Evaluation of Activated Carbons Prepared from Bioprecursors for the Removal of Cadmium and Chromium (VI)

Touzani, Ibrahim; El Machrafi, Imane; Harboul, Kaoutar; Boudouch, Otmane; Alouiz, Imad; Hammani, Khalil; Flouchi, Rachid; Fikri-Benbrahim, Kawtar

doi:https://doi.org/10.1155/2024/8663114

Applied and Environmental Soil Science

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Abstract Introduction Materials and Methods Results and Discussion Conclusion Data Availability Conflicts of Interest References Copyright Related Articles

Research Article | Open Access

Volume 2024 | Article ID 8663114 | https://doi.org/10.1155/2024/8663114

Evaluation of Activated Carbons Prepared from Bioprecursors for the Removal of Cadmium and Chromium (VI)

Ibrahim Touzani,^1,2Imane El Machrafi,³Kaoutar Harboul,⁴Otmane Boudouch,⁵Imad Alouiz,⁴Khalil Hammani,⁴Rachid Flouchi,^1,2and Kawtar Fikri-Benbrahim¹

Academic Editor: Yousef Alhaj Hamoud

Received19 Aug 2023

Revised10 Jan 2024

Accepted16 Jan 2024

Published06 Feb 2024

Abstract

Trace metals found in industrial effluents are highly toxic pollutants, and these include cadmium and chromium (VI). The objective of this work is to remove cadmium and chromium (VI) on activated carbons, prepared from biomaterials such as nuclei of Ziziphus lotus and coffee grounds. The characterization of adsorbents was performed by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The results of the characterization showed an important porosity on the activated carbon’s surface, with sizes between 6 and 50 μm. Similarly, the adsorption results showed that the adsorption process is very rapid and that the increase in contact time and temperature improves the efficiency of the Cd and Cr(VI) removal process. Indeed, abatement rates (R%) of 80% for Cr(VI) and 60% for Cd were obtained after 80 minutes of adsorption on activated carbon prepared from Ziziphus lotus, whereas activated carbon obtained from coffee grounds allows a reduction rate of about 50% for Cr(VI) and Cd. Hence, it seems clearly that the activated carbon of Ziziphus lotus is more effective than that of coffee grounds, especially for the Cr(VI) adsorption. The kinetic modeling of the adsorption process followed the pseudo-second-order model, and the Freundlich model has better explained the adsorption isotherm for Cd and Cr(VI). The thermodynamic study showed that adsorption was spontaneous and endothermic.

1. Introduction

All natural resources are dependent on water as the most essential element. Indeed, it is essential and necessary for the man’s survival and health. Therefore, most countries in the world struggle with managing water resources, which are of great importance. However, these resources are under increasing pressure globally due to agricultural and industrial activities and high drinking water consumption. The discharge of untreated or partially treated effluents is currently affecting these water resources, which can lead to pollution of surface and groundwater waters and have a direct impact on ecosystems [1]. Furthermore, wastewater can be made up of several compounds, either solid or dissolved [2]. These micropollutants include metallic trace elements (MTEs), used in many industrial sectors. Due to the toxicity of many MTEs in industrial effluents, even at low concentrations, adverse health and environmental effects may occur [3–5]. The direct and indirect toxic effects of MTEs have been highlighted by numerous studies, which showed that they can cause various health problems in the respiratory, digestive, and urinary systems [6, 7].

Although some heavy metals play an important role in biological systems, they are generally toxic to living organisms depending on the dose and duration of exposure [8]. In toxicology, it is well known that high rates of any compound can have negative impacts and cause toxicity. Indeed, essential heavy metals are necessary in trace amounts in the body but become toxic above certain limits or threshold concentrations, while nonessential heavy metals (Cr, Cd, Pb, and Hg) can be toxic even at very low concentrations [9]. Moreover, unlike organic matter, which can be degraded, MTEs accumulate in water, soil, pond bottoms, and even living organisms [10, 11]. Rapid industrialization has thus led to an expansion of manufacturing and environmental contamination, mainly by heavy metals, particularly in developing countries. Therefore, metal contamination problems are becoming increasingly common worldwide, and numerous studies have been carried out on metal toxicity, particularly in regions where anthropogenic activities are significant.

