* Corresponding Author
Synthesis, Characterization, and Application of Magnetic Mesoporous MCM-41-Fe3O4 Core-Shell Nanoparticles in the Removal of Eosin Yellow Dye
https://doi.org/10.22146/ijc.108056 Rawaa Abd Alattar(1*), Hayder Hamied Mihsen(2), Luma Majeed Ahmed(3)
(1) Department of Chemistry, College of Science, University of Kerbala, Kerbala 56001, Iraq
(2) Department of Chemistry, College of Science, University of Kerbala, Kerbala 56001, Iraq
(3) Department of Chemistry, College of Science, University of Kerbala, Kerbala 56001, Iraq; Al-Zahraa Center for Medical and Pharmaceutical Research Sciences (ZCMRS), Al-Zahraa University for Women, Karbala 56001, Iraq
(*) Corresponding Author
Abstract
Spinel ferrite (Fe3O4) nanoparticles have been produced as a black powder using precipitation and ultrasonic methods. The framework of MCM-41 was built using sodium silicate as the source of silica and CTAB as a template. Fe3O4 was immobilized on MCM-41 using the microwave method at 100 °C for 20 min, yielding MCM-41-Fe3O4 as a brown solid powder. This characterization was performed using FTIR, XRD, BET, TGA, FESEM-EDX, VSM, AFM, and TEM. The FTIR analysis demonstrated that the MCM-41-Fe3O4 had been properly synthesized. Two M−O bond peaks were discovered, one for the (Fe3+−O2−) octahedral site and one for the (Fe2+−O2−) tetrahedral sites. The XRD analyses revealed that MCM-41-Fe3O4 was synthesized with a highly ordered hexagonal building. The particles exhibited a spherical agglomeration and appeared smooth, as observed in TEM and FESEM examinations. The EDX analysis indicates that it was formed purely from Si, Fe, and O, with a weight percentage of 100%. BET analysis indicated that the sample had a relatively high surface area. In terms of a kinetic model, it was determined that a pseudo-second-order model provided the most suitable description. The thermodynamic study revealed that physical adsorption was exothermic and the adsorption process was nonspontaneous.
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[1] Mousavi, S.R., Asghari, M., and Mahmoodi, N.M., 2020, Chitosan-wrapped multiwalled carbon nanotube as filler within PEBA thin film nanocomposite (TFN) membrane to improve dye removal, Carbohydr. Polym., 237, 116128.
[2] Wen, Z., Gao, D., Niu, H., Lin, J., Li, Z., Zeng, J., Ke, F., Zhang, F., Xia, Z., and Wang, D., 2023, Three-dimensional porous adsorbent based on chitosan-alginate-cellulose sponge for selective and efficient removal of anionic dyes, J. Environ. Chem. Eng., 11 (5), 110831.
[3] Shah, S.S., Sharma, T., Dar, B.A., and Bamezai, R.K., 2021, Adsorptive removal of methyl orange dye from aqueous solution using populous leaves: Insights from kinetics, thermodynamics and computational studies, Environ. Chem. Ecotoxicol., 3, 172–181.
[4] Chun, J., Mo Gu, Y., Hwang, J., Oh, K.K., and Lee, J.H., 2020, Synthesis of ordered mesoporous silica with various pore structures using high-purity silica extracted from rice husk, J. Ind. Eng. Chem., 81, 135–143.
[5] Hello, K.M., Mihsen, H.H., and Mosa, M.J., 2014, Modification of silica with 2,4-dinitrophenylhydrazanomethylphenol for monosaccharide productions, Iran. J. Catal., 4 (3), 195.
[6] Hossain, S.S., and Roy, P.K., 2020, Waste rice husk ash derived sol: A potential binder in high alumina refractory castables as a replacement of hydraulic binder, J. Alloys Compd., 817, 152806.
[7] Hossain, S.S., Yadav, S., Majumdar, S., Krishnamurthy, S., Pyare, R., and Roy, P.K., 2020, A comparative study of physico-mechanical, bioactivity and hemolysis properties of pseudo-wollastonite and wollastonite glass-ceramic synthesized from solid wastes, Ceram. Int., 46 (1), 833–843.
