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[Display omitted] • PVA/PSSNa semi-IPN@Ni foam removes 95.17% CIP and 99.20% Ni(II) from wastewater. • Satisfactory adsorption occurs under neutral to slightly acidic pH (3–7). • In the binary system, Ni(II) greatly affects CIP adsorption, while CIP slightly affects Ni(II). • The interactive term of Ni(II) concentration and pH notably affects the CIP removal. • Removal of CIP and Ni(II) is most affected by their own concentration and pH. The coexistence of antibiotics and heavy metals in wastewater notably influences their adsorption removal behavior. However, the synergistic and antagonistic characteristics and mechanisms of their co-adsorption remain unclear. A novel adsorbent, PVA/PSSNa semi-IPN@Ni foam, was synthesized and applied to study its features and mechanisms in the single and binary systems of ciprofloxacin (CIP) and Ni(II). Exceptional removal efficiencies of 95.17 % for CIP and 99.20 % for Ni(II) were achieved. The interactive effects between CIP and Ni(II) were comprehensively explored through adsorption capacity ratio (Rq) and response surface methodology. Mechanistic insights were obtained through NaCl charge shielding experiments, substructure analog molecule probes experiments, theory calculations, as well as FTIR and XPS characterizations. The outcomes suggest that in the single system of CIP, the adsorption mechanisms include electrostatic attraction, hydrogen bonding, and π-π interactions. In the single system of Ni(II), mechanisms include electrostatic attraction and coordination. In the binary system of CIP + Ni(II), low Ni(II) concentrations facilitate CIP adsorption through coordination and bridging, whereas high Ni(II) concentrations let to competition for adsorption sites. Interestingly, the presence of CIP had minimal impact on Ni(II), exhibiting only a slight synergistic effect. These findings highlight the PVA/PSSNa semi-IPN@Ni foam as a hopeful candidate for removing CIP and Ni(II) from wastewater, and contribute to a deeper comprehension of synergistic and antagonistic mechanisms in the binary system involving CIP and Ni(II). [ABSTRACT FROM AUTHOR]