Chromium is a naturally occurring heavy metal and is considered a major environmental pollutant due to its toxicity for ecological, nutritional, and environmental reasons [12]. Cr exists in the aqueous environment mainly in the oxidation states of Cr(VI) and Cr(III). The discharge of Cr-containing effluents into municipal sanitary sewers has become a matter of concern in recent decades [13]. These toxic chromium ions are generally produced by industries such as pigment and paint manufacture, textile processing, and leather tanning. Indeed, due to its advantages for tanneries, textile, wood processing, and food processing, chromium is one of the most commonly used heavy metals in industry. One of the most dangerous and toxic form of this MTE is chromium (VI) due to its high solubility, which enhances tremendously its mobility in ecosystems [14].

The treatment of wastewater containing various MTEs has, therefore, a great importance in the environment preservation. In this sense, several treatment techniques have been used for wastewater purification to remove chemical contaminants, including the oxidation processes, chemical precipitation, ion exchange, coagulation/flocculation processes, reverse osmosis, membrane filtration, adsorption, and solvent extraction [15]. Unfortunately, most of these methods are sometimes costly and inefficient, particularly when contaminants are present in low or trace concentrations, such as heavy metal ions present at concentrations up to 100 mg/l [16]. Thanks to its economic, environmental, and technical advantages very important to eliminate soluble, insoluble, and biological contaminants, adsorption remains the most commonly used method for treating certain micropollutants such as dyes, trace metals, pesticides, and pharmaceuticals [17]. Since this process was introduced, activated carbon has been most widely used because of its high ability of adsorption depending mainly on its activation, preparation, and purification processes [18]. Many researchers are still struggling to select inexpensive and available precursors for activated carbon production, which has been widely studied [19]. To this end, adsorption using an adsorbent manufactured from biomass may be an interesting and promising solution.

In this context, the present study focuses on the elimination of cadmium (Cd) and chromium (VI) (Cr(VI)) by active carbon prepared from the nuclei of Ziziphus lotus and coffee grounds. These residues are widely available and are renewable sources for the environment. The recovery of these residues has significant environmental and socioeconomic benefits. The obtained active coals were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD). The kinetic models of the pseudo-first-order and the pseudo-second-order, as well as the Langmuir and Freundlich isotherms, are studied to explain the mechanisms and the efficiency of the process of elimination of contaminants under study.

2. Materials and Methods

2.1. The Activated Carbon Preparation

The process of preparation of activated carbon using the nucleus of Ziziphus lotus (NZL) and coffee grounds (GC) as raw materials follows several steps, according to Touzani et al. [20, 21]. Step 1: The NZL and GC are washed, dried, and then crushed into fine particles; step 2: Chemical activation of the NZL and GC by sulfuric acid (H₂SO₄) for 24 h; step 3: The carbonization of the paste obtained after chemical activation is made at 500°C for 2 h; and step 4: The active carbons obtained are sieved with a sieve smaller than 100 μm. The activated carbon produced from NZL and GC, according to the steps described above, is named CA1 and CA2, respectively. These two carbons will be used to eliminate Cd and Cr(VI).

Moisture was measured by weighing a mass quantity of CA1 and CA2 before and after drying at 110°C for one hour. The moisture content obtained was 2.5% and 3% for CA1 and CA2, respectively.

The rate of ash (TC) was measured by weighing the final mass after incineration at 500°C of a 1 g mass of CA1 and CA2 followed by its cooling. The ash content of 2.2% and 2.9% was obtained for CA1 and CA2, respectively.

The prepared CA1 and CA2 were characterized by analytical techniques, including scanning electron microscopy (SEM) by a Quanta 200 model SEM equipped with a tungsten filament electron gun and X-ray diffraction (XRD) undertaken by an XPERT-PRO type XRD within a scan area between 5 and 120° 2θ.

