Influence of Alkaline and Acidic Co-precipitation Media on Fe₃O₄/TiO₂ Photocatalyst Performance for the Photodegradation of Cypermethrin
DOI:
https://doi.org/10.26418/positron.v15i1.92902Keywords:
Fe₃Oâ‚„"“TiOâ‚‚ composite, Photocatalysis, Cypermethrin degradation, Co-precipitation methodAbstract
The persistence of pesticide residues such as cypermethrin in water bodies has raised environmental concerns, necessitating the development of effective photocatalytic materials for their degradation. This study examines the influence of solvent-assisted magnetite synthesis on the structural, magnetic, and photocatalytic properties of Fe₃O₄/TiO₂ composites for cypermethrin degradation under UV light with a focus on a comparative approach between alkaline and acidic synthesis routes, which has not been extensively reported. Fe₃O₄ was synthesized via co-precipitation using NaOH and HCl to assess the impact of solvent conditions. Xray diffraction confirmed the spinel-phase structure in both samples, while SEM showed finer and more uniform particles in the NaOH-derived sample. VSM analysis revealed that Fe₃O₄–HCl exhibited higher saturation magnetization (Ms = 57.98 emu/g) but lower coercivity (Hc = 0.0206 T) than Fe₃O₄–NaOH (Ms = 41.26 emu/g; Hc = 0.0241 T), indicating synthesis-dependent magnetic properties. UV–Vis analysis identified a cypermethrin absorption peak at 220 nm, which was used to monitor degradation. The Fe₃O₄–NaOH:TiO₂ composite showed superior photocatalytic activity (31.98% degradation in 90 minutes) compared to Fe₃O₄– HCl:TiO₂ (22.86%). Kinetic modeling using the pseudo first-order equation yielded a higher rate constant for Fe₃O₄-NaOH:TiO₂ (k = 0.00172 min⁻¹; R² = 0.769), while Fe₃O₄–HCl:TiO₂ showed slower kinetics but better linearity (k = 0.00030 min⁻¹; R² = 0.9999). These results suggest that alkaline synthesis enhances particle morphology and charge transfer efficiency, improving photocatalytic performance. Therefore, Fe₃O₄–NaOH:TiO₂ represents a promising candidate for cypermethrin remediation in wastewater treatment.References
Zeshan, M. , Bhatti, I. A. , Mohsin, M. , Iqbal, M. , Amjed, N. , Nisar, J. , AlMasoud, N. , and Alomar, T. S. , Remediation of pesticides using TiO2 based photocatalytic strategies: A review, Chemosphere, 300(March), pp.134525, 2022.
Kansal, I. , Kapoor, A. , Solanki, S. , and Singh, R. , Cypermethrin toxicity in the environment: analytical insight into detection methods and microbial degradation pathways, Journal of Applied Microbiology, 134(6), pp.1–12, 2023.
Environment Agency , Cypermethrin: Sources, pathways and environmental data, Bristol, (October), 2019.
Bisaria, K. , Sinha, S. , Singh, R. , and Iqbal, H. M. N. , Recent advances in structural modifications of photocatalysts for organic pollutants degradation – A comprehensive review, Chemosphere, 284(June), pp.131263, 2021.
Kalidhasan, S. and Lee, H. Y. , Preparation of TiO2-deposited silica-based catalysts for photocatalytic decomposition of chloro-pesticide to environmentally less toxic species, Chemosphere, 290(December 2021), pp.133300, 2022.
Celia, C., Marsooli, M. A., Rahimi-nasrabadi, M., and Fasihi-ramandi, M. , Preparation of Fe3O4/ SiO2/TiO2/CeVO4 Nanocomposites: Investigation of Photocatalytic Effects on Organic Pollutants , Bacterial Environments , and New Potential Therapeutic Candidate Against Cancer Cells11(March), pp.1–15, 2020.
Hernandez-Del, C. P. C. , Oliva, J. , and Rodriguez-Gonzalez, V. , An eco-friendly and sustainable support of agave-fibers functionalized with graphene / TiO2 : SnO2 for the photocatalytic degradation of the 2 , 4-D herbicide from the drinking water, Journal of Environmental Management, 317 (11551(January), 2022.
