Biochar materials are good examples of sustainable adsorbents with appreciable recent interests and applications in water treatment. The disadvantage of using unmodified pristine biochars in water treatment is mainly related to the inhomogeneous distribution of various surface functional groups. Therefore, the current study is designed to functionalize and homogenize the surface of a selected nanobiochar with a cation exchanger using hydrothermal and solvothermal microwave irradiation. The adsorption behavior of immobilized Amberlite cation exchanger onto Cynara scolymus nanobiochar (ACE@CSNB) was compared versus the pristine Cynara scolymus nanobiochar (CSNB). ACE@CSNB was categorized as a typical mesoporous material (mean pore size = 2.238 nm) and the FT-IR spectra confirmed surface modification via two characteristic peaks at 1140–1250 cm−1 and 1030–1070 cm−1 for R-SO3− with S = O. The TPD–MS analysis of CSNB and ACE@CSNB referred to the presence of carboxyl, lactonic, and acid anhydride groups as well as phenolic moieties. The adsorption behavior of methylene blue dye and lead ions by ACE@CSNB was found much higher than those concluded by CSNB providing maximum adsorptive capacity values owing to the played clear role by Amberlite cation exchanger. Moreover, ACE@CSNB was efficiently regenerated and confirmed MB and Pb(II) removal with 92.26% and 1000 µmol g−1, respectively Finally, the removal efficiency values from three water matrices by ACE@CSNB biochar were characterized as 91.74–98.19% and 96.27–99.14% for Pb(II) and MB, respectively to refer to the validity and applicability of the investigated ACE@CSNB biochar for treatment of these two pollutants from real water samples with excellent efficiency.
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