2.2. Experimental Adsorption of Cd and Cr(VI)

2.2.1. Adsorbate Preparation

The Cd stock solution was obtained by solubilizing 10 g of eight hydrated cadmium sulphate (3CdSO₄, 8 H₂O) in 1 liter of distilled water, while the Cr(VI) stock solution (at 1000 mg/l potassium dichromate) was prepared by dissolving 2.829 g of potassium dichromate K₂Cr₂O₇ in 1 liter of distilled water. Then, the other concentrations used for adsorption tests are obtained by successive dilutions.

2.2.2. Contact Time’s Effect

Contact time is one of the most important factors during chemical reactions. In a closed reactor, a 100 ml volume of one of the concentrations of cadmium or chromium (VI) is brought into contact with 0.1 g of activated carbon, under an agitation of 300 r/min. After every 10 min of contact, the suspension is centrifuged 5 min at 5000 rpm. The Cd concentration was determined by inductively coupled plasma mass spectrometry (ICP-AES) at the “Cité d’Innovation” in Fez. In addition, the concentration of Cr(VI) was determined by an UV/visible spectrophotometer (UV 240 Shimadzu mode) using 1–5 diphenylcarbazide as a complexing agent in an acid medium (H₂SO₄) at the wavelength of 540 nm in the laboratory of natural resources and environment of the Polydisciplinary Faculty of Taza.

The effect of contact time on the removal rate of adsorbates was studied during a time interval of 10–280 min for each of the initial following concentrations of 25, 40, 50, and 75 mg/l for Cd and Cr(VI) in the presence of 0.1 g of activated carbon (CA1 and CA2) at ambient temperature. The abatement rate R(%) was calculated from the following equation:where C₀ (mg/l) is the initial adsorbate concentration and C_t (mg/l) is the adsorbate concentration in solution.

2.2.3. Temperature’s Effect

To evaluate the effect of temperature on the adsorption capacity of the various pollutants on the adsorbent, a quantity of 0.1 g of activated carbon with concentration of 25 mg/l for the metallic elements Cd and Cr(VI) was placed in the batch system for 60 minutes. The adsorption temperatures studied were 25–50°C. Finally, the residual concentrations (C_e) were determined for each adsorbate.

2.2.4. Kinetics of Adsorption

The adsorption mechanism and the transfer mode of solutes from the liquid to the solid phase are covered in kinetics. Simplified kinetic models are approved to understand the adsorption mechanism and are commonly well adjusted by a pseudo-first-order kinetic model [22] and a pseudo-second-order kinetic model [23]. These two classical models were tested to study the adsorption kinetics of the investigated pollutants Cd and Cr(VI) on the activated carbons produced (CA1 and CA2).

2.2.5. Pseudo-First-Order

The pseudo-first-order model is defined according to Das et al. [24] as follows:where q_e and q_t are the quantities of the adsorbed ion (mg·g⁻¹) at equilibrium and time t, respectively, while k₁ is the constant of equilibrium velocity for this model (min⁻¹).

2.2.6. Pseudo-Second-Order

The present model is defined according to Raoul et al. [25].where k₂ is the pseudosecond-order adsorption rate constant (g/mg·min).

2.2.7. Adsorption Isotherms

Adsorption isotherms can describe an adsorption process. Langmuir and Freundlich isotherms are used to study the adsorption of Cd and Cr(VI) on activated carbons.

The amount of an adsorbed solute is calculated according to Ojemaye et al. [26].where q_e is the quantity of solute adsorbed at equilibrium per adsorbent’s unit weight (mg/g); C₀ is the initial concentration of solute (mg/l); C_e is the equilibrium concentration of solute (mg/l); m is the adsorbent mass ; and V is the solution volume (l)

The Langmuir model [27] is described mathematically by the following equation:

This equation is often written in the linear form as follows [28]:where q_e and q_max are the equilibrium and the maximum adsorption capacities (mg/g), respectively. K_L is the characteristic Langmuir constant, corresponding to the concentration at equilibrium of the adsorbate solution per unit mass of solid (mg/l).

