author.
E-mail addresses: rasha83@wrec.uoqasim.edu.iq (R.A. Al-husseiny), shahlaa.ebrahim@coeng.uobaghdad.edu.iq (S.E. Ebrahim).
https://doi.org/10.1016/j.inoche.2022.109318
Received 22 December 2021; Received in revised form 10 February 2022; Accepted 15 February 2022
Available online 18 February 2022
1387-7003/© 2022 Elsevier B.V. All rights reserved.
R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
2.5. Isothermal equilibrium experimentations filtered and examined. After repeating the process at 400, 600, and
1000 rpm, the concentration time decay curves were produced by
Various weights of MGP (0.0.25, 0.05, 0.1, 0.15, 0.2, 0.25, 0.3, 0.35, plotting the Ce/Co vs. time.
and 0.4) g were utilized in, 100 ml volumetric hipflasks.Methylene blue
solution with a concentration of 50 mg/L were prepared, and each 2.6.1. Adsorption kinetics models
hipflask received 50 ml of the solution. 0.1 M sodium hydroxide (NaOH)
or hydraulic acid (HCL) were used to adjust the pH of solutions to the 2.6.1.1. Pseudo-first-order kinetic model. This model may be expressed
desired value.A shaker set at 200 rpm was used to agitate the mixture with reliability using the Lagergren equation. It describes how the MB
constantly for 2 h. Centrifuge were used to filter each sample. A UV adsorps MGP kinetically [34]. The following equation represents the
spectrophotometer was used to quantify the ultimate equilibrium con model [35]:
centrations. The equilibrium MB uptake (qe, mg/g) and removing effi
dq
ciency (%) were estimated using Eqs. (1) and (2), respectively [31,32]. = k1 (qe − qt ) (5)
dt
V(Co − Ce)
qe = (1) where qt (mg/g) and qe (mg/g) are the solute amounts adsorbed at
W any given time t (min) and equilibrium, respectively. The pseudo-first
Co − Ce order rate constant is k1 (min− 1). Take integration of.Eq. (2), depend
Removalefficiency% = 100( (2) ing on the boundary conditions of qt = 0 at t = 0 and qt = qt at t = t, the
Co
equation becomes Eqn 6 [35]:
Where, Co and Ce (mg/L) are the beginning and final MB concen
trations, respectively; VL is the volume of the solution, and W (g) is the ln(qe − qt) = lnqe − (K1 t) (6)
weight of the adsorbent utilized. To find the isotherm constants, the A plotting graph of ln (qe – qt) versus t can yield the slope (k1) and
collected data was fitted using two models.. The Langmuir equation can intercept (log qe). The equilibrium MB solute uptake (qe) and first order
be expressed as followsEqn 3: kinetic constant (k1) can eventually be determined.
qm *KL *Ce
qe = (3) 2.6.1.2. Pseudo-second-order kinetic model. The pseudo second-order
1 + KL *Ce
model is represented by the equation below. As illustrated below in
Where qe is the solid-phase equilibrium concentration (mg/g), Ce is
Eqn 7, the mass transfer of driving force, (qe - qt), is proportional to the
the MB liquid equilibrium concentration in solusion (mg/l), KL is the
number of unoccupied sites. [36]:
equilibrium constant associated to binding site affinity (l/mg), and qm is
the maximum quantity of MB per unit weight of adsorbent for full sur dq
= k2 (qe − qt )2 (7)
face coverage. Adsorption on a heterogeneous surface with varying dt
adsorption energies is explained by the Freundlich isotherm. The Taking integration of Eq. (4) whilst considering boundary conditions
Freundlich constant KF represents the change in adsorption energy with of qt = 0 at t = 0 and qt = qt at t = t, the equation converts to Eqn 8:
surface coverage (qe) in Eq. (4).[33]
1 1
= + k2 t (8)
qe = KF Ce1/n (4) (qe − qt ) qe
Where KF is a rough estimate of adsorption capacity. where k2 is a second-order rate constant. To illustrate a linear rela
tionship, rearrange Eq. (5) as follows in Eqn 9:
2.6. Kinetic experiments
t 1 t
=( 2+ ) (9)
qt k2 qe qe
The adsorbent type is used in a kinetic process to determine the
optimal mixing speed for removing 95% of the MB and to determine the The connection between t/qt and t yields the slope (1/qe) and
best kinetic adsorption model to explain the experimental results. A intercept 1/(k2qe2). Finally, the second order rate constant (k2) and the
Pyrex glass beaker with a volume of 2 L was used for kinetic process amount of adsorbed dye per mass of composite at the final equilibrium
experiments. In the beaker, 1 L of MB aqueous solution at 50 mg /L was point (qe) are determined.
