AbstractHerein, two sulfhydryl‐functionalized polymers, namely, EDT‐HCPS and TMPMP‐HCPS, were synthesized according to the Friedel‐Craft s alkylation and nucleophilic substitution, and they were used to adsorb Pd2+ and Ag+ from aqueous solution. The Friedel‐Crafts alkylation offered the polymers with hyper‐cross‐linking frameworks composed of plentiful rigid methylene. The nucleophilic substitution brought abundant functional SH groups (the sulfur contents were 12.6 and 9.4 wt%, respectively) to the polymers. The adsorption results showed that the capacities of Pd2+ and Ag+ on EDT‐HCPS were larger than TMPMP‐HCPS, and the higher quantities of functional SH groups and the porosity played a beneficial role. The equilibrium data can be characterized by the Langmuir model, and the maximum capacities of Pd2+ and Ag+ on EDT‐HCPS at 308 K were predicted to be 383.92 and 212.93 mg g−1, respectively. The produced polymers represented superior adsorption selectivity, reproducibility, and reusability, demonstrating their excellent performance for the adsorption of Pd2+ and Ag+, and analysis of the adsorption mechanism demonstrated that the SH groups played a major role due to the strong chemical complexation of the functional SH with Pd2+/Ag+.
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