HF-free dry gel synthesis of MIL-100(Fe) for adsorptive removal of salicylic acid in wastewater treatment
DOI:
https://doi.org/10.24191/mjcet.v8i2.5013Keywords:
Adsorption, Dry gel conversion, MIL-100(FE), Salicylic acid, Wastewater treatmentAbstract
This study reports an HF-free dry-gel conversion route to synthesise MIL-100(Fe) and evaluate its performance for adsorptive removal of salicylic acid from wastewater. Comprehensive characterisation of the material was conducted using XRD, FT-IR, FESEM and zeta potential. The dry gel conversion method successfully produced MIL-100(Fe) with an amorphous structure with an average particle size of 27 μm. Adsorption experiments achieved a maximum salicylic acid removal efficiency of 82.62% across the tested range (10 to 50 µg/mL), corresponding to an adsorption capacity of 80.93 mg/g at 120 minutes. Significant reductions in FT-IR peaks associated with carboxylic acid O–H stretching vibrations were observed, particularly in regions 3600 to 4000 cm−1 and 2500 to 3600 cm−1. These changes indicate strong interactions between the carboxyl groups of salicylic acid and the active sites on the MIL-100(Fe) surface, confirming effective adsorption and removal of salicylic acid. These findings demonstrate that MIL-100(Fe) synthesised through a hydrofluoric acid-free dry gel conversion route is an effective and environmentally benign adsorbent for the removal of pharmaceutical pollutants from wastewater.
References
Abdel-Rahman, F. A., Khafagi, E. Y., Soliman, M. S., Shoala, T., & Ahmed, Y. (2021). Preharvest application of salicylic acid induces some resistant genes of sweet pepper against black mold disease. European Journal of Plant Pathology, 159(4), 755–768. https://doi.org/10.1007/s10658-020-02199-z
Ashara, K. C., & Shah, K. V. (2017). Nuts and bolts of oil and temperature in topical preparations of salicylic acid. Folia Medica, 59(3), 279–288. https://doi.org/10.1515/folmed-2017-0034
Chakraborty, A., Adhikary, S., Bhattacharya, S., Dutta, S., Chatterjee, S., Banerjee, D., Ganguly, A., & Rajak, P. (2023). Pharmaceuticals and personal care products as emerging environmental contaminants: Prevalence, toxicity, and remedial approaches. ACS Chemical Health and Safety, 30(6), 362–388. https://doi.org/10.1021/acs.chas.3c00071
Daginnus, K., Gottardo, S., Payá-Pérez, A., Whitehouse, P., Wilkinson, H., & Zaldívar, J. M. (2011). A model-based prioritisation exercise for the European Water Framework Directive. International Journal of Environmental Research and Public Health, 8(2), 435–455. https://doi.org/10.3390/ijerph8020435
Duan, S., Li, J., Liu, X., Wang, Y., Zeng, S., Shao, D., & Hayat, T. (2016). HF-free synthesis of nanoscale metal-organic framework NMIL-100(Fe) as an efficient dye adsorbent. ACS Sustainable Chemistry and Engineering, 4(6), 3368–3378. https://doi.org/10.1021/acssuschemeng.6b00434
He, Z., Meng, M., Yan, L., Zhu, W., Sun, F., Yan, Y., Liu, Y., & Liu, S. (2015). Fabrication of new cellulose acetate blend imprinted membrane assisted with ionic liquid ([BMIM]Cl) for selective adsorption of salicylic acid from industrial wastewater. Separation and Purification Technology, 145, 63–74. https://doi.org/10.1016/j.seppur.2015.03.005
Hijosa-Valsero, M., Matamoros, V., Pedescoll, A., Martín-Villacorta, J., Bécares, E., García, J., & Bayona, J. M. (2011). Evaluation of primary treatment and loading regimes in the removal of pharmaceuticals and personal care products from urban wastewaters by subsurface-flow constructed wetlands. International Journal of Environmental Analytical Chemistry, 91(7–8), 632–653. https://doi.org/10.1080/03067319.2010.526208
