Solid-phase extraction process using chelating sorbent is a novel technique due to its high separation efficiency and simplicity. A designed three-dimensional cross-linked hydrophilic chelating polymeric sorbent, polyacrylhydroxamic acid, was developed for enhanced uptake of uranium from waste solution (pH 6–9) by complexation between the sorbent’s active functional group and uranium. The sorbent was synthesized by polymerization of acrylamide with cross-linking agent, followed by conversion and functionalization with hydroxylamine hydrochloride. In this paper, removal and recovery of uranium from effluent of uranium material processing plant in the presence of competitive ions such as sodium, calcium and magnesium were studied using the sorbent. Uranium uptake property of the developed sorbent was also investigated with respect to sorbent’s physical characteristics such as bead size distribution and bead swelling, in batch experiments. Distribution coefficient of uranium in the sorbent was substantially high (1,250 mL of effluent/g of sorbent), and immobilization factor was 0.028. The results showed that more than 90 % recovery of uranium is viable from nuclear effluent without preconditioning. Breakthrough profiles of column operation were successfully described for effective removal of uranium in continuous mode. The novel sorbent has been used for polishing the nuclear wastewater and hence to mitigate the environmental issues.