Boronic acid copolymers with a large number of functional groups were obtained via a free radical polymerization method. The corresponding composite membranes for alkaline diffusion dialysis (DD) were prepared by a crosslinking reaction between polyvinyl alcohol (PVA) and the as-obtained boronic acid copolymers. The composite membranes possessed water uptake (WR) of 122.1–194.4%, ion exchange capacities (IECs) of 0.79–1.17 mmol/g, as well as both good mechanical stability (tensile strength of 40.7–49.9 MPa and elongation at break of 52.1–121.1%) and thermal stability. The as-prepared membranes were stable in 2 M NaOH solution at 65 °C with a swelling degree and mass loss of as-prepared membranes in the range of 305–368% and 9.2–22%, respectively. A NaOH/Na2WO4 mixture was used to investigate the separation properties of as-prepared membranes via the DD process. Results indicated that the dialysis coefficients of OH− (UOH) were in the range of 0.0079–0.0150 m/h, while the separation factors (S) were in the range of 26.6–53.2. The functional groups from boronic acid copolymer and –OH from PVA were demonstrated to promote the ion transport synergistically.
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