Djellabi, R. , Yang, B. , Adeel Sharif, H. M. , Zhang, J. , Ali, J. , and Zhao, X. , Sustainable and easy recoverable magnetic TiO2-Lignocellulosic Biomass@Fe3O4 for solar photocatalytic water remediation, Journal of Cleaner Production, 233pp.841–847, 2019.
Iman Amir, M. N. , Julkapli, N. M. , Bagheri, S. , and Yousefi, A. T. , TiO2 hybrid photocatalytic systems: Impact of adsorption and photocatalytic performance, Reviews in Inorganic Chemistry, 35(3), pp.151–178, 2015.
Balassa, L. , Ãgoston, Ã. , Kása, Z. , Hornok, V. , and Janovák, L. , Surface sulfate modified TiO2 visible light active photocatalyst for complex wastewater purification: Preparation, characterization and photocatalytic activity, Journal of Molecular Structure, 1260pp.132860, 2022.
Ismael, M. , Latest progress on the key operating parameters affecting the photocatalytic activity of TiO2-based photocatalysts for hydrogen fuel production: A comprehensive review, Fuel, 303(April), pp.121207, 2021.
Harifi, T. and Montazer, M. , A novel magnetic reusable nanocomposite with enhanced photocatalytic activities for dye degradation, Separation and Purification Technology, 134pp.210–219, 2014.
Khashan, S. , Dagher, S. , Tit, N. , Alazzam, A. , and Obaidat, I. , Novel method for synthesis of Fe3O4@TiO2 core/shell nanoparticles, Surface and Coatings Technology, 322pp.92–98, 2017.
Beduk, F. , Superparamagnetic nanomaterial Fe3O4–TiO2 for the removal of As(V) and As(III) from aqueous solutions, Environmental Technology, 37(14), pp.1790–1801, 2016.
Nengsih, S. , Nur Abdulmadjid, S. , Mursal, M. , and Jalil, Z. , Photocatalytic performance of Fe3O4-TiO2 in the degradation of methylene blue dye: Optimizing the usability of natural iron sand, Materials Science for Energy Technologies, 7(May), pp.374–380, 2024.
Kubiak, A. , Comparative study of TiO2–Fe3O4 photocatalysts synthesized by conventional and microwave methods for metronidazole removal, Scientific Reports, 13(1), pp.1–13, 2023.
MirzaHedayat, B. , Noorisepehr, M. , Dehghanifard, E. , Esrafili, A. , and Norozi, R. , Evaluation of photocatalytic degradation of 2,4-Dinitrophenol from synthetic wastewater using Fe3O4@SiO2@TiO2/rGO magnetic nanoparticles, Journal of Molecular Liquids, 264pp.571–578, 2018.
Zhao, X. , Wang, R. , Lu, Z. , Wang, W. , and Yan, Y. , Dual sensitization effect and conductive structure of Fe3O4@mTiO2/C photocatalyst towards superior photodegradation activity for bisphenol A under visible light, Journal of Photochemistry and Photobiology A: Chemistry, 382pp.111902, 2019.
Fawzi Suleiman Khasawneh, O. and Palaniandy, P. , Removal of organic pollutants from water by Fe2O3/TiO2 based photocatalytic degradation: A review, Environmental Technology and Innovation, 21pp.101230, 2021.
Jesus, A. C. B. , Jesus, J. R. , Lima, R. J. S. , Moura, K. O. , Almeida, J. M. A. , Duque, J. G. S. , and Meneses, C. T. , Synthesis and magnetic interaction on concentrated Fe3O4 nanoparticles obtained by the co-precipitation and hydrothermal chemical methods, Ceramics International, 46(8), pp.11149–11153, 2020.
RadoÅ„, A. , DrygaÅ‚a, A. , HaweÅ‚ek, Å. , and Åukowiec, D. , Structure and optical properties of Fe3O4 nanoparticles synthesized by co-precipitation method with different organic modifiers, Materials Characterization, 131pp.148–156, 2017.
Rahmawati, R. , Permana, M. G. , Harison, B. , Nugraha , Yuliarto, B. , Suyatman , and Kurniadi, D. , Optimization of Frequency and Stirring Rate for Synthesis of Magnetite (Fe3O4) Nanoparticles by Using Coprecipitation- Ultrasonic Irradiation Methods, Procedia Engineering, 170pp.55–59, 2017.