The Freundlich model [29] is described as follows:

It can also be expressed in the logarithmic form [30].where q_e is the amount of the material adsorbed per unit mass of adsorbent at equilibrium (mg/g). This is the equilibrium concentration (mg/l), K_f is the capacity of the adsorbent adsorption, and n is the intensity of sorption of adsorbent-adsorbate.

2.2.8. Thermodynamic Study

The thermodynamic equilibrium constant K_d, enthalpy (ΔH₀), entropy (ΔS₀), and the variation of Gibbs free energy (ΔG₀) are among the most important thermodynamic parameters involved in the establishment of an adsorption system. Thus, to assess the adsorption process’s feasibility and nature [31], the thermodynamic parameters were determined as follows [32].where k is the equilibrium constant (l/mg), R is the gas constant (8.314 J/mol·K), and T is the absolute temperature (K).

Plotting lnK_d, a function of 1/T, a line having a slope of −∆H₀/R and an intercept of ∆S₀/R is obtained. Subsequently, the standard thermodynamic parameters of adsorption (∆G_0, ∆H₀, and ∆S₀) are calculated.

3. Results and Discussion

3.1. Scanning Electron Microscopy (SEM)

Scanning electron microscopy (SEM) enables to determine the activated carbon’s morphology and external porosity. The porosity increase enables to enhance the active site’s number, thus offering several advantages to the adsorption process [33] and promoting the fixation of the studied metal elements (Cd and Cr(VI)). The results of the SEM analysis of CA1- and CA2-activated carbons are presented in Figures 1(a) and 1(b), respectively. These results show that the surface of the active coals CA1 and CA2 have a very porous morphology with pores of different sizes ranging from 6 to 50 µm and having different cavity shapes. Indeed, the presence of cavities in activated carbons results from the activating agent reaction during the chemical activation process of the precursor by sulfuric acid, followed by pyrolysis. This suggests that the activation process has led to the development of pores and the modification of the produced carbons structure. Thus, the formation of cavities on the surface of the coal seems to result from the evaporation of the activator during carbonization, leaving the space previously occupied by this agent. Moreover, the porous structure can also develop after the evaporation of most of the volatile organic matter, resulting in a fractured activated charcoal surface with large pores.

(a)

(b)

This is in agreement with other research works, such as the optimization of the preparation conditions of activated carbon from Diplotaxis harra biomass and removal of heavy metals carried out by Tounsadi et al. [34] and the production of mesoporous-activated carbon from Indonesian Schleichera oleosa by the combination of pyrolysis and H₂SO₄ activation by Neolaka et al. [35], for Pb(II) adsorption in aqueous solution.

Similarly, it appears from the elementary analysis (Table 1) that the CA1- and CA2-activated carbons contain very interesting carbon percentages of 88.98% and 92.35%, respectively, as well as low oxygen percentages, especially for CA2 (6%), which means that carbonization at 500°C has a significant effect on the elements composition on the activated carbons’ surface. The presence of trace sulfur is also observed, which is due to the use of sulfuric acid (H₂SO₄) as an activating agent.

3.2. X-Ray Diffraction (XRD)

X-ray diffraction (XRD) is used to identify the crystalline or amorphous structure of materials. Figures 2(a) and 2(b) of the X-ray diffraction of CA1 and CA2 show very wide diffraction peaks. Thus, a large peak at about 2θ = 25° indicates the presence of carbon [36]. Moreover, the absence of an acute peak reveals an essentially amorphous structure for both CA1 and CA2 materials [37]. Similarly, there are noise signals corresponding to ash powder in the activated carbons.

