Adsorption of Methyl Orange from Aqueous Solution Using Chitosan/ZSM-5 Composite
Mencui Ning and Runhu Zhang** Author for corresponding; e-mail address: kmzhrh@snnu.edu.cn
ORCID ID: https://orcid.org/0000-0003-2146-4181
Volume: Vol.53 No.5 (September 2026)
Research Article
DOI: https://doi.org/10.12982/CMJS.2026.085
Received: 6 June 2026, Revised: 15 July 2026, Accepted: 3 August 2026, Published: 18 September 2026
Citation: Ning M. and Zhang R., Adsorption of methyl orange from aqueous solution using chitosan/zsm-5 composite. Chiang Mai Journal of Science, 2026; 53(5): e2026085. DOI 10.12982/CMJS.2026.085.
Graphical Abstract
HIGHLIGHTS
- Chitosan/ZSM-5 composite prepared for MO removal.
- Fast adsorption rate; equilibrium reached in 60 min.
- Maximum adsorption capacity achieved at pH=4.0.
- Fits Langmuir isotherm and pseudo-second-order model.
- Spontaneous and exothermic process with high potential.
Abstract
In this work, a chitosan/ZSM-5 composite was prepared as an adsorbent to remove methyl orange (MO) from aqueous solutions. The material’s morphological features and surface functional groups were examined using scanning electron microscopy (SEM) and Fourier-transform infrared (FTIR) spectroscopy. Batch experiments were carried out to investigate the effect of adsorption time, adsorption isotherms, pH effect and thermodynamics. Adsorption kinetics indicated a fast adsorption rate and reached an equilibrium within 60 min; Adsorption capacity was maximum at pH=4.0; The experimental data fitted better to Langmuir than to Freundlich isotherm equation, while the sorption process was described by pseudo-second-order model. The thermodynamic analysis of the removal reaction carried out at three temperatures: 293K, 303K,313K and 323K gave following values (ΔH°=−44.75 kJ mol−1). The values for ΔG° were between –1.06 and –5.12 kJ·mol-1 while ΔS° was equal to –135.26 J·mol-1·K-1. Thermodynamic analysis shows spontaneous adsorption process at the given conditions that are feasible and exothermic in nature. These results indicate that chitosan/ZSM-5 composite materials hold promising potential for the removal of MO from aqueous environments.
1. INTRODUCTION
The textile, printing, dyeing, paper-making, and leather industries have seen considerable expansion recently, leading to major environmental problems, because they produce large amounts of wastewaters containing synthetic dyes, which in the environment pose a great risk to ecosystems as well as human’s health if they are discharged into water bodies [1-3]. Among them, azo dyes are widely used as a dye because of their low cost, wide color palette, and good color fastness characteristics, accounting for more than 60% of the total industrial dye usage. Methyl orange (C14H14N3NaO3S), a representative anionic azo compound, is extensively utilized across diverse fields, including textile manufacturing, food processing, printing, pharmaceutical production, and laboratory research [4]. However, methyl orange is difficult to biodegrade in natural environments, and its metabolites may have carcinogenic and mutagenic properties, making it a priority pollutant in many countries [5-6].
Currently several traditional methods are developed to treat the dyestuff-containing wastewaters like adsorption, chemical precipitation, photochemical oxidation, ozonation, membrane processes and coagulation/flocculation [7-17]. However, such methods are often associated with high costs, low efficiency or secondary pollution problems etc. On the other hand, adsorption represents one of the most promising approaches to treating dye-contaminated wastewater, owing to its favorable attributes such as cost-effectiveness, operational simplicity, high removal efficiency, and regenerability [18-19]. The selection of adsorbent materials is a key factor determining the adsorption effect. Although activated carbon exhibits excellent adsorption performance, its high cost and difficult regeneration have led to a research focus on developing new adsorbent materials that are efficient, low-cost, and biodegradable.
