The increasing concern of dye contamination in wastewater results in the toxicity of aquatic life and water quality, so wastewater treatment is required to treat the low water quality standard for safety purposes. Lemon peel beads-doped iron(III) oxide-hydroxide (LBF) and lemon peel beads-doped zinc oxide (LBZ) were synthesized and characterized to investigate their crystalline structure, surface morphology, chemical compositions, chemical functional groups, and ζ potentials by X-ray diffraction, field emission scanning electron microscopy and focused ion beam, energy dispersive X-ray spectroscopy, Fourier transform infrared, and zetasizer techniques. Their effects of dose, contact time, temperature, pH, and concentration for reactive blue 4 (RB4) dye removal efficiencies were investigated by batch experiments, and their adsorption isotherms, kinetics, and desorption experiments were also studied. LBF and LBZ demonstrated semicrystalline structures, and their surface morphologies had a spherical shape with coarse surfaces. Five main elements of carbon (C), oxygen (O), calcium (Ca), chlorine (Cl), and sodium (Na) and six main function groups of O–H, CN, CC, C–OH, C–O–C, and C–H were detected in both materials. The results of ζ potential demonstrated that both LBF and LBZ had negative charges on the surface at all pH values, and their surfaces increased more of the negative charge with the addition of the pH value from 2–12. For batch tests, the RB4 dye removal efficiencies of LBF and LBZ were 83.55 and 66.64%, respectively, so LBF demonstrated a higher RB4 dye removal efficiency than LBZ. As a result, the addition of iron(III) oxide-hydroxide helped in improving the material efficiency more than zinc oxide. In addition, both LBF and LBZ could be reused in more than five cycles for RB4 dye removal of more than 41%. The Freundlich model was a good explanation for their adsorption patterns relating to physiochemical adsorption, and a pseudo-second-order kinetic model was a well-fitted model for explaining their adsorption mechanism correlating to the chemisorption process with heterogeneous adsorption. Therefore, LBF was a potential adsorbent to further apply for RB4 dye removal in industrial applications.
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