In this work, new thermosensitive copolymers bearing phosphonated groups were synthesized and used to remove metal pollution. Sorption properties are brought by hydrolyzed (dimethoxyphosphoryl)methyl 2-methylacrylate (hMAPC1) monomer. N-n-propylacrylamide (NnPAAm) led to the thermoresponsive properties of the copolymers. Low lower critical solution temperature (LCST) values were observed, ranging between 20 and 25 °C depending on the molar ratio of each monomer in the copolymer. Sorption properties of these copolymers towards nickel ions were evaluated for increasing temperatures (10–40 °C), Ni ion concentrations of 20 mg L−1 and pH values between 3 and 7. Best results were observed for temperatures just lower than the LCST (20 °C), when the copolymer was fully soluble in water solution. For temperature higher than the LCST, phosphonic diacid groups accessibility was considerably reduced by the precipitation of the thermosensitive part of the copolymer leading to lower sorption properties. In these conditions, the highest Ni removal by the copolymer was observed for pH = 7, when there was almost no competition between the sorption of H+ and Ni2+ ions on the phosphonic acid groups. These optimal conditions enabled removal of about 70% of the nickel in the synthetic effluent.

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