added and the pH was set to 7. The beaker cell’s center was fixed with a
three-bladed stainless-steel axial flow impeller. At room temperature, 2.6.1.3. Intra-particle diffusion model. Weber and Morris proposed intra-
the impeller’s agitation was begun at 200 rpm. The exact weight of particle diffusion model, which can be written as Eqn 10 [37]:
adsorbent was applied at zero time interval. At various time periods,
samples from the beaker were obtained. The ultimate equilibrium qt = kid t1/2 + C (10)
MB concentration of these samples was determined after they were
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
Fig. 5. FT-IR analysis for a) Fe3O4, b) Geopolymer, c)MGP, and (d) MGP after
removal MB.
Fig. 3. The schematic diagram of experimental equipments.
2.7. Continuous experiments
Table (2) lists the BET surface properties of the gopolymer and MGP.
The characteristics of geopolymer were enhanced when the nano
particles were precipitated. MGP improved the initial geopolymer sur
face area by 62 % while increasing the pore volume by 61%.
Furthermore, following precipitation, the geopolymer’s adsorptive
properties, such as pore surface area, enhanced. These improvements
are the first indication that MGP may operate as an adsorbent. MGP has
a mesoporous structure with diameters ranging from 2 to 50 nm, ac
cording on its pore structure value.
The magnetite, MGP, and geopolymer XRD patterns were presented
in Fig. (4). The crystalline phases quartz, as well as an amorphous
structure with a high level of reflection at 2θ between 15 and 40◦ , can be
identified in the geopolymer [17,39]. XRD diffraction peaks for geo
polymer at 2θ = 20.136◦, 21.03◦, 25.487◦, 26.823◦, 29.54◦, 30.66◦,
36.75◦, 39.65◦, 42.63◦, 50.35◦, 59.985◦, and 68.247◦ are shown in this
Figure with reference code of (00–038-0471). The XRD diffraction peaks
for MGP are shown also, including the reference code (01–081-0537).
Fig. 4. X-ray diffraction (XRD) pattern for structure of (a) Synthesized Fe3O4
magnetite is responsible for the variation in intensity noticed in the
(b) Synthesized Geopolymer and (c) Crystalline structure MGP.
peaks at 30 and 36◦ on the MGP sample [40].
The FTIR spectroscopic analysis of magnetite, gepolymer, and MGP
Where qt (mg/g) is the quantity adsorbed at time t (s), Kid (mg/g s1/
at the 400–4000 nm wavelength range was used to confirm the existence
2) is the intra-particle diffusion rate constant, and C is the value of the
of functional groups that could be responsible for the adsorption process,
intercept, which indicates the thickness of the boundary layer; the
as shown in Fig. (5). The peak at 583 nm in the FTIR of magnetite (Fig. 5-
bigger the intercept, the greater the boundary layer impact. The linear
a) is connected to the Fe–O group. The development of two asymmetric
plots of qt against t1/2 with zero intercept show that the total rate of
bands between 467 and 786 nm was detected by FTIR studies (Fig. 5),
adsorption is determined by intra-particle factors [38].
which is indicative of the spinel structure of magnetite [41]. The O–H
stretching and H–O–H hydrogen-binding water peaks in the
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
Fig. 6. VSM analysis for (a) the synthesis magnetite and (b) MGP.
