Design and assembly of novel, sustainable, ecofriendly and low-cost nanobiosorbents by facile and green approaches are generally aimed to apply in remediation of toxic and nonbiodegradable pollutants from aquatic systems. Hence, the current study is directed to synthesize a novel nanobiosorbent by a facile solid–solid and microwave-assisted approach for direct impregnation of derived nanobiochar from pomegranate peels waste feedstock (PPNC) onto magnesium (II) aluminum (III)-layered double hydroxide (MgAl-LDH) for the generation of MgAl-LDHs@PPNC. This was initially characterized by several techniques to confirm the morphological and structural features. The particle size range was identified (13.47–41.78 nm) and the concluded elemental compositions were Al (9.49 %), Mg (19.33 %), C (25.4 %), and O (45.78 %) according to the energy-dispersive X-ray (EDX) analysis. The Fourier Transform-infrared (FT-IR) study denoted to several incorporated surface functionalities as –COOH, –OH, metal–O and others functionalities. MgAl-LDHs@PPNC exhibited a good surface area 275.57 m2g−1, while the zero-charge point was also detected at 6.0. Some experimental impacting conditions were testified and optimized by the batch removal system of methylene blue dye pollutant (MBDP) by MgAl-LDHs@PPNC. The concluded optimum conditions were figured out at pH 7.0, 15 min reaction duration, 25 mg nanobiosorbent dosage and 25 °C reaction temperature. Related expressions to isotherm and kinetic investigations were testified to confirm the most correlated experimental data to both Freundlich and pseudo-2nd-order expressions. Thermodynamic parameters were additionally computed to refer to the exothermal spontaneity trends in adsorptive reaction of MBDP onto MgAl-LDHs@PPNC. The evaluated nanobiosorbent is therefore, labeled with high stability to providing highly acceptable efficiency at 82.7–99.2 % (5 mgL−1) by the first-fifth regeneration processes. MgAl-LDHs@PPNC was finally afforded excellent removal uptake of MBDP (5 mgL−1) from real contaminated waters giving 93.17–98.27 %.
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