[8] Kadhem, F.H., Ahmed, L.M., Abed, S.A., Tami, A.N., and Wan Salleh, W.M.N.H., 2025, Friendly green synthesis of cerium oxide nanoparticles using Citrus aurantuim extract and applied in removal of eosin yellow dye, J. Nanostruct., 15 (4), 2553–2571.
[9] Hossain, S.S., Mathur, L., Bhardwaj, A., and Roy, P.K., 2019, A facile route for the preparation of silica foams using rice husk ash, Int. J. Appl. Ceram. Technol., 16 (3), 1069–1077.
[10] Ghorbani, F., Kamari, S., Zamani, S., Akbari, S., and Salehi, M., 2020, Optimization and modeling of aqueous Cr(VI) adsorption onto activated carbon prepared from sugar beet bagasse agricultural waste by application of response surface methodology, Surf. Interfaces, 18, 100444.
[11] Sanati, A.M., Kamari, S., and Ghorbani, F., 2019, Application of response surface methodology for optimization of cadmium adsorption from aqueous solutions by Fe3O4@SiO2@APTMS core–shell magnetic nanohybrid, Surf. Interfaces, 17, 100374.
[12] Mirheidari, M., and Safaei‐Ghomi, J., 2021, Design, synthesis, and catalytic evaluation of aluminum‐incorporated magnetic core–shell mesoporous microsphere catalyst NiFe2O4@SiO2@Al‐MS for the synthesis of functionalized indenopyrazolones, Appl. Organomet. Chem., 35 (8), e6274.
[13] Ghorbani, F., and Kamari, S., 2019, Core–shell magnetic nanocomposite of Fe3O4@SiO2@NH2 as an efficient and highly recyclable adsorbent of methyl red dye from aqueous environments, Environ. Technol. Innovation, 14, 100333.
[14] Ramazani, Z., Elhamifar, D., Norouzi, M., and Mirbagheri, R., 2019, Magnetic mesoporous MCM-41 supported boric acid: A novel, efficient and ecofriendly nanocomposite, Composites, Part B, 164, 10–17.
[15] Hatem, R.S., Hussain, A.F., and Mihsen, H.H., 2024, Green synthesis, characterization, and adsorption of Co(II) and Cu(II) ions from aqueous solution by mesoporous silica MCM-41, Chem. Pap., 78 (11), 6331–6342.
[16] Hülsey, M.J., Yang, H., and Yan, N., 2018, Sustainable routes for the synthesis of renewable heteroatom-containing chemicals, ACS Sustainable Chem. Eng., 6 (5), 5694–5707.
[17] Alattar, R.A., 2025, Microwave-assisted green synthesis of SBA-15 and its application on photodecolorization of eosin yellow dye, Al-Zahraa J. Health Med. Sci., 3 (2), 91–104.
[18] Hameed, M.A., and Ahmed, L.M., 2024, Controllable cetrimide – assisted hydrothermal synthesis of MoFe2O4 and coupling with Al2O3 as an effective photocatalyst for decolorization of indigo carmine dye, Indones. J. Chem., 24 (1), 170–184.
[19] Mohammad, H.M., Saeed, S.I., and Ahmed, L.M., 2023, Ease Synthesis of broccoli-like Fe3O4 Nanostructures for superior removal of eosin yellow dye, J. Nanostruct., 13 (2), 483–494.
[20] Mihsen, H.H., and Sobh, H.S., 2018, Preparation and characterization of thiourea-silica hybrid as heterogeneous catalyst, Asian J. Chem., 30 (5), 937–943.
[21] Ali, H.H., Hussein, K.A., and Mihsen, H.H., 2023, Antimicrobial applications of nanosilica derived from rice grain husks, Silicon, 15 (13), 5735–5745.
[22] Attol, D.H., Mihsen, H.H., Jaber, S.A., Alwazni, W.S., and Eesa, M.T., 2023, Synthesis of organic functionalized silica from rice husk as an antibacterial agents, Silicon, 15 (5), 2349–2357.