(a)

(b)

3.3. Effect of Contact Time

The contact time and the initial concentration of adsorbates play a very important role in the adsorption process. Indeed, the concentration of adsorbates represents the driving force of mass transfer between the solid/liquid phases. Figure 3 represents the evolution of the abatement rate (R%) as a function of time (T) for Cd and Cr(VI) at different concentrations of 25, 40, 50, and 70 mg/l by adsorption on activated carbons CA1 and CA2, respectively. Results show that abatement rates (R%) of 80% and 60% were obtained for Cr(VI) and Cd, respectively, after 80 minutes of adsorption on activated carbon prepared from Ziziphus lotus, whereas reduction rates for both Cr(VI) and Cd did not exceed 50%, with activated carbon obtained from coffee grounds. Hence, the activated carbon of Ziziphus lotus seems to be more effective than that of coffee grounds, especially for the Cr(VI) adsorption.

(a)

(b)

On the other hand, the adsorption curves of Cd and Cr(VI) on the CA1 and CA2 show the same gaits with a metal retention that increases with the increase of the contact time and reaches a saturation phase at about 120 minutes, the time from which retention becomes almost constant. In fact, two kinetic phases can be observed in the Cd and Cr(VI) adsorption process on CA1 and CA2, a rapid phase that can be attributed to the high number of active sites available on the surface of activated carbons, which increases the mass transfer potential and makes it more important. As adsorption progresses, the accumulation of metallic element molecules on the surface of the adsorbents hinders diffusion of the molecules into the pores, which results in slower speed and adsorption capacity.

3.4. Effect of Temperature

The effect of solution temperature on the removal of Cd and Cr(VI) by CA1 and CA2 was studied to determine the effect of temperature on adsorption capacity and process. The results obtained show that the adsorption capacity of Cd and Cr(VI) on CA1 and CA2 increases with increasing temperature (Figure 4). It goes from 4.1 to 4.3 and from 3.68 to 3.97 for Cd and Cr(VI) on CA1, respectively, and from 2.98 to 3.25 and from 2.6 to 3 for Cd and Cr(VI) on CA2, respectively, when the solution temperature increases from 293 K to 323 K. This can be attributed mainly to the penetration of Cd and Cr(VI) molecules into micropores or apparent surface cavities, as it can be attributed to the creation of new active sites at higher temperatures [8, 38]. In addition, a greater affinity between the adsorbate and active sites can be created due to an increase in the chemical interaction between adsorbate and adsorbent at a higher temperature.

(a)

(b)

3.5. Adsorption Kinetics

The correlation coefficients and kinetic parameters of the two diffusion models are presented in Table 2. These results show that the values of the correlation coefficients of the pseudo-first-order model are lower than those obtained for the pseudo-second-order model, which are very close to the unit for the adsorption of Cd and Cr(VI) on CA1 and CA2 activated carbons. In addition, the quantities theoretically adsorbed at equilibrium calculated from the pseudo-second-order model for all studied concentrations (25, 40, 50, and 70 mg/l) are fairly close to the experimental results for Cd and Cr(VI). Furthermore, the velocity constants K₂ decrease as the initial metal concentrations increase, indicating that the adsorbates studied reaches equilibrium more quickly at low initial concentrations than at higher concentrations [39]. More specifically, the pseudo-second-order model represents the involvement of valence forces by electron exchange between adsorbate and adsorbent [40]. These results confirm that the pseudo-second-order model is better suited to the adsorption of Cd and Cr(VI) on CA1 and CA2.

3.6. Adsorption Isotherms

The modeling of the Cd and Cr(VI) adsorption isotherms was done using the Langmuir and Freundlich models. The model constants K_L and K_F and the correlation coefficients () obtained from the two models are listed in Table 3. The Langmuir model reveals that the maximum adsorbed quantity values are 23.256 mg/g for Cd and 17.857 mg/g for Cr(VI) on CA1. Similarly, the K_L constant values for Cd are higher than those for Cr(VI), indicating that the adsorption energy of Cd is higher compared to that of Cr(VI) on the two materials studied. The Freundlich model presents values close to unity in comparison with the Langmuir model, suggesting that the Freundlich model presents a good fit to the experimental data of Cd and Cr(VI) adsorption on CA1 and CA2. This shows that adsorption is a multilayer process, involving interactions between the studied metals’ molecules and the activated carbons surface.

