The new one-pot hydrolysis-crosslinking reaction was used to synthesize a new, waste poly(methyl methacrylate) (PMMA)-based material for zinc(II) ions removal. The alkaline hydrolysis of PMMA in diethylene glycol diethyl ether was used to obtain polymer matrix and it was then crosslinked with Ca and Mg ions to obtain the sorbent. As a result, the macroporous materials were obtained with a yield of 87% when waste PMMA was used, and about 95% when the commercial PMMAs were used. The degree of hydrolysis was similar, from 32% to 35%. New materials were then tested for their affinity towards zinc(II) ions. Two kinetic models (pseudo-first and pseudo-second order), as well as two isotherms (Langmuir and Freundlich), were used to describe the kinetics and equilibrium of zinc(II) ion sorption on the studied materials, respectively. All the prepared PMMA-based sorbents showed similar or higher sorption capacity (q up to 87.7 mg/g) compared to commercially available materials in a broad pH range (4–7). The study shows sorption was fast—above 80% of equilibrium capacity was achieved after ca. 0.5 h. Presented results show that waste PMMA may be an interesting raw material for the preparation of sorbents for zinc(II) ions removal.
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