Chitosan, a natural cationic polysaccharide obtained through deacetylation of chitin, possesses abundant amine and hydroxyl functionalities, enabling it to adsorb anionic dyes via mechanisms such as electrostatic attraction, hydrogen bonding, and coordination. Furthermore, chitosan is widely sourced, non-toxic, and biodegradable, making it an ideal green adsorbent material [20]. This material demonstrates versatile utility in environmental remediation, particularly for the effective removal of heavy metal ions and synthetic dyes from contaminated water [21–26]. However, unmodified chitosan exhibits some drawbacks such as poor mechanical properties, susceptibility to dissolution in acidic solutions and a small specific surface area that limits its industrial applications. ZSM-5 is a high silica-to-alumina ratio zeolite with MFI topology, featuring regular microporous channels (about 0.55 nm), large specific surface area (>300 m2/g) and excellent thermal/chemical stability [27-28]. Its surface is rich in silanol groups and a small amount of aluminum-oxygen tetrahedra, providing adsorption sites. However, the adsorption of large molecular dyes (such as methyl orange, with a molecular size of approximately 1.4 nm) by ZSM-5 is limited by the pore size, making it difficult to achieve efficient adsorption. Combining chitosan with ZSM-5 is expected to harness the strengths of both materials: chitosan provides abundant active groups and a flexible network structure, while ZSM-5 contributes to enhanced mechanical stability, heat resistance and specific surface area. These properties improve both the mechanical strength of the composite as well as synergistic effects enhancing MO uptake capacity. Based in these aspects we have prepared a new chitosan/ZSM-5 composite that can increase the stability and strength of the chitosan matrix.
To the best of the authors’ knowledge, very limited information was available regarding the capacity of chitosan/ZSM-5 composite to remove MO dye from aqueous solution. This study innovatively combines chitosan’s amine groups with porous ZSM-5 to form a composite that achieves highly efficient methyl orange (MO) removal via enhanced electrostatic interactions, while maintaining strong structural stability and reusability. Specifically, this work investigates the adsorption performance of the chitosan/ZSM-5 nanocomposite in aqueous solutions. To clarify the removal mechanism, the effects of contact time, solution pH, and temperature were examined, along with a comprehensive analysis of adsorption isotherms and kinetics.
2. MATERIALS AND METHODS
2.1 Materials and Analytical Method
All chemicals used during this work were analytical grade, thus they were directly used without any further pretreatment or cleaning procedures. All solutions and reagents were formulated with deionized water. An appropriate amount of methyl orange dye was dissolved in purified water and diluted to the mark in a volumetric flask to obtain a stock solution with a concentration of 1000 mg L⁻¹. The dye was supplied by Shanghai Sanai Chemical Reagent Co., Ltd., China. The further diluted solutions were used as working solutions in lower concentrations.
The concentration of methyl orange in solution was determined using a Shimadzu UV-160A UV–Vis spectrophotometer. Measurements were performed at the maximum absorption wavelength of 465 nm [29].
The equilibrium adsorption capacity qe (mg/g) can be determined using the mass balance equation below:
Where V is the solution volume (L), W is the amount of adsorbent (g), and C0 and Ce are the initial and equilibrium MO concentrations (mg/L), respectively.
2.2 Preparation of Adsorbents
The accurate weight of 1.00 g chitosan is weighed and placed in the 250 mL glass flask. Then, 2 mL of 4% glacial acetic acid was added, followed by 50 mL of deionized water. A magnetic stirrer was placed in the beaker, and the mixture was stirred until the chitosan was completely dissolved. Subsequently, 5 g of ZSM-5 zeolite was weighed and gradually added to the chitosan solution under continuous stirring. The addition was carried out slowly while stirring to ensure thorough mixing. The reaction between chitosan and ZSM-5 proceeded until completion, resulting in a homogeneous, milky-white, viscous solution. This mixture was then transferred into an electric thermostatic drying oven and dried at 60 °C for 18–20 h until all moisture was completely removed. Finally, the dried precursor underwent milling and screening to yield the chitosan/ZSM-5 composite with uniform particle morphology.
2.3 Characterization of the Adsorbents
The surface functional groups of the chitosan/ZSM-5 composite were identified by FTIR analysis (Nexus 470, Thermo Nicolet, USA) within the spectral range of 4000 to 400 cm-1. The prepared samples of the composite were mixed in a ratio of 1:2 w/w with KI and pressed as pellets for FTIR measurements. In addition, to obtain high-resolution micrographs, the composite morphology was characterized by scanning electron microscopy (SEM; Quanta 200 FEG, FEI Company, USA) operated at an accelerating voltage of 20 kV.
