catalysts Article Fenton Degradation of Ofloxacin Using a Montmorillonite–Fe 3 O 4 Composite Alamri Rahmah Dhahawi Ahmad, Saifullahi Shehu Imam, Wen Da Oh and Rohana Adnan *   Citation: Ahmad, A.R.D.; Imam, S.S.; Oh, W.D.; Adnan, R. Fenton Degradation of Ofloxacin Using a Montmorillonite–Fe 3 O 4 Composite. Catalysts 2021, 11, 177. https:// doi.org/10.3390/catal11020177 Academic Editor: Vincenzo Vaiano Received: 13 December 2020 Accepted: 25 January 2021 Published: 28 January 2021 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). School of Chemical Sciences, Universiti Sains Malaysia, Penang 11800, Malaysia; rahalamri@student.usm.my (A.R.D.A.); ssimam.chm@buk.edu.ng (S.S.I.); ohwenda@usm.my (W.D.O.) * Correspondence: r_adnan@usm.my Abstract: In this work, FeM composites consisting of montmorillonite and variable amounts of Fe 3 O 4 were successfully synthesized via a facile co-precipitation process. They were characterized using X- ray photoelectron spectroscopy (XPS), a field emission scanning electron microscope (FESEM), energy- dispersive X-ray spectroscopy (EDX), a transmission electron microscope (TEM), N 2 adsorption– desorption, and Fourier transform infrared spectroscopy (FTIR) techniques to explain the effect of Fe 3 O 4 content on the physicochemical properties of the Fe 3 O 4 –montmorillonite (FeM) composites. The FeM composites were subsequently used as heterogeneous Fenton catalysts to activate green oxidant (H 2 O 2 ) for the subsequent degradation of ofloxacin (OFL) antibiotic. The efficiency of the FeM composites was studied by varying various parameters of Fe 3 O 4 loading on montmorillonite, catalyst dosage, initial solution pH, initial OFL concentration, different oxidants, H 2 O 2 dosage, reaction temperature, inorganic salts, and solar irradiation. Under the conditions of 0.75 g/L FeM-10, 5 mL/L H 2 O 2 , and natural pH, almost 81% of 50 mg/L of OFL was degraded within 120 min in the dark, while total organic carbon (TOC) reduction was about 56%. Although FeM composites could be a promising heterogeneous catalyst for the activation of H 2 O 2 to degrade organic pollutants, including OFL antibiotic, the FeM-10 composite shows a significant drop in efficiency after five cycles, which indicates that more studies to improve this weakness should be conducted. Keywords: Fenton degradation; ofloxacin; Fe 3 O 4 ; montmorillonite; wastewater 1. Introduction For the past few years, the high consumption of antibiotics has resulted in their continuous detection in surface, ground, drinking, and wastewater around the world [1]. Their presence is a threat to the ecological environment due to their chemical stability and slow biodegradation since antibiotics are harmful to microorganisms [2,3]. Among the antibiotics, ofloxacin (OFL) is an extensively used 2nd-generation fluoroquinolone due to its good antibacterial activity [4,5]. It is commonly used to treat bronchitis, infectious diarrhea, pneumonia, pelvic inflammatory disease, eye infections, ear infections, gonorrhea, respiratory tract infections, urinary tract infections, gastrointestinal infections, and skin infections [68]. However, approximately 90% is excreted via urination in its original form 48 h after administration [7]. The presence of OFL in water results in unpleasant odors and may also present a significant risk to aquatic species due to its toxicity [9,10]. Unfortunately, OFL is still being detected in wastewater even after conventional treatment [11]. Thus, the development of an effective method for the removal of OFL from wastewater becomes imperative. The Fenton reaction is an effective process that has gained widespread acceptance due to its efficiency in degrading and even mineralizing persistent organic contaminants with the highly reactive hydroxyl radicals ( OH) generated from H 2 O 2 using Fe 2+ from a Fenton reagent [12]. However, to overcome the shortcomings of the homogeneous Fenton process, various heterogeneous Fenton catalysts, including Fe 3 O 4 nanoparticles [13], Fe-Mn Catalysts 2021, 11, 177. https://doi.org/10.3390/catal11020177 https://www.mdpi.com/journal/catalysts