International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol.
, 2025 .
https://ijeise.
id/ E-ISSN: 2721-8775 Article Synthesis of Magnetic Composites of Chitosan-Fly Ash-Fe3O4 Nanoparticle to Improve Congo Red Dye Adsorption Novi Eka Mayangsari1.
Dewi One Dira Pratiwi1.
Naura Aqillafasha Ashifa 1.
Tarikh Azis Ramadani2.
Nora Amelia Novitrie3.
Ayu Nindyapuspa 1.
Luqman Cahyono4.
1 Waste Treatment Engineering Study Program.
Shipbuilding Institute of Polytechnic Surabaya.
Jalan Teknik Kimia.
Kampus ITS Sukolilo.
Surabaya.
Indonesia 2 Shipbuilding Engineering Study Program.
Shipbuilding Institute of Polytechnic Surabaya.
Jalan Teknik Kimia.
Kampus ITS Sukolilo.
Surabaya.
Indonesia 3 Safety and Risk Engineering Study Program.
Shipbuilding Institute of Polytechnic Surabaya.
Jalan Teknik Kimia.
Kampus ITS Sukolilo.
Surabaya.
Indonesia 4 Shipbuilding Construction Engineering Technology Study Program.
Shipbuilding Institute of Polytechnic Surabaya.
Jalan Teknik Kimia.
Kampus ITS Sukolilo.
Surabaya.
Indonesia E-mail: anoviekam@ppns.
id, bonepratiwi03@student.
id, cnauraaqillafasya02@student.
dtarikh@ppns.
id, enoranovitrie@ppns.
id, fayunindyapuspa@ppns.
gluqmancahyono24@ppns.
*Corresponding author: noviekam@ppns.
Phone number: 62315947186 Received: 02nd May 2025.
Revised: 16th May 2025.
Accepted: 28th May 2025.
Available online: 30th May 2025.
Published regularly: May and November Abstract Chitosan, an environmentally friendly adsorbent, is derived from the deacetylation of crab shell chitin.
this study, the chemical and physical properties of chitosan were enhanced through the direct compositing process of magnetic chitosan (Ch.
with fly ash powder particles (FA).
This research is of considerable importance in the development of environmentally friendly adsorbent materials for the treatment of wastewater contaminated with synthetic dyes, particularly azo dyes such as congo red.
The utilization of crab shell waste as a source of chitosan, in conjunction with fly ash and FeCEOCE to form Chi-FA-FeCEOCE magnetic composites, has been demonstrated to exhibit considerable promise in enhancing adsorption The magnetic composite of Chi-FA-FeCEOCE was characterized by XRD and SEM.
The present study investigated the effect of adsorption process parameters on CR dye removal.
The parameters that were investigated included contact time .
-150 minute.
and initial concentration of CR dye at an adsorbent dosage of 0.
06 grams in 100 milliliters and a pH of 4.
The maximum removal efficiency of the Chi-FA-FeCEOCE composite for CR dye was recorded as 99.
82% at an initial concentration of 100 parts per million .
CR dye for 150 minutes.
Pursuant to the analysis of XRD, it has been confirmed that the compositing process was successfully executed, thereby yielding 2 values indicative of FeCEOCE and FA.
Additionally, an enhancement in the intensity of the Chi-FA-FeCEOCE composite was observed following the adsorption of CR dye.
Concurrently.
SEM analysis revealed that the Chi-FA-FeCEOCE composite and the Chi-FA-FeCEOCE composite exhibited an augmented intensity.
Keywords: chitosan, composites, magnetic, fly ash, congo red Introduction Water contamination represents a grave environmental concern, significantly contributing to overall pollution levels and posing a substantial DOI:10.
International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol.
, 2025
threat to public health.
Annually, a substantial quantity of dye-containing waste is produced from industrial activities, including textiles, food, pharmaceuticals, paper, and cosmetics .
, .
These dyes have been shown to impede the penetration of sunlight through water, exhibit chemical persistence, and are not biodegradable .
, .
Congo red (CR) is a type of azo .
dye, which is the predominant class of synthetic dyes and is extensively utilized by numerous The compound is classified as a carcinogen due to its structural elements, specifically the presence of aromatic amines.
The aromatic structure of these dyes renders them resistant to natural degradation, a property that is characteristic of azo dyes.
Dyes that persist in the environment for extended periods, exerting detrimental effects on fauna and flora .
Therefore, water treatment is necessary to eliminate CR dyes.
A substantial amount of progress has been achieved in the domain of wastewater treatment A variety of techniques have been employed to remove dyes from wastewater, electrochemical oxidation, and adsorption .
Among these methods, adsorption technology is ideal for wastewater treatment due to its costeffectiveness, high efficiency, and low energy consumption .
In the field, numerous researchers have developed various materials that function as adsorbents for dye removal.
These include activated carbon .
, zeolite .
, silica .
, cellulose .
, and chitosan .
