Characterization of Low-Cost Multi-Precursor Ceramic Membranes from Nigerian Agricultural and Biogenic Wastes for Synergistic Removal of Heavy Metals and Azo Dyes from Wastewater
DOI:
https://doi.org/10.61424/ijans.v4i1.765Keywords:
Low-cost ceramic membranes; multi-precursor; Nigerian waste materials; heavy metal removal; azo dye rejection; wastewater treatment; membrane characterization; sustainable optimizationAbstract
The contamination of water resources by heavy metals and recalcitrant azo dyes from textile and industrial effluents remains a critical environmental and public-health challenge, particularly in developing regions. Conventional ceramic membranes, while effective, are often prohibitively expensive due to high-purity raw materials. This study reports the optimized fabrication of a novel low-cost multi-precursor ceramic membrane using abundant, locally sourced Nigerian wastes and natural materials—sawdust, rice husk, snail shell, kaolin clay, and natural clay. Raw materials were pretreated, homogeneously mixed with binders and additives (boric acid, PVA, PEG, CTAB), uniaxially pressed into flat disks (40 mm diameter, 3 mm thickness), and subjected to controlled two-stage sintering. A top-layer coating of fine clay suspension (<2 µm) was applied to enhance selectivity. Comprehensive characterization of both precursors and the final membrane (optimal Sample 25) was performed using EDX, SEM, XRD, FTIR, TG-DTA, XRF, and BET surface-area analysis. The optimized membrane exhibited a high BET surface area of 255.52 m²/g, a hierarchical micro-mesoporous structure, crystalline phases including quartz, kaolinite, and zeolite, and surface functional groups (Si–O–Si, O–H, C–O) conducive to adsorption and ion exchange. SEM revealed irregular, porous morphologies ideal for high permeability and antifouling, while thermal analysis confirmed structural stability up to sintering temperatures. These properties support synergistic pollutant removal through size exclusion, electrostatic repulsion, adsorption, and Donnan exclusion. The developed membrane, integrated into a custom CAD-designed stainless-steel filtration unit, offers a sustainable, circular-economy approach that valorizes agricultural and biogenic wastes, significantly reduces production costs compared with commercial alumina/zirconia membranes, and aligns with UN Sustainable Development Goals for clean water and sanitation. This work provides a scalable, low-energy fabrication pathway for advanced ceramic membranes tailored for simultaneous heavy-metal and azo-dye remediation in real wastewater matrices.
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References
Adeniyi, F. I., Ogundiran, M. B., Hemalatha, T., & Hanumantrai, B. B. (2020). Characterization of raw and thermally treated Nigerian kaolinite-containing clays using instrumental techniques. SN Applied Sciences, *2*(5), 821. https://doi.org/10.1007/s42452-020-2610-x
Akoumeh, R., Al-Ejji, M., Aljaoni, B and Abbas, M. (2025). Advances in ceramic membrane technology: Versatility of fabrication technique, industrial applications, and challenges, Inorg. Chem. Commun., vol. 179. 114685, doi: 10.1016/j.inoche.2025.114685.
Abhisek, K., Vhatkar, S.S., Mathew, H.T., Singh P and Oraon, R. (2025). A critical review on the challenges and techno-economic assessment of dyes removal technologies from wastewater, Discov. Chem., 2(1). 1–37, doi: 10.1007/s44371-025-00111-4.
Abu-Dief, A.M., Alsaedi W.H and Zikry M.M. (2025). A collective study on the fabrication of nano-materials for water treatment, J. Umm Al-Qura Univ. Appl. Sci., doi: 10.1007/s43994-025-00227-4.
Boussemghoune, A., Chihi, S., & Benmounah, A. (2020). Microstructural and mechanical properties of fired clay bricks incorporating natural waste materials. Journal of Building Engineering, *32*, 101–112.
Bensalah, H., Derouich, G., Wang, X., Alami Younssi S and Bekheet, M.F. (2023). Graphene-Oxide-Grafted Natural Phosphate Support as a Low-Cost Ceramic Membrane for the Removal of Anionic Dyes from Simulated Textile Effluent, Membranes, 13(3). 345, doi: 10.3390/membranes13030345.