Nengsih, S. , Madjid, S. N. , Mursal , and Jalil, Z. , Synthesis and characterization of magnetite particles from Syiah Kuala iron sand prepared by co-precipitation method, Journal of Physics: Conference Series, 2582(012005), pp.1–7, 2023.
Venkateswarlu, S. , Kumar, B. N. , Prathima, B. , SubbaRao, Y. , and Jyothi, N. V. V. , A novel green synthesis of Fe 3 O 4 magnetic nanorods using Punica Granatum rind extract and its application for removal of Pb(II) from aqueous environment, Arabian Journal of Chemistry, 12(4), pp.588–596, 2019.
Zhang, Q. , Yu, L. , Xu, C. , Zhang, W. , Chen, M. , Xu, Q. , and Diao, G. , A novel method for facile preparation of recoverable Fe3O4@TiO2 core-shell nanospheres and their advanced photocatalytic application, Chemical Physics Letters, 761(August), 2020.
Afzal, S. , Julkapli, N. M. , and Mun, L. K. , Visible light active TiO2/CS/Fe3O4 for nitrophenol degradation: Studying impact of TiO2, CS and Fe3O4 loading on the optical and photocatalytic performance of nanocomposite, Materials Science in Semiconductor Processing, 131(November 2020), pp.105891, 2021.
Mufti, N. , Munfarriha, U. , Fuad, A. , and Diantoro, M. , Synthesis and photocatalytic properties of Fe3O4@TiO2 core-shell for degradation of Rhodamine B, AIP Conference Proceedings, 1712(February 2016), 2016.
Govindhan, P. , Pragathiswaran, C. , and Chinnadurai, M. , A magnetic Fe3O4 decorated TiO2 nanoparticles application for photocatalytic degradation of methylene blue (MB) under direct sunlight irradiation, Journal of Materials Science: Materials in Electronics, 29(8), pp.6458–6469, 2018.
Heryanto, H. and Tahir, D. , The correlations between structural and optical properties of magnetite nanoparticles synthesised from natural iron sand, Ceramics International, 47(12), pp.16820–16827, 2021.
Rahmayanti, M. , Santosa, S. J. , Sutarno, S. , Hamidi, H. , and Binagara, L. , Synthesis, Characterization, and Application of Magnetite (Fe3O4) Particles as Gold Adsorbent from Simulation Waste, CHEMICA: Jurnal Teknik Kimia, 7(2), pp.151, 2021.
Nengsih, S. , Karakteristik Nanopartikel Magnetite Besi Oksida Lampanah Aceh Besar Melalui Metode Kopresipitasi, Elkawnie, 5(1), pp.76, 2019.
Nengsih, S. , Abdulmajid, S. N. , Mursal , and Jalil, Z. , Magnetization Study of Iron Sand from Sabang , Indonesia : The Potential of Magnetic Materials in the, Bulletin of Chemical Reaction Engineering & Catalysis (BCREC), 18(2), pp.344–352, 2023.
Sunaryono , Taufiq, A. , Mashuri , Pratapa, S. , Zainuri, M. , Triwikantoro , and Darminto , Various magnetic properties of magnetite nanoparticles synthesized from iron-sands by coprecipitation method at room temperature, Materials Science Forum, 827(June), pp.229–234, 2015.
Mufti, N. , Atma, T. , Fuad, A. , and Sutadji, E. , Synthesis And Characterization Of Black , Red And Yellow Nanoparticles Pigments From The Iron Sand, AIP Conference Proceeding, 165(2014), 2018.
Liu, H. and Valentin, C. Di , Band Gap in Magnetite above Verwey Temperature Induced by Symmetry Breaking, The Journal of Physical Chemistry C, 121(46), pp.25736–25742, 2017.
Priyadarshana, G. , Kottegoda, N. , Senaratne, A. , Alwis, A. De , and Karunaratne, V. , Synthesis of magnetite nanoparticles by top-down approach from a high purity ore, Journal of Nanomaterials, 20152015.