In recent years, significant attention has been directed towards the development of environmentally adsorbents, particularly those derived from Chitosan (Ch.
is a cationic polysaccharide composed of D-glucosamine Chi is typically derived from the deacetylation of chitin found in shrimp shells, crab shells, lobster shells, and oyster shells, thereby ranking as the second most prevalent biopolymer in nature after cellulose .
The distinctive molecular configuration of Chi is attributable to the presence of amine (-NH.
and hydroxyl (-OH) functional groups, which function as dynamic adsorption sites capable of removing various water pollutants, including dyes .
Chi can be modified by compositing to increase porosity and surface area, and to reduce internal diffusion resistance.
Such modifications can be achieved through the incorporation of ZnO nanoparticles.
TiO2 nanoparticles, clay nanocomposites, magnetic (Fe 3O.
, and fly ash (FA) .
Adsorption is a promising method of removing pollutants from water, and FA is a promising adsorbent.
The chemical composition, surface area, porosity, particle size, and waterholding capacity of FA all suggest that it has the potential to increase its adsorption capacity.
The composition of FA predominantly consists of metal oxides, including silica (SiO.
, alumina (Al2O.
, and magnetite (Fe 2O.
, in addition to unburned carbon .
Another modification that can be made is adding Fe3O4 nanoparticles as a magnetic core in composite materials to achieve effective separation and easy collection of adsorbents from aqueous media with an external magnetic field .
Ferrite (FeCEOCE) are frequently utilized magnetic particles due to their exceptional properties, including elevated surface area, biocompatibility, magnetic responsiveness, and chemical stability .
The primary objective of this study was to develop a novel magnetic chitosan-fly ash-Fe 3O4 (Chi-FA-Fe 3O.
composite that functions as an It is characterized by high chemical stability, and can be both recovered and separated.
The effectiveness of Chi-FA-Fe3O4 was examined based on its capacity to remove CR dye from an aqueous environment.
The synthesis and application of Chi-FA-FeCEOCE as an adsorbent are contingent upon two primary parameters: contact time and initial concentration of CR dye.
Material and Method Materials Fly ash (FA) is a byproduct of the combustion of coal, a material that is a fundamental component of the power generation Chi is derived from deacetylation of crab shell chitin.
The following reagents were procured from Merck: iron .
chloride hexahydrate (FeCl3.
6H2O), iron (II) sulfate heptahydrate (FeSO4.
7H2O), congo red (C32H22N6Na2O6S.
, acetic acid (CH 3CO2H), and sodium hydroxide (NaOH).
All experiments were conducted using distilled water.
DOI:10.
International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol.
, 2025
Synthesis of Chi-FA-Fe3O4 composite A mixture of 1 g of Chi and 1 g of FA particles was prepared in an acetic acid solution .
%, 50 mL).
The solution was subjected to gentle stirring for a period of 24 hours at room This procedure was intended to ensure complete dissolution of Chi and the subsequent loading of FA particles into the molecular structure of Chi.
Subsequently, 3.
9 g of FeCl3.
6HCCO and 2.
7 g of FeSO4.
7HCCO were dissolved in 10 mL of distilled water and added to the Chi-FA solution under slow stirring .
for a duration of one hour.
The obtained solution was subsequently introduced into a sodium hydroxide solution .
M, 1000 mL) with a rate of 10 mL over a period of 6 hours, under conditions of slow stirring.
This process resulted in the instantaneous formation of magnetic Chi-FAFe3O4.
The newly synthesized magnetic Chi-FAFe3O4 was subjected to a thorough wash with distilled water, with the objective of eradicating residual sodium hydroxide solution.
Following this step, the material was dried in a controlled After a thorough examination of the pulverization process, it was determined that the desired result, i.
, the Chi-FA-Fe3O4 composite powder, was finally obtained.
Characterization The characterization of the Chi-FA-Fe3O4 composites was carried out by various analytical methods and techniques.
The morphology of the Chi-FA-Fe3O4 samples was analysed using a scanning electron microscopy (SEM.
FeI Inspect S50-AMETEX).
The analysis of the Chi-FAFe3O4 composites before and after the adsorption of CR dye is the subject of this investigation.
XRay Diffraction (XRD.
Bruker D8 Advance Eco.
German.
was utilized to examine the crystallinity and amorphous nature of Chi-FA-Fe3O4 composites and Chi-FA-Fe3O4 composites following CR dye adsorption.
pH 4.
Subsequent to this, the mixture was separated between the filtrate and the residue.
The filtrate from the adsorption process was analyzed using a UV-Vis spectrophotometer (Agilent Cary 60 Spectrophotometer.
= 497 n.
to determine the concentration of CR adsorbed in the The calculation of removal efficiency can be performed using equation 1.
ya Oeya %ycIyceycoycuycycayco = ycu yce y 100% .
yaycu Where Co and Ce are the initial concentration of CR and the final concentration of CR in ppm.
Results and Discussion XRD analysis The crystal structure of the adsorbent was determined by XRD analysis.