2.4 Adsorption Studies
Adsorption experiments have been carried out for investigating the effect of different variables on removal efficiency of methyl orange dye by chitosan/ZSM-5 composite namely pH, adsorption temperature, adsorbent dose. At each stage, only one variable was altered, and its impact was subsequently evaluated to determine the optimal operation condition. The MO solution was adjusted to different pH values by adding 0.1 mol·L-1 NaOH solution and HCl solution, without the use of buffer solutions. All experiments were carried out under identical temperature conditions in an orbital shaker incubator set at 120 rpm. Contact time is a key parameter governing the adsorption process, as it depends on the properties of the system employed. To study the effect of contact time, 50 mg/L methyl orange solution (100 mL) was taken in a beaker and 0.2 g of chitosan/ZSM-5 composite was added into it. The reaction was carried out at room temperature by stirring continuously. All samples were subjected to shaking at room temperature, with time intervals varying between 10 and 80 min. Afterward, the mixtures were centrifuged, and 5 mL aliquots of the supernatant were taken for analysis. The pH value plays a critical role in controlling the adsorption behavior. The effect of pH on MO removal was systematically examined to identify the optimal condition for maximum efficiency. The experiments were conducted under constant temperature conditions (20±1°C), with the pH range set between 2 and 9 and the initial concentration of Methyl Orange (MO) fixed at 50 mg/L. Having determined the optimal agitation time and pH for MO removal, experiments were also carried out to study the effect of different amounts of adsorbents on MO removal efficiency while keeping C₀ constant as 50 mg/L. Specifically, 100 mL of the solution was combined with 0.05–0.4 g of adsorbent and then shaken. Adsorption isotherms were determined at 20 °C using 2 g/L adsorbent dosage across initial MO concentrations of 20–50 mg·L-1. Kinetic analyses employed 20 mg·L-1, 40 mg·L-1 and 60 mg·L-1 MO solutions at 293 K. Thermodynamic behavior was subsequently evaluated by treating 100 mL of 50 mg·L-1 dye solution (pH 4.0) with 0.2 g adsorbent for 60 min across temperatures of 293–323 K (20–50 °C).
3. RESULTS AND DISCUSSION
3.1 Sorbent Characterization
The morphology of the ZSM-5 and chitosan/ZSM-5 were investigated using SEM analysis. The SEM images in Figure 1a show that the ZSM-5 exhibits regular block-shaped or rhombic dodecahedral crystal morphology with smooth surfaces, well-defined edges, and uniform particle size, displaying typical crystalline features of zeolite molecular sieves.) Following chitosan loading onto the ZSM-5, SEM images of the chitosan/ZSM-5 material reveal that the ZSM-5 crystal outlines remain identifiable. However, the surface is covered by an amorphous chitosan layer, with some particles exhibiting encapsulation, agglomeration, or pore blockage. Crystal plane details become blurred, and the overall morphology tends toward roughness and irregularity, indicating successful chitosan attachment to the ZSM-5 surface (Figure 1b.).
Figure 2 shows the FT-IR spectra of the chitosan and chitosan/ZSM-5 composite. This infrared spectrum (Figure 2a.) exhibits typical chitosan characteristics. The main peak at 1073 cm-1 corresponds to the glycosidic bond (C-O-C), while 1213 cm-1 is attributed to hydroxyl bending vibrations. Vibrations at 790, 537, and 445 cm-1 originate from the sugar ring skeleton. Characteristic siloxane peaks of ZSM-5 molecular sieve (~1100 and ~450 cm-1) are not distinctly observed, suggesting their signals may be masked by chitosan or their content is relatively low. The weak siloxane (Si–O–Si) peaks in the FTIR spectrum are attributed to the high framework condensation and structural symmetry of ZSM-5, which reduce IR activity. Additionally, overlapping with intense bands in the fingerprint region (1000–1200 cm⁻¹) further obscures these peaks. The spectrum is primarily dominated by the chitosan component. The infrared spectrum (Figure 2b.) of the chitosan/ZSM-5 composite undergoes significant changes. The characteristic peak of native chitosan at 1073 cm-1 (C-O-C) shifts to 1088 cm-1, and the peak at 1213 cm-1 disappears, indicating that its hydroxyl groups form strong hydrogen bonds and electrostatic interactions with the sulfonic acid groups of methyl orange. The emergence of new peaks at 609 cm-1 and 461 cm-1 directly confirms the successful adsorption of methyl orange molecules. The retention of the 790 cm-1 peak indicates the stability of the composite framework. Collectively, these changes demonstrate that adsorption is primarily driven by the chitosan component within the composite, whose active sites undergo effective chemical bonding with methyl orange.
3.2 Effect of Contact Time
The influence of contact time on the removal percentage of MO was shown in Figure 3. Adsorption time is critical variable in the adsorption process. As shown in Figure 3, the influence of contact time on the adsorption capacity of chitosan/ZSM-5 for removing methyl orange was investigated between 10 and 80 min. The removal rate of methyl orange gradually increased with extended contact time until reaching equilibrium. During the initial 10 minutes, the removal rate rose rapidly, followed by a gradual increase up to 60 min. At 60 min contact time, maximum removal efficiency (98.56%) was obtained. This is attributed to the abundance of active sites initially available for dye molecule uptake at the solid-liquid interface. Over time, the repulsive forces between dye molecules adsorbed on the chitosan/ZSM-5 composite surface and the solution phase intensify. Consequently, the remaining vacant surface sites become increasingly difficult to occupy, leading to a slowing adsorption rate until a stable state is ultimately reached. Thus, the optimal contact time was determined to be 60 min.