Vinosel, V. M. , Anand, S. , Janifer, M. A. , Pauline, S. , Dhanavel, S. , Praveena, P. , and Stephen, A. , Preparation and performance of Fe3O4/TiO2 nanocomposite with enhanced photo-Fenton activity for photocatalysis by facile hydrothermal method, Applied Physics A: Materials Science and Processing, 125(5), pp.1–13, 2019.
AbouSeada, N. , Ahmed, M. A. , and Elmahgary, M. G. , Synthesis and characterization of novel magnetic nanoparticles for photocatalytic degradation of indigo carmine dye, Materials Science for Energy Technologies, 5pp.116–124, 2022.
Al-Salihi, S. , Bayati, M. , Jasim, A. M. , Fidalgo, M. M. , and Xing, Y. , Magnetic mesoporous TiO2/Fe3O4 nanocomposite adsorbent for removal of sulfamethazine from water, Environmental Advances, 9(August), pp.100283, 2022.
Nkurikiyimfura, I. , Wang, Y. , Safari, B. , and Nshingabigwi, E. , Temperature-dependent magnetic properties of magnetite nanoparticles synthesized via coprecipitation method, Journal of Alloys and Compounds, 8462020.
Dubey, M. , Kumar, R. , Srivastava, S. K. , and Joshi, M. , Visible light induced photodegradation of chlorinated organic pollutants using highly efficient magnetic Fe3O4/TiO2 nanocomposite, Optik, 243pp.167309, 2021.
Wang, X. , Sø, L. , Su, R. , Wendt, S. , Hald, P. , Mamakhel, A. , Yang, C. , Huang, Y. , Iversen, B. , and Besenbacher, F. , The influence of crystallite size and crystallinity of anatase nanoparticles on the photo-degradation of phenol, Journal of Catalysis, 310pp.100–108, 2014.
Jiang, Q. and Zhu, R. , Facile synthesis of highly efficient and cost-effective photo-Fenton catalyst by ball milling commercial TiO2 and natural magnetite, Journal of Alloys and Compounds, 862pp.158670, 2021.
Iwasaki, T. , Mizutani, N. , Watano, S. , Yanagida, T. , and Kawai, T. , Size control of magnetite nanoparticles by organic solvent-free chemical coprecipitation at room temperature, Journal of Experimental Nanoscience, 5(3), pp.251–262, 2010.
Baumgartner, J. , Bertinetti, L. , Widdrat, M. , Hirt, A. M. , and Faivre, D. , Formation of Magnetite Nanoparticles at Low Temperature: From Superparamagnetic to Stable Single Domain Particles, PLoS ONE, 8(3), pp.1–6, 2013.
Shaheed, I. M. and Dhahir, S. A. , Extraction and determination of alpha-Cypermethrin in environmental samples from Kerbala city / Iraq and in its formulation using high performance liquid chromatography (HPLC)., IOP Conference Series: Materials Science and Engineering, 871(1), 2020.
Kunarti, E. S. , Kartini, I. , Syoufian, A. , and Widyandari, K. M. , Syntehsis and Photoactivity of Fe3O4/TiO2-Co as a Magnetically Separable Visible Light Responsive Photocatalyst, Indonesian Journal of Chemistry, 18(3), pp.403–410, 2018.
Gunlazuardi, J. , Fisli, A. , Ridwan , Krisnandi, Y. K. , and Robert, D. , Magnetically Separable Fe3O4/SiO2/TiO2 Photocatalyst Composites Prepared through Hetero Agglomeration for the Photocatalytic Degradation of Paraquat, Makara Journal of Science, 25(4), pp.236–246, 2021.
Mansour, H. , Omri, K. , Bargougui, R. , and Ammar, S. , Novel α-Fe2O3/TiO2 nanocomposites with enhanced photocatalytic activity, Applied Physics A: Materials Science and Processing, 126(3), 2020.
Mu, Q. , Sun, Y. , Guo, A. , Yu, X. , Xu, X. , Cai, A. , and Wang, X. , Biolated synthesis of Fe3O4-TiO2 composites derived from Chlorella pyrenoidosa with enhanced visible-light photocatalytic performance, Materials Research Express, 6(9), 2019.
Hong, T. , Mao, J. , Tao, F. , and Lan, M. , Recyclable magnetic titania nanocomposite from ilmenite with enhanced photocatalytic activity, Molecules, 22(12), 2017.
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