3.7. Adsorption Thermodynamics

In order to study the thermodynamic behavior of Cd and Cr(VI) adsorption on CA1 and CA2, thermodynamic parameters such as Gibbs free energy (ΔG₀), enthalpy (ΔH₀), and entropy (ΔS₀) were calculated using the expressions mentioned above. Table 4 presents the thermodynamic parameters ΔG₀, ΔH₀, and ΔS₀ of adsorption of Cd and Cr(VI) on CA1 and CA2.(i)Feasibility and spontaneity Negative ΔG₀ values for all cases indicate that the adsorption is feasible and spontaneous under the studied conditions. This means the process proceeds naturally without external energy input and reaches equilibrium in a way that minimizes the total system free energy. Increasing absolute values of ΔG₀ with temperature suggest that spontaneity is enhanced at higher temperatures. This aligns with the expected increased kinetic energy of adsorbate molecules at higher temperatures, making them more likely to overcome the energy barrier for adsorption.(ii)Endothermic nature Positive ΔH₀ values indicate that the adsorption process is endothermic. This means it absorbs heat from the surrounding environment. This aligns with the expectation that breaking bonds in the solution and forming new bonds with the adsorbent surface require energy input. The increase in quantity adsorbed with temperature is consistent with the endothermic nature. Higher temperatures provide more energy for overcoming the adsorption barrier, allowing more molecules to stick to the adsorbent.(iii)Entropy change A positive ΔS₀ contributes favorably to the driving force for spontaneity, as increasing entropy generally leads to lower free energy.

Overall, our analysis aligns with established principles of thermodynamics in adsorption processes [41]. Moreover, physisorption can be considered as the predominant adsorption process.

3.8. Performance of the Prepared CA1 and CA2

The development of activated carbon materials has been widely reported by researchers as adsorbents for heavy metals such as Cr(VI), Pb(II), Cu(II), Cd, Zn, and Hg [42]. In general, agricultural resources and bioresources rich in cellulose and hemicellulose are used as precursors in the production of activated carbon. However, in order to assess the MTE removal preferences studied on CA1 and CA2, a comparative study of this work was conducted with other relevant studies (Table 5) using the adsorption capacity (q_max) as the comparative parameter. The results show that the adsorption capacity obtained in this study is comparable to that obtained in the previous work. Furthermore, it is important to point out that the biomaterials used in this study are very abundant, so Ziziphus lotus is a species found in several biotopes in arid and semiarid regions and occupies various geographical areas of Morocco [20]. Whereas, coffee grounds represent waste, resulting from coffee consumption, which can have a great added value. For this reason, CA1- and CA2-activated carbons offer a real advantage as new agent or the depollution of industrial effluents loaded with MTEs.

4. Conclusion

This work aims to study the removal of cadmium and chromium (VI) on activated carbons prepared from biomaterials such as the nucleus of Ziziphus lotus and coffee grounds. Activated carbon was obtained using a chemical activation process with sulphuric acid (H₂SO₄), followed by carbonization carried out at 500°C during 2 h. The results of the SEM characterization revealed the presence of a porous and amorphous structure on the surface of the prepared activated carbons (CA1 and CA2). The adsorption results for MTEs (Cd and Cr(VI)) show that the adsorption process is influenced by a number of parameters such as the initial concentration, contact time, and temperature. The kinetic modeling of adsorption follows the pseudo-second-order model. Similarly, the adsorption isotherm data were better adjusted with the Freundlich model. The thermodynamic parameters (∆G₀, ∆S₀, and ∆H₀) indicate that the adsorption process of the contaminants studied is an endothermic process and that the quantity adsorbed at equilibrium increases with increasing temperature. These results show that Ziziphus lotus and coffee grounds can be considered as an interesting source of the raw material for the preparation of high-quality activated carbon which can be used to decontaminate effluents containing trace metals.

Data Availability

The data used to support the findings of this study are available from the corresponding author upon reasonable request.

Conflicts of Interest

The authors declare that they have no conflicts of interest.

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Copyright © 2024 Ibrahim Touzani et al. This 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.

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