Fig. 7. FESEM image for (a) Synthesized geopolymer (b) MGP(c) MGP after adsorption of MB.
Fig. 8. EDS analysis for a) Synthesized geopolymer, b)MGP (c) MGP after adsorption of MB.
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
Table 3
Compares the adsorption capacity of MB dye and the influence of geopolymer development in this study to previous researches.
Adsorbent Type Concentration Adsorbent dose pH Contact time Adsorption capacity References
macrofungi spent mushroom waste 50 mg/L 0.55 mg/100 ml 8 4 hr 239.818 mg/g [44]
fly ash geopolymer monoliths 1–50 mg/L (0.11–0.55) (2–12) 30hr 15.4 mg/g [49]
Clay and rice husk 25 mg/L 4 3 20–80 min 15.95, 17.89 and 20.22 mg/g [50]
GP-1 and GP-2 and GP-3
MKG (5–60 mg/L) 0.1 g/100 ml (2–13) 2 hr 43.48 mg/g [15]
LD Slag (50–150) mg/L 0.25 g/L to 2 g/L 4–9 0–200 min 86 mg/g [51]
Fly Ash –based geopolymer spheres (10–250)mg/L (1–2.5)g/ 0.2L – 24 hr 30.1 mg/g [52]
Magnetite /geopolymer composite MGP (10–100)mg/L 0.2 mg /50 ml 7 30 min 76.34 mg/g This study
[44,45].
Table 4
Isotherm models parameters for Methylene blue.
3.2.2. The impact of dose
Model Parameters MB Using a variety of adsorbent quantities, the effect of MB adsorption
Langmuir qm(mg/g) 76.34 on the quantity of adsorbent (MGP) dosage was investigated (0.025 to
KL(l/mg) 0.233 0.4 g). Each dosage was added to 50 ml of aqueous contaminant solution
R2 0.9186 and continuously mixed under the following conditions: Co = 50 mg/L,
RL 1.163
Freundlich KF, 13.6
pH = 7, agitation rate = 200 rpm, and contact time = 1 h in a batch test.
n-1 0.537 Fig. (9b) illustrates the effectiveness of removing of MB as a function of
R2 0.9903 MGP quantity. The results show that increasing the adsorbent dosage
within the prescribed range improves removal efficiency. This trend was
predicted because it is general knowledge that the higher the sorbent
before and after removal of methylene blue are illustrated in Fig. (8 a-c),
dose in a solution, the much more active sites are available. However, it
respectively. The EDS data showed that the chemical composition had
appears that adding 0.2 g to 50 ml of contaminated solution is enough to
changed: geopolymer elemental content were Si, O, Al and Na as shown
achieve equilibrium [46].
in Fig. (8-a). This content of elements were changed in the EDS analysis
for MGP of (Si, Al, O, Na, Fe, and Cl). The EDS analysis of MGP decreased
3.2.3. The impact of contact time
and the The high mass ratio of Fe and O components emphasized the
The proportion of MB adsorbed was calculated at various contact
effective interaction of geopolymer with magnetite nanoparticles. The
times while all other factors remained constant. The relationship
EDS analysis of MGP after adsorption of MB presented the content of MB
elements (C, S and N) as shown in Fig. (8-c).
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
Fig. 14. Error computations in ANN model based on the testing sample.
precipitate magnetite on the surface of the geopolymer. In compared to 3.4. Continuous process results
utilizing simply geopolymer or other materials, this modification
improved the adsorbent’s surface area, mechanical strength, and In the column study, theoretical minimum fluidized velocity (Umf)
chemical resistance, as well as its capacity to absorb MB (see Table (3)). calculated using Eq. (12) [54].