[23] Mihsen, H.H., Rfaish, S.Y., Abass, S.K., and Sobh, H.S., 2018, Synthesis and characterization of silica-thioamide hybrid compounds derived from rice husk ash with expected biological and catalytic activity, J. Global Pharma Technol., 10 (11), 590–598.
[24] Suyanta, S., and Kuncaka, A., 2011, Utilization of rice husk as raw material in synthesis of mesoporous silicates MCM-41, Indones. J. Chem., 11 (3), 279–284.
[25] Timofeeva, M.N., Kalashnikova, G.O., Shefer, K.I., Mel’gunova, E.A., Panchenko, V.N., Nikolaev, A.I., and Gil, A., 2020, Effect of the acid activation on a layered titanosilicate AM-4: The fine-tuning of structural and physicochemical properties, Appl. Clay Sci., 186, 105445.
[26] Radica, F., Mura, S., Carboni, D., Malfatti, L., Garroni, S., Enzo, S., Della Ventura, G., Tranfo, G., Marcelli, A., and Innocenzi, P., 2020, Phenyl-modified hybrid organic-inorganic microporous films as high efficient platforms for styrene sensing, Microporous Mesoporous Mater., 294, 109877.
[27] Xie, W., and Zang, X., 2016, Immobilized lipase on core–shell structured Fe3O4–MCM-41 nanocomposites as a magnetically recyclable biocatalyst for interesterification of soybean oil and lard, Food Chem., 194, 1283–1292.
[28] Molaei, S., and Ghadermazi, M., 2020, Selective and efficient oxidation of sulfides and thiols to their corresponding sulfoxides and disulfides catalyzed with praseodymium (III) and dysprosium (III) isonicotinamide (INA) complexes grafted onto modified mesoporous MCM-41, Solid State Sci., 100, 106091.
[29] Baabu, P.R.S., Kumar, H.K., Gumpu, M.B., Babu K.J., Kulandaisamy, A.J., and Rayappan, J.B.B., 2022, Iron oxide nanoparticles: A review on the province of its compounds, properties and biological applications, Materials, 16 (1), 59.
[30] Zhang, J., Shang, X., Ren, H., Chi, J., Fu, H., Dong, B., Liu, C., and Chai, Y., 2019, Modulation of inverse spinel Fe3O4 by phosphorus doping as an industrially promising electrocatalyst for hydrogen evolution, Adv. Mater., 31 (52), 1905107.
[31] Chai, P.V., Mahmoudi, E., Teow, Y.H., and Mohammad, A.W., 2017, Preparation of novel polysulfone-Fe3O4/GO mixed-matrix membrane for humic acid rejection, J. Water Process Eng., 15, 83–88.
[32] Abdollahi-Alibeik, M., and Ramazani, Z., 2022, Synthesis, characterization and application of magnetic mesoporous Fe3O4@Fe-Cu/MCM‐41 as efficient and recyclable nanocatalyst for the Buchwald-Hartwig C-N cross-coupling reaction, J. Chem. Sci., 134 (3), 77.
[33] Al Rihaymee, L.M.A., 2013, Enhanced Photocatalytic Activity of Titanium Dioxide Nanoparticles by Metal Deposition, Dissertation, University of Babylon-College of Science, Iraq.
[34] Abbas, S.K., Hassan, Z.M., Mihsen, H.H., Eesa, M.T., and Attol, D.H., 2020, Uptake of nickel(II) ion by silica-o-phenylenediamine derived from rice husk ash, Silicon, 12 (5), 1103–1110.
[35] Galacho, C., Carrott, M.M.L.R., and Carrott, P.J.M., 2008, Evaluation of the thermal and mechanical stability of Si-MCM-41 and Ti-MCM-41 synthesised at room temperature, Microporous Mesoporous Mater., 108 (1-3), 283–293.