Idrees, M., Mastronardo, E., Piperopoulous, E., Milone, C., Calabrese, L. (2025). Impact of HF-free synthesis modification on purity and adsorption performance of MOF MIL-100(Fe) for gas capture and energy storage applications. Applied Sciences, 15(11), 6097. https://doi.org/10.3390/app15116097
Li, W., Zhang, T., Lv, L., Chen, Y., Tang, W., & Tang, S. (2021). Room-temperature synthesis of MIL-100(Fe) and its adsorption performance for fluoride removal from water. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 624, 126791. https://doi.org/10.1016/j.colsurfa.2021.126791
Luo, Y., Tan, B., Liang, X., Wang, S., Gao, X., Zhang, Z., & Fang, Y. (2019). Dry gel conversion synthesis of hierarchical porous MIL-100(Fe) and its water vapor adsorption/desorption performance. Industrial and Engineering Chemistry Research, 58(19), 7801–7807. https://doi.org/10.1021/acs.iecr.9b01647
Muñoz-Senmache, J. C., Kim, S., Arrieta-Pérez, R. R., Park, C. M., Yoon, Y., & Hernández-Maldonado, A. J. (2020). Activated carbon–metal organic framework composite for the adsorption of contaminants of emerging concern from water. ACS Applied Nano Materials, 3(3), 2928–2940. https://doi.org/10.1021/acsanm.0c00190
Rojas, S., & Horcajada, P. (2020). Metal-organic frameworks for the removal of emerging organic contaminants in water. Chemical Reviews, 120(16), 8378–8415. https://doi.org/10.1021/acs.chemrev.9b00797
Sivanesan, J., Rameshwar S. S., Sivaprakash, B., Rajamohan, N., Osman, A. I., Al-Muhtasesb, A. (2024). Advanced methods for treating gemfibroil and carbamazepine in wastewater:A review, Environmental Chemistry Letters, 22, 3171–3194. https://doi.org/10.1007/s10311-024-01765-9
Siyal, A. A., Mohamed R., Ahmad, F., Abdul Malek, M., Alsubih, M., Shamsuddin, R., Hussain, S., Musa, S. (2025) A review of the developments in adsorbents for the efficient adsorption of ibuprofen from wastewater, RSC Advances, 15, 17843–17861. https://doi.org/10.1039/D5RA02007G
Ślósarczyk, K., Jakóbczyk-Karpierz, S., Różkowski, J., & Witkowski, A. J. (2021). Occurrence of pharmaceuticals and personal care products in the water environment of Poland: A review. Water (Switzerland), 13(16). https://doi.org/10.3390/w13162283
Sobhani, D., Djahaniani, H., Duong, A., & Kazemian, H. (2024). Efficient removal of microcystin-LR from contaminated water using water-stable MIL-100(Fe) synthesized under HF-free conditions. Environmental Science and Pollution Research, 31(16), 24512–24524. https://doi.org/10.1007/s11356-024-32675-6
Taherzade, S. D., Abbasichaleshtori, M., Soleimannejad, J. (2022). Efficient and ecofriendly cellulose-supported MIL-100(Fe) for wastewater treatment. RSC Advances, 12, 9023-9035. https://doi.org/10.1039/D1RA08949H
Tran, N. H., Reinhard, M., & Gin, K. Y. H. (2018). Occurrence and fate of emerging contaminants in municipal wastewater treatment plants from different geographical regions-a review. In Water Research (Vol. 133). Elsevier. https://doi.org/10.1016/j.watres.2017.12.029
White, B., Banerjee, S., Brien, S. O., Turro, N. J., & Herman, I. P. (2007). Zeta-potential measurements of surfactant-wrapped individual single-walled carbon nanotubes. Journal of Physical Chemistry C, 2(1), 13684–13690. https://doi.org/10.1021/jp070853e
Zhi, K., Xu, J., Li, S., Luo, L., Liu, D., Li, Z., Guo, L., Hou, J. (2024). Progress in the elimination of organic contaminants in wastewater by activation persulfate over iron-based metal-organic frameworks. Nanomaterials (Basel), 14(5), 473. https://doi.org/10.3390/nano14050473
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