El Ouahabi, M., Daoudi, L., Hatert, F., & Fagel, N. (2015). Modified mineral phases during clay ceramic firing. Clays and Clay Minerals, *63*(5), 404–413. https://doi.org/10.1346/CCMN.2015.0630506
Hossain, S. S., Mathur, L., & Roy, P. K. (2018). Rice husk/rice husk ash as an alternative source of silica in ceramics: A review. Journal of Asian Ceramic Societies, *6*(4), 299–313. https://doi.org/10.1080/21870764.2018.1539210
Ihekweme, G. O., Shondo, J. N., Orisekeh, K. I., Kalu-Uka, G. M., Nwuzor, I. C., & Onwualu, A. P. (2020). Characterization of certain Nigerian clay minerals for water purification and other industrial applications. Heliyon, *6*(4), e03783. https://doi.org/10.1016/j.heliyon.2020.e03783
Jannat, N., Latif Al-Mufti, R., Hussien, A., Abdullah, B., & Cotgrave, A. (2021). Influence of sawdust particle sizes on the physico-mechanical properties of unfired clay blocks. Designs, *5*(3), 57. https://doi.org/10.3390/designs5030057
Jarrar, R., Abbas M.K.G and Al-Ejji, M. (2024). Environmental remediation and the efficacy of ceramic membranes in wastewater treatment—a review, Emergent Mater., 7(4). 1295–1327, Aug. 2024, doi: 10.1007/s42247-024-00687-0.
Jonathan, K. M., Kuria, K. P., Mwangi, G. J., & Gichuki, N. F. (2020). Characterization of rice husk ash prepared by open air burning and furnace calcination. Journal of Chemical Engineering and Materials Science, *11*(2), 21–30. https://doi.org/10.5897/JCEMS2020.0348
Kirk, C.H., Wang, P., Chong, C.Y.D., Zhao, Q., Sun J and Wang, J., (2024). TiO2 photocatalytic ceramic membranes for water and wastewater treatment: Technical readiness and pathway ahead, J. Mater. Sci. Technol. 152–164, June, doi: 10.1016/j.jmst.2023.09.055.
Marques, A. V. S., Barbosa, A. dos S., Maia, L. F., Rodrigues, M. G. F., Lins Almeida Barbosa, T., & Luna, C. B. B. (2025). Development and characterization of sawdust-based ceramic membranes for textile effluent treatment. Membranes, *15*(10), 298. https://doi.org/10.3390/membranes15100298
Malebadi, K.A., Sawunyama, L., Seheri N.H and Onwudiwe, D.C. (2025). Application of Ceramic Membranes Derived from Waste and Natural Materials for the Removal of Organic Dyes from Wastewater: A Review, Ceramics, 8(3). 80, doi: 10.3390/ceramics8030080.
Mgbemere, H., Ekpe, I., Lawal, G., Ovri, H., & Chaudhary, A.-L. (2019). Preparation and characterization of zeolite type 4A using kaolin from Ajebo, Nigeria. Pertanika Journal of Science and Technology, *27*(4), 1865–1878.
Mohamed Ariff, A. H., Othman, M. H. D., Tai, Z. S., Hubadillah, S. K., & Ismail, A. F. (2022). Rice husk-derived silica-based ceramic membranes for water treatment: A review. Journal of the European Ceramic Society, *42*(5), 1893–1912.
Obada, D. O., Dodoo-Arhin, D., Dauda, M., Anafi, F. O., Ahmed, A. S., & Ajayi, O. A. (2017). The impact of kaolin dehydroxylation on the porosity and mechanical integrity of kaolin-based ceramics using different pore formers. Results in Physics, *7*, 2718–2727. https://doi.org/10.1016/j.rinp.2017.07.048
Olorunnisola C.G. (2025). Clay-based photocatalytic membranes: low-cost alternative materials for water treatment,” Mater. Adv., 6(14). 4623–4645, 2025, doi: 10.1039/D5MA00313J.
Onyenanu C.N and Nwabanne, J.T. (2025) Application of Ceramic Membranes for the Removal of Heavy Metals and Dyes: Efficiency and Performance Review, Res. J. Civ. Ind. Mech. Eng., vol. 2, no. 2, pp. 84–98, 2025, doi: DOI:2010.61424/rjcime.v2i2.338.
Oshani, F., Kargari, A., Norouzbeigi, R., & Mahmoodi, N. M. (2025). Performance optimization and fouling study of geopolymer-zeolite composite membranes for sustainable textile wastewater treatment. Scientific Reports, *15*(1), 35463. https://doi.org/10.1038/s41598-025-19349-0
Onyenanu C.N and Onyenanu, I.U. (2025). Advanced Treatment Technologies for Heavy Metal Removal from Water and Wastewater: A Comprehensive Review, IJANS, vol. 3, no. 2, pp. 111–131, Jun. 2025.
Parveen, S., Chakraborty, A., Chanda, D. K., Pramanik, S., Barik, A., & Aditya, G. (2020). Microstructure analysis and chemical and mechanical characterization of the shells of three freshwater snails. ACS Omega, *5*(40), 25757–25771. https://doi.org/10.1021/acsomega.0c03064
Podaralla, N. K., Paramasivam, P., & Jacquemin, J. (2024). Characterization of hydrothermally decomposed and synthesized CaCO₃ reinforcement from dead snail shells. ACS Omega, *9*(2), 2183–2191. https://doi.org/10.1021/acsomega.3c05330
Prabhakar, N., Isloor, A.M., Farnood R and Ismail, A.F. (2025). Efficient removal of hazardous dyes/heavy-metal ions by in-house fabricated poly (vinylidene fluoride) thin-film nanocomposite membranes with functionalized Zr-based metal-organic framework, J. Environ. Chem. Eng., vol. 13, no. 3, p. 116434, doi: 10.1016/j.jece.2025.116434.
