<p>This study investigated combining fine clinoptilolite with iron hydroxide coagulant, as a cost-effective, dual-purpose flocculant for enhanced removal of Pb²⁺ or Cu²⁺ ions, along with the solid–liquid separation and physicochemical analysis. For the clinoptilolite, adsorption kinetics fitted a pseudo-second-order (PSO) rate model with higher rate constants for Pb²⁺, while equilibrium adsorption data fitted the Langmuir monolayer model, with <i>Q</i>_<i>max</i> similar at 18.8&#xa0;mg/g for Pb²⁺ and 18.3&#xa0;mg/g Cu²⁺. TEM elemental mapping of the clinoptilolite evidenced areas of K and Fe impurities, while SEM suggested a uniform distribution of aggregates comprising a clinoptilolite core with decorated FeOOH. X-ray diffraction (XRD) indicated the FeOOH phase as α-FeOOH (Goethite) with no change in structure on inclusion of adsorbed Pb²⁺. Combined clinoptilolite-FeOOH flocs were significantly larger than FeOOH only precipitates, while flocs formed from 0.5&#xa0;wt% FeOOH and 1 wt% clinoptilolite produced the fastest settling rates and greatest consolidation. Compressive yield stress data also correlated with enhanced dewatering of the combined systems, due to the dense clinoptilolite acting as a weighter material. For final metals removal, combined flocs outperformed FeOOH across a broad concentration range, achieving &gt; 98% removal for both Pb²⁺ or Cu²⁺. The greater metals removal combined with denser floc production and improved settling features highlights significantly enhanced performance above that possible from either ion exchange or precipitation alone.</p> Graphical abstract <p></p>