[36] Vaysipour, S., Rafiee, Z., and Nasr-Esfahani, M., 2020, Synthesis and characterization of copper (II)-poly(acrylic acid)/M-MCM-41 nanocomposite as a novel mesoporous solid acid catalyst for the one-pot synthesis of polyhydroquinoline derivatives, Polyhedron, 176, 114294.
[37] Kamari, S., and Ghorbani, F., 2021, Extraction of highly pure silica from rice husk as an agricultural by-product and its application in the production of magnetic mesoporous silica MCM–41, Biomass Convers. Biorefin., 11 (6), 3001–3009.
[38] Si, Z., Wang, Z., Cai, D., Li, G., Li, S., and Qin, P., 2020, A high-permeance organic solvent nanofiltration membrane via covalently bonding mesoporous MCM-41 with polyimide, Sep. Purif. Technol., 241, 116545.
[39] Lam, C.D., and Park, S., 2025, Nanomechanical characterization of soft nanomaterial using atomic force microscopy, Mater. Today Bio, 31, 101506.
[40] Qiao, J., Gao, Y., Zheng, K., Shen, C., Jia, A., and Zhang, Q., 2025, One-pot synthesis of magnetic core-shell Fe3O4@C nanospheres with Pt nanoparticle immobilization for catalytic hydrogenation of nitroarenes, Appl. Sci., 15 (10), 5773.
[41] Mukhlis, M., Hidayah, N., Hanifah, A., Itnawira, I., Anita, S., Devi, S., and Tamboesai, E.M., 2025, Optimization of contact time and stirring speed in the adsorption of Cd(II) using Acacia crassicarpa bark powder as adsorbent, Indones. J. Chem. Anal., 8 (2), 111–120.
[42] Chen, S., Qin, C., Wang, T., Chen, F., Li, X., Hou, H., and Zhou, M., 2019, Study on the adsorption of dyestuffs with different properties by sludge-rice husk biochar: adsorption capacity, isotherm, kinetic, thermodynamics and mechanism, J. Mol. Liq., 285, 62–74.
[43] Bibi, S., Ahmad, A., Shah, S.S., Siddiq, M., Habila, M.A., and Choi, D., 2024, Synthesis of Cit-Fe3O4@TiO2 photocatalyst for the degradation of eosin-Y and methylene blue dye, Ceram. Int., 50 (20, Pt. A), 37533–37540.
[44] Hassan, A.A., Ali, M.E.M., Abdel-Latif, S.A., Hasani, I.W., and Fahim, Y.A., 2025, Efficient removal of Remazol Red dye from aqueous solution using magnetic nickel ferrite nanoparticles synthesized via aqueous reflux, Sci. Rep., 15 (1), 17527.
[45] Fakhri, F.H., and Ahmed, L.M., 2019, Incorporation CdS with ZnS as composite and using in photo-decolorization of Congo red dye, Indones. J. Chem., 19 (4), 936–943.
[46] Ulu, A., Noma, S.A.A., Koytepe, S., and Ates, B., 2018, Magnetic Fe3O4@MCM-41 core–shell nanoparticles functionalized with thiol silane for efficient l-asparaginase immobilization, Artif. Cells, Nanomed., Biotechnol., 46 (sup2), 1035–1045.
[47] Iryani, A., Nur, H., Santoso, M., and Hartanto, D., 2020, Adsorption study of rhodamine B and methylene blue dyes with ZSM-5 directly synthesized from Bangka kaolin without organic template, Indones. J. Chem., 20 (1), 130–140.
[48] Lafi, R., Mabrouk, W., Al Zahrani, A.Y.A., Hafiane, A., Keshk, S.M.A.S., and Montasser, I., 2024, Methyl orange adsorption onto modified extracted cellulose from olive stones: Kinetics, isotherms, thermodynamic, mechanism studies, and desorption, Water Conserv. Sci. Eng., 9 (2), 38.
[49] Guo, Y., Chen, B., Zhao, Y., and Yang, T., 2021, Fabrication of the magnetic mesoporous silica Fe-MCM-41-A as efficient adsorbent: Performance, kinetics and mechanism, Sci. Rep., 11 (1), 2612. DOI: https://doi.org/10.22146/ijc.108056
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