Microwave/ultrasound-assisted synthesis of an Fe(III)-coordinated oxazolone–polyamide metallopolymer for coordination-driven Cu(II) removal from water
8 affiliations
- 1Department of Pharmaceutical Sciences, Faculty of Pharmacy, Umm Al-Qura University, Makkah, 21955, Saudi Arabia
- 2Department of Chemistry, College of Science, King Faisal University, Al-Ahsa, 31982, Saudi Arabia
- 3Department of Chemistry, Faculty of Science, Umm Al-Qura University, Makkah, 21955, Saudi Arabia
- 4Department of Chemistry, College of Science, Northern Border University, Arar, 91431, Saudi Arabia
- 5Department of Chemistry, Science Faculty, Ain Shams University, Cairo, 11566, Egypt
- 6Department of Green Chemistry, National Research Centre, Dokki, P.O. Box 12622, Cairo, Egypt
- 7Chemistry Department, College of Science, Imam Mohammad Ibn Saud Islamic University (IMSIU), Riyadh, 11623, Saudi Arabia
- 8Chemistry Department , Faculty of Science, Assiut University, Assiut, 71516, Egypt
Abstract
This study investigated the microwave/ultrasound-assisted synthesis of a new O/N-rich oxazolone–polyamide framework and its Fe(III)-coordinated metallopolymer for Cu(II) removal from aqueous solution. The oxazolone precursor was prepared using microwave irradiation at 300 W for 10-15 min, followed by ultrasound activation at 40 kHz for 20 min, giving a yield of approximately 70%, while the reduced diamine monomer was obtained in 66% yield. The resulting NH-OXAZAM-CO polymer was further coordinated with Fe(III) to produce Fe-(NH-OXAZAM-CO), containing abundant amide, oxazolone, carbonyl, and nitrogen donor sites. The prepared materials were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy with energy-dispersive X-ray analysis, X-ray diffraction, thermogravimetric analysis, X-ray photoelectron spectroscopy, and density functional theory calculations. Cu(II) adsorption was evaluated using synthetic CuSO 4 solutions under controlled conditions: adsorbent dose 1.0 g L −1 , particle size 125–250 μm, initial Cu(II) concentration 10–50 mg L −1 , pH 5.5 ± 0.1, ionic strength 0.01 M NaNO 3 , and temperature 25 ± 1 °C. The Langmuir model provided the best fit, with a maximum adsorption capacity of 54.9 mg/g, a Langmuir constant of 0.1689, a separation factor of 0.10, and a correlation coefficient of R 2 = 0.9999, confirming favorable monolayer adsorption on finite active sites. The Temkin model also showed acceptable fitting (R 2 = 0.9701), indicating adsorbent–adsorbate interactions, whereas the Dubinin–Radushkevich model gave an adsorption energy of 1.16 kJ mol −1 , suggesting that weak physical interactions contribute to the initial uptake stage. Spectroscopic evidence from infrared and X-ray photoelectron analyses confirmed Cu(II) binding through oxygen and nitrogen donor sites, while computational descriptors supported the role of electron-rich coordination centers in metal-ion capture. Overall, the study demonstrates that Fe(III)-modified oxazolone–polyamide metallopolymers are promising coordination-based adsorbents for Cu(II)-contaminated water treatment.
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BibTeX
@article{almalki2026microwaveultrasoundassisted,
title = {{Microwave/ultrasound-assisted synthesis of an Fe(III)-coordinated oxazolone–polyamide metallopolymer for coordination-driven Cu(II) removal from water}},
author = {Faisal A. Almalki and Faisal M. Alkahtani and Jalal T. Althakafy and Muteb H. Alshamari and Sameh A. Rizk and Asmaa Mahmoud Fahim and Mohamed Abdel‐Megid and Atef Samir Darwish and Saleh A. Ahmed},
journal = {Polymer Testing},
year = {2026},
month = jun,
doi = {10.1016/j.polymertesting.2026.109246},
url = {https://doi.org/10.1016/j.polymertesting.2026.109246},
note = {CC BY},
}
RIS
TY - JOUR
TI - Microwave/ultrasound-assisted synthesis of an Fe(III)-coordinated oxazolone–polyamide metallopolymer for coordination-driven Cu(II) removal from water
AU - Faisal A. Almalki
AU - Faisal M. Alkahtani
AU - Jalal T. Althakafy
AU - Muteb H. Alshamari
AU - Sameh A. Rizk
AU - Asmaa Mahmoud Fahim
AU - Mohamed Abdel‐Megid
AU - Atef Samir Darwish
AU - Saleh A. Ahmed
PY - 2026
DA - 2026/06/06
JO - Polymer Testing
DO - 10.1016/j.polymertesting.2026.109246
UR - https://doi.org/10.1016/j.polymertesting.2026.109246
AB - This study investigated the microwave/ultrasound-assisted synthesis of a new O/N-rich oxazolone–polyamide framework and its Fe(III)-coordinated metallopolymer for Cu(II) removal from aqueous solution. The oxazolone precursor was prepared using microwave irradiation at 300 W for 10-15 min, followed by ultrasound activation at 40 kHz for 20 min, giving a yield of approximately 70%, while the reduced diamine monomer was obtained in 66% yield. The resulting NH-OXAZAM-CO polymer was further coordinated with Fe(III) to produce Fe-(NH-OXAZAM-CO), containing abundant amide, oxazolone, carbonyl, and nitrogen donor sites. The prepared materials were characterized using Fourier transform infrared spectroscopy, scanning electron microscopy with energy-dispersive X-ray analysis, X-ray diffraction, thermogravimetric analysis, X-ray photoelectron spectroscopy, and density functional theory calculations. Cu(II) adsorption was evaluated using synthetic CuSO 4 solutions under controlled conditions: adsorbent dose 1.0 g L −1 , particle size 125–250 μm, initial Cu(II) concentration 10–50 mg L −1 , pH 5.5 ± 0.1, ionic strength 0.01 M NaNO 3 , and temperature 25 ± 1 °C. The Langmuir model provided the best fit, with a maximum adsorption capacity of 54.9 mg/g, a Langmuir constant of 0.1689, a separation factor of 0.10, and a correlation coefficient of R 2 = 0.9999, confirming favorable monolayer adsorption on finite active sites. The Temkin model also showed acceptable fitting (R 2 = 0.9701), indicating adsorbent–adsorbate interactions, whereas the Dubinin–Radushkevich model gave an adsorption energy of 1.16 kJ mol −1 , suggesting that weak physical interactions contribute to the initial uptake stage. Spectroscopic evidence from infrared and X-ray photoelectron analyses confirmed Cu(II) binding through oxygen and nitrogen donor sites, while computational descriptors supported the role of electron-rich coordination centers in metal-ion capture. Overall, the study demonstrates that Fe(III)-modified oxazolone–polyamide metallopolymers are promising coordination-based adsorbents for Cu(II)-contaminated water treatment.
SN - 0142-9418
SN - 1873-2348
ER -