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A closed-cycle technology regarding the use of an exhausted Pd-based adsorbent as a photocatalyst in the degradation process of phenol is presented. Pd (II) represents a precious metal of great economic importance. Its obtained from natural sources become more difficult to achieve. Therefore, also considering the regulations of the “circular economy,” its recovery from secondary sources turn out to be a stringent issue in the last years. Pd(II) ions are removed from aqueous solution through adsorption onto Florisil (an inorganic solid support—magnesium silicate) impregnated with Cyphos IL 101 (trihexyl tetradecyl phosphonium chloride). It was observed that the presence of the ionic liquid (IL) in the adsorbent structure doubles the adsorption efficiency of the studied materials. The newly obtained Pd-based photocatalyst was exhaustively characterized and was used in the degradation process of phenol from aqueous solutions. The phenol degradation process was studied in terms of the nature of the photocatalyst used, time of photodegradation and solid: liquid ratio. It was observed that both the presence of IL and Pd lead to an increase in the efficiency of the phenol degradation process. The new Pd-based photocatalyst could be efficiently used in more cycles of phenol photodegradation processes. When is used as a photocatalyst the Florisil impregnated with IL and loaded with 2 mg/g of Pd, a degree of mineralization of 93.75% is obtained after 180 min of irradiation of a phenol solution having a concentration of 20 mg/L and using a solid:liquid ratio = 1:1.

Photodegradation of Phenolic Compounds from Water in the Presence of a Pd-Containing Exhausted Adsorbent