μl (ρl − ρp)g
3.3. Mathematical models Umf = [√(33.7)2 + 0.0408dp3ρl − 33.7] (12)
dpρp μl2
3.3.1. Isotherm models According to Eq. (12), the minimum fluidization velocity (Umf) and
In order to determine the isotherm constants, the collected data was minimum flow rate were calculated as 0.1715 mm/s and 1.21 L/h,
fitted using two models. Linear fitting to the experimental data yielded respectively, producing motion and uniform mass transfer of pollutants
the parameters for each model. Table(4) summarizes all the parameters from bulk liquids to the surface of the adsorbent, and the optimal flow
and their respective determination coefficients.Fig. (10) present linear rate used in this investigation was 10 L/h. As shown in Fig. 13, the
fitting to the experiments data Table(4) indicated that Freundlich breakpoint time to establish equilibrium for the MB was decreased by
isotherm model was the best-fit model to describe the sorption of MB on utilizing a lower bed height. As demonstrated in Figs. 13 and Fig 14, data
the MGP with higher determination coefficients R2 of 0.99.3. Value of n from MB in a continuous study were well fitted with expected data
greater than unity indicates a favourable adsorption taking place [52]. generated by an artificial neural network in IBM SPSS software version
This indicated that the adsorption occurs under a multilayer and het 26.
erogeneous surface for MB.
4. Conclusion
3.3.2. Kinetic models
The typical concentration decay curves of MB in batch experiment In comparison to the geopolymer as presented in the study, magne
are shown in Fig. 11 at different agitation speed which represents the tite was precipitated on the surface of the geopolymer to improve their
relation between Ce/Co and different contact times. The optimum performance in pollutants removal. This alteration increased the ad
agitation speed needed to achieve Ce/Co = 0.05 was (400) rpm for MB. sorbent’s surface area, mechanical strength, and chemical resistance pH
The optimum mass of adsorbent (WA) necessary to achieve 95 % value, efficient contact duration and molecular weight, adsorbate mol
removal performance for a liter of MB solution (Co = 50 mg/L at room ecules, initial MB concentration, and agitation speed are all important
temperature) with a final equilibrium concentration of C/Co = 0.05 was variables in the removal of methylene blue solution by magnetite/geo
2.18 g, as calculated using the isothermal and balancing equations for polymer composite. The presence of more negative and energetic func
solute as shown in Eq. (11) [53]. tional sites on the surface of MGP, different pore sizes in the adsorbent’s
structure, and having various different active compositions (detected by
VL(Co − Ce)
WA = (11) FTIR) are the main reasons for the adsorbent’s performance in MB
KF C1/n
e
removal and demonstrating higher removal rates compared to MB
Where WA is the low mass of adsorbent, VL is the volume of the so removal by synthesized geopolymer only as reported in the literature.
lution, Co and Ce (mg/L) are the beginning and final adsorbate con This adsorbent is more economically feasible to operate, cost effective
centrations, respectively, KF is a rough estimate of adsorption capacity. and friendly environment.
The adsorption kinetics of MB onto MGP was investigated using pseudo
first order, pseudo second order and intra-particle diffusion models as Declaration of Competing Interest
shown in (Fig. 12), using the experimental data at various initial con
centrations. The calculated parameters values obtained from the appli The authors declare that they have no known competing financial
cation of three models are tabulated in Table (5). By comparing R2 for interests or personal relationships that could have appeared to influence
each applied model and the compatibility between the estimated and the work reported in this paper.
observed qe values, the most favourable model may be identified. The
pseudo 2nd order R2 value are greater than other models, and the qe cal Acknowledgment
values for MB are considerably closer to the qe expirement for MB than
other kinetic models. The authors are thankful to the University of Babylon /material en
gineering college / Ceramic laboratories staff for the assistance provided
for this study.
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R.A. Al-husseiny and S.E. Ebrahim Inorganic Chemistry Communications 139 (2022) 109318
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