Ramanamane, K. P., Kaseka, P. K., & Nkosi, S. S. (2024). Hierarchical mesoporous materials from clay and rice husk for wastewater treatment applications. Journal of Porous Materials, *31*(3), 789–802.
Rakcho Y et al. (2025). Fabrication of low-cost ceramic nanofiltration membrane from natural resources for the removal of cationic and anionic dyes: Experimental and DFT investigations, Chem. Eng. J. 159779, doi: 10.1016/j.cej.2025.159779.
Schackow, A., Stringari, D., Senff, L., Correia, S. L., & Segadães, A. M. (2020). Influence of firing temperature on the physical and mechanical properties of red ceramic. Ceramics International, *46*(10), 15678–15685.
Santra, B., Ramrakhiani, L., Kar, S. Ghosh, S and Majumdar, S. (2020). Ceramic membrane-based ultrafiltration combined with adsorption by waste-derived biochar for textile effluent treatment and management of spent biochar, J. Environ. Health Sci. Eng., 18(2). 973–992, doi: 10.1007/s40201-020-00520-w.
Sandhya Rani S.L and Kumar, R.V. (2021). Insights on applications of low-cost ceramic membranes in wastewater treatment: A mini-review, Case Stud. Chem. Environ. Eng., p. 100149, Dec., doi: 10.1016/j.cscee.2021.100149.
Sawunyama, L., Olatunde, O.C., Oyewo, O.A., Bopape, M.F and Onwudiwe, D.C. (2024). Application of coal fly ash-based ceramic membranes in wastewater treatment: A sustainable alternative to commercial materials,” Heliyon, vol. 10, no. 2, p. e24344, Jan. 2024, doi: 10.1016/j.heliyon. 2024.e24344.
Solaiman, J.M., Rajamohan, N., Yusuf M and Kamyab, H. (2024). Nanocomposite ceramic membranes as novel tools for remediation of textile dye waste water – A review of current applications, machine learning based modeling and future perspectives,” J. Environ. Chem. Eng., vol. 12(2) 112353, doi: 10.1016/j.jece.2024.112353.
Serra, M. F., Conconi, M. S., Gauna, M. R., Suárez, G., Aglietti, E. F., & Rendtorff, N. M. (2016). Mullite (3Al₂O₃·2SiO₂) ceramics obtained by reaction sintering of rice husk ash and alumina, phase evolution, sintering, and microstructure. Journal of Asian Ceramic Societies, *4*(1), 61–67. https://doi.org/10.1016/j.jascer.2015.11.003
Thiedeitz, M., Schmidt, W., & Härder, M. (2020). Rice husk ash as a sustainable pozzolan in concrete: A review. Construction and Building Materials, *263*, 120–132.
Tripathi M et al. (2023). Recent Strategies for the Remediation of Textile Dyes from Wastewater: A Systematic Review, Toxics, 11(11). 940, doi: 10.3390/toxics11110940.
Tayara, A., Shang, C., Zhao J and Xiang, Y. (2024). Machine learning models for predicting the rejection of organic pollutants by forward osmosis and reverse osmosis membranes and unveiling the rejection mechanisms, Water Res., 266. 122363, doi: 10.1016/j.watres.2024.122363.
Velusamy, S., Roy, A., Sundaram S and Kumar Mallick T. (2021) A Review on Heavy Metal Ions and Containing Dyes Removal Through Graphene Oxide-Based Adsorption Strategies for Textile Wastewater Treatment, Chem. Rec., 21(7). 1570–1610, 2021, doi: 10.1002/tcr. 202000153.
Wang, X., Wang, M. Chen M and Zhang, Y. (2023). A Mini Review of Ceramic-Based MOF Membranes for Water Treatment, Membranes, 13(9). 751, doi: 10.3390/membranes13090751.
Xu, W., Lo, T. Y., & Memon, S. A. (2012). Microstructure and reactivity of rich husk ash. Construction and Building Materials, *29*, 541–547. https://doi.org/10.1016/j.conbuildmat.2011.11.005
Yang, Y., Wang, L., & Zhang, J. (2023). Morphological characterization of kaolinite using SEM and AFM techniques. Applied Clay Science, *235*, 106–118.
Ye Y et al. (2025). Integrating artificial intelligence with mechanistic epidemiological modeling: a scoping review of opportunities and challenges, Nat. Commun., 16(581), doi: 10.1038/s41467-024-55461-x.
Yepes, J. L., Torres, A., & Muñoz, F. (2011). Morphological characterization of wood dust particles. Wood Science and Technology, *45*(4), 621–634.
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