3.3 Effect of pH
The pH of the solution plays a significant role in controlling the sorption process because it affects both the surface binding site of the sorbent and aqueous charge distribution. The effect of pH on removal of MO dye from aqueous solution at various solution pH is shown in Figure 4. As shown in in Figure 4, the removal efficiency of methyl orange decreases significantly with increasing pH. At pH=3–6, the removal efficiency exceeds 90%. According to the literatures [30], the optimum pH was frequently reported around pH 3-6. At pH > 8, it falls below 10%. The removal efficiency of methyl orange reaches its maximum at pH 4, and the MO removal over 98%. The reason lies in the following: At low pH, –NH2 protonates to –NH3+, forming strong electrostatic attraction with the anion MO. At high pH, chitosan deprotonates, weakening electrostatic interactions, and MO may undergo structural transformation, leading to reduced adsorption capacity. Therefore, the optimal pH is 4.0.
3.4 Effect of Adsorbent Dosage on Adsorption
The effect of different adsorbent dosages on MO removal is shown in Figure 5. It can be observed that increasing the adsorbent amount led to a higher removal percentage until an optimum value was reached. Beyond this point, adding extra chitosan/ZSM-5 did not increase the removal efficiency, as the same mass was used and further increments yielded no improvement. At the optimized dosage of 0.2 g, the chitosan/ZSM-5 composite achieved the highest removal efficiency (99%) for methyl orange. Therefore, considering economic aspects, a dosage of 0.2 g was deemed reasonable.
3.5 The Adsorption Isotherm
The adsorption behavior was analyzed using the most employed mathematical models, i.e., the Langmuir and Freundlich isotherms that were applied to interpret the experimental adsorption data [31-32]. The corresponding mathematical expressions are presented as the following:
Langmuir:
Freundlich:
Where: Ce and qe correspond to the equilibrium concentration (mg/L) and the amount adsorbed per gram of adsorbent (mg/g), respectively. The Langmuir constants Q0 and b signify the theoretical maximum adsorption capacity and the adsorption affinity constant. Conversely, the Freundlich constants K and 1/n quantify the adsorption capacity and surface heterogeneity, respectively.
Furthermore, the suitability of the adsorbent for MO removal was assessed using the separation factor constant, RL [33], defined by Equation (4):
Where, b (L/mg) represents the Langmuir constant, and C₀ (mg/L) denotes the maximum initial concentration of MO. The RL value helps in predicting the nature of adsorption; if 0 < RL < 1 then it can be considered as good adsorption, where RL > 1 suggests an unfavorable process, RL = 1 corresponds to a linear adsorption behavior and RL = 0 indicates irreversible adsorption process.
The linear fits for the Langmuir and Freundlich isotherm models are presented in Figure 6 and Figure 7, respectively. Table 1 shows corresponding correlation coefficient (R2) and calculated parameters of the two models. A value of n= 1.25 indicates moderate surface heterogeneity, reflecting a favorable adsorption process driven by a diverse range of binding sites with varying affinities. Analysis of the R2 values, which were both acceptably high, indicates that the Langmuir model (R2 = 0.9971) describes better the experimental data compared to the Freundlich one.
The data strongly imply that the Langmuir theory is the most suitable model for describing MO adsorption on this composite, which is characteristic of monolayer coverage on a uniform surface. The Langmuir parameters derived from experimental data revealed a Q₀ value of 36.72 mg/g, corresponding to the maximum monolayer adsorption capacity, alongside an adsorption constant b of 0.203 L/mg. As shown in Table 2, the dimensionless separation factor (RL) ranged from 0.0897 to 0.1976 under the investigated concentration conditions. Since all calculated RL values were confined within the interval (0, 1), the adsorption was deemed highly favorable, underscoring the material's strong efficacy in removing MO from water.
3.6 Thermodynamic Parameters
To quantify the thermodynamics of MO adsorption onto chitosan/ZSM-5, the changes in Gibbs free energy (ΔG°), enthalpy (ΔH°), and entropy (ΔS°) were evaluated. These parameters were derived from the equations below [34,35]:
Where Kc represents the equilibrium constant, determined by the ratio of the adsorbed amount of methyl orange per litre at equilibrium (CAe, mg/L) to its equilibrium concentration in solution (Ce, mg/L). The gas constant R and the absolute temperature T are 8.314 J·mol-1·K-1 and (K), respectively.
