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Zeolite-carbon composites (Na-P1(C), Na-X(C)) and pure zeolites (Na-P1, Na-X) were synthesized from hazardous high-carbon fly ash waste (HC FA) via hydrothermal reaction with sodium hydroxide (NaOH). These solids were applied in the removal of diclofenac (DCF) from aqueous solution, with and without poly(acrylic acid) (PAA). The experiments included adsorption–desorption measurements, as well as electrokinetic and stability analyses. The obtained results showed that HC FA and Na-P1(C) had the greatest adsorption capacity towards DCF, i.e., 26.51 and 21.19 mg/g, respectively. PAA caused considerable decrease in the DCF adsorption due to the competition of both adsorbates of anionic character for active sites. For example, the adsorbed amount of DCF on Na-P1 without PAA was 14.11 mg/g, whereas the one measured with PAA was 5.08 mg/g. Most of prepared solids were effectively regenerated by the use of NaOH. Desorption degree reached even 73.65% in the single systems (with one adsorbate) and 97.24% in the mixed ones (with two adsorbates). Zeolitic materials formed suspensions of rather low stability, which underwent further deterioration in the organic molecules presence. All the results obtained in this study indicated that HC FA can be successfully managed in the removal of organic substances.
