Methylene blue dye in water sources can pose health risks to humans, potentially causing methemoglobinemia, a condition that impairs the blood’s ability to carry oxygen. Hence, the current study investigates the synthesis of novel magnesium borate/magnesium oxide (Mg3B2O6/MgO) nanostructures and their efficiency in removing methylene blue dye from aqueous media. The nanostructures were synthesized using the Pechini sol–gel method, which involves a reaction between magnesium nitrate hexahydrate and boric acid, with citric acid acting as a chelating agent and ethylene glycol as a crosslinker. This method helps in achieving a homogeneous mixture, which, upon calcination at 600 and 800 °C, yields Mg3B2O6/MgO novel nanostructures referred to as MB600 and MB800, respectively. The characterization of these nanostructures involved techniques like X-ray diffraction (XRD), Fourier-transform infrared (FTIR) spectroscopy, N2 gas analyzer, and field-emission scanning electron microscope (FE-SEM). These analyses confirmed the formation of orthorhombic Mg3B2O6 and cubic MgO phases with distinct features, influenced by the calcination temperature. The mean crystal size of the MB600 and MB800 samples was 64.57 and 79.20 nm, respectively. In addition, the BET surface area of the MB600 and MB800 samples was 74.63 and 64.82 m2/g, respectively. The results indicated that the MB600 sample, with its higher surface area, generally demonstrated better methylene blue dye removal performance (505.05 mg/g) than the MB800 sample (483.09 mg/g). The adsorption process followed the pseudo-second-order model, indicating dependency on available adsorption sites. Also, the adsorption process matched well with the Langmuir isotherm, confirming a homogeneous adsorbent surface. The thermodynamic parameters revealed that the adsorption process was physical, exothermic, and spontaneous. The MB600 and MB800 nanostructures could be effectively regenerated using 6 M HCl and reused across multiple cycles. These findings underscore the potential of these nanostructures as cost-effective and sustainable adsorbents for methylene blue dye removal.