The thermodynamic quantities ΔH° and ΔS° were obtained from the van’t Hoff plot, which is shown in Figure 8. The values of ΔG°, ΔH°, and ΔS° are given in Table 3. At 20, 30, 40, and 50°C, the calculated ΔG° values are −5.12, −3.37, −2.41, and −1.06 kJ/mol, respectively. The gradual reduction in the absolute magnitude of ΔG as temperature rises suggests that cooler conditions thermodynamically favor the adsorption process. Additionally, the negative ΔS points to a more ordered arrangement at the boundary between the adsorbate and the solution. Furthermore, the exothermic nature of MO uptake by the chitosan/ZSM-5 composite, evidenced by the negative ΔH, is consistent with a multilayer adsorption mechanism [36].
The enthalpy change (ΔH°) over the temperature range of 20–50 °C was determined to be -44.75 kJ/mol. This negative value confirms the exothermic nature of the adsorption process, implying that higher temperatures are thermodynamically unfavorable. Moreover, the negative standard entropy change (ΔS° = −135.26 J·mol⁻¹·K⁻¹) reflected enhanced structural ordering at the solid-solution interface. This observation suggests that the adsorbent's internal structure remained largely intact during adsorption.
3.7 Adsorption Kinetics
To elucidate the adsorption rate mechanism, a kinetic analysis was performed by fitting the experimental data with the pseudo-first-order (Lagergren) and pseudo-second-order (Ho) models [37-38].
Lagergren pseudo-first-order:
Ho pseudo-second-order:
Where qt is the adsorption capacity (mg g−1) at time t, and qe is the equilibrium adsorption capacity; k1 (min−1) and k2 (mg g−1·min−1) are rate coefficients of pseudo first- and second-order model, respectively.
The graphs of all mentioned kinetic models are shown in Figs. 9, 10. The different values of kinetics parameters were determined for MO uptake onto chitosan/ZSM-5 at various initial MO concentration (Table 4). The kinetic analysis confirmed that the adsorption process follows pseudo-second-order kinetics, as evidenced by the significantly higher coefficient of determination (R2) for this model compared to the pseudo-first-order model. This result is consistent with previous studies reporting analogous kinetic behavior for methyl orange (MO) adsorption on chitosan-alumina composite [39].
4. CONCLUSIONS
A novel chitosan–ZSM-5 composite adsorbent was prepared and characterized. Batch adsorption experiments evaluated its efficacy in removing MO from aqueous solution. Optimal conditions were established at 60 min contact time, pH 4.0, and an adsorbent dosage of 0.2 g. Equilibrium data conformed closely to the Langmuir isotherm model (R2 > 0.99), confirming monolayer adsorption and yielding a maximum capacity of 36.72 mg·g-1 at 293 K. These results underscore the composite’s potential as an efficient material for dye-contaminated wastewater treatment. Kinetic analysis revealed that the pseudo-second-order model described the adsorption process more accurately than the pseudo-first-order model, suggesting a chemisorption mechanism. Thermodynamic parameters (ΔG° and ΔH°) confirmed that MO adsorption onto the chitosan/ZSM-5 composite was thermodynamically feasible, spontaneous, and exothermic. Under optimal conditions, the adsorbent achieved a removal efficiency of 98.56% for MO. Owing to the synergistic integration of chitosan and ZSM-5, the composite maintains high adsorption capacity and structural integrity over repeated cycles, enabling scalable and cost-effective water treatment. This study provides valuable insights into utilizing this low-cost composite adsorbent for the effective removal of methyl orange dye from wastewater.
ACKNOWLEDGEMENTS
The authors appreciate the financial supports by the doctoral research startup fund of Kunming Metallurgy University (Xxrcxm202402).
AUTHOR CONTRIBUTIONS
Mencui Ning: Conceptualization, Methodology, Resources, Project administration. Runhu Zhang: Supervision, Conceptualization, Data curation, Project administration, Writing - Review & Editing.
CONFLICT OF INTEREST STATEMENT
The authors are required to declare whether or not they hold any conflicting interests.
DECLARATION OF USE OF GENERATIVE AI
We confirm that this manuscript is the original work of the authors. No generative AI or AI-assisted tools were used to generate, edit, or analyze any part of the text or data. The authors take full responsibility for the content and integrity of this submission.
FUNDING
This research was financially supported by the doctoral research startup fund of Kunming Metallurgy University (Xxrcxm202402).
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