As illustrated in Figure 1, the XRD patterns of the Chi-FA-Fe 3O4 composite adsorbent and the Chi-FA-Fe 3O4 composite after CR dye adsorption are shown.
The highest peaks of the Chi-FA-Fe3O4 composite prior to adsorption are located at 2 = 35.
492A and 8168A.
The presence of Fe 3O4 particles is indicated by characteristic peaks at 2 = 30A, 35A, 43A, 53A, 57A, and 62A.
Furthermore, the prominent peaks observed at 2 = 16A, 22A, 26A, 33A, 39A, 41A, 50A, 60A, 61A, and 68A correspond to the crystalline phases of the FA particles, including alumina (Al2O.
, quartz (SiO.
, and hematite (Fe 2O.
The presence of these peaks is indicative of the insertion of FA particles into the molecular structure of magnetic chitosan.
Following the adsorption process, an increase in intensity at 2 = 17.
36A is observed, suggesting that a change occurs during the adsorption process, indicating that the CR dye molecules are inserted into the adsorbent pore .
Adsorption experiments The effect of contact time .
-150 minute.
was studied using initial CR adsorbate concentrations of 100 and 150 ppm.
The adsorption process was carried out with a dose of 06 g of adsorbent in 100 ml of CR adsorbate at DOI:10.
International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol.
, 2025
Fig 1.
XRD analysis of Chi-FA-Fe 3O4 composite adsorbent and Chi-FA-Fe3O4 composite after CR dye adsorption SEM analysis The surface morphological structure of the Chi-FA-Fe3O4 composite adsorbent and Chi-FAFe3O4 composite after CR dye adsorption was examined by SEM analysis.
Figures 2a and b illustrate the SEM images of the Chi-FA-Fe3O4 Chi-FA-Fe3O4 composite following CR dye adsorption, respectively.
illustrated in Figure 2a, the surface morphology of the Chi-FA-Fe3O4 composite is characterized by its roughness, porosity, and the presence of crevices and cracks.
Figure 2a also demonstrates the discrepancy in size of the embedded spherical objects that are clearly visible on the surface of the Chi-FA-Fe3O4 composite.
This indicates the successful incorporation of FA particles into the molecular structure of the Chi-FA-Fe3O4 The surface of the Chi-FA-FeCEOCE sample exhibited a more compact morphology following MB dye adsorption, as observed in Figure 2b.
This change was accompanied by the emergence of crevices on the surface, suggesting the presence of CR molecules adsorbed on the surface of Chi-FA-FeCEOCE.
was a decrease in the removal efficiency after 120 The increase in removal efficiency is because there are many active sites on the surface of Chi-FA-Fe3O4, and with the extension of time, the adsorption gradually tends to equilibrium saturation .
After passing the equilibrium condition, the removal efficiency starts to decrease slowly.
This decrease occurs because the adsorbent experiences desorption, which occurs when the adsorbate on the surface of the adsorbent is released back into the solution because the active groups on the adsorbent are saturated .
In addition, the initial concentration of CR dye also affects the removal efficiency.
As the initial concentration increases, the removal efficiency of CR dye on Chi-FA-Fe3O4 gradually This occurs because the adsorption capacity of activated carbon is limited, i.
, the adsorption sites on its surface are limited .
low solution concentration, the activated carbon does not reach adsorption saturation, and CR ions can fully occupy the adsorption sites on its surface, and the removal rate is high, but the adsorption amount per unit is relatively small.
As the solution concentration increases, the diffusion rate of CR ions also increases, and the amount of CR ions adsorbed on the surface of the activated carbon unit increases .
Fig 2.
SEM analysis with 10,000x magnification .
Chi-FA-Fe3O4 composite and .
Chi-FA-Fe3O4 composite after adsorption of CR dye Effect of contact time concentration of CR dye and initial Contact time and initial concentration of CR dye are one of the most important factors affecting the adsorption efficiency.
As shown in Figure 3, the removal efficiency of CR in solution by Chi-FA-Fe3O4 increased with time at an initial concentration of 100 ppm of CR dye.
However, at the initial concentration of 150 ppm CR dye, there Fig 3.
Effect of contact time and initial dye concentration on the adsorption of CR dye with Chi-FA-Fe3O4 composite adsorbent Conclusions Magnetic chitosan-fly ash-Fe3O4 (Chi-FAFe3O.
composites were successfully synthesized and applied as effective bio adsorbents for the DOI:10.
International Journal of Eco-Innovation in Science and Engineering (IJEISE) Vol.
, 2025
removal of azo .
The Chi-FA-Fe3O4 composite was easily separated and collected from aqueous solution after the adsorption process by external magnetic field.
The results showed that the highest CR dye removal efficiency .
was obtained from the significant interaction effect between contact time and initial concentration of CR dye at pH 4.
This study introduces an innovative and efficient adsorbent for removing diazo dyes from water.
Acknowledgement The authors are grateful for the financial support of the DIPA Politeknik Perkapalan Negeri Surabaya 2025.
References