Selective recovery of gold from cyanide leach liquors is hindered by the co-dissolution of iron minerals that generate ferrocyanide complexes which strongly compete with [Au(CN)
2]
− at ion-exchange sorbents. Here, we investigate mixed-bed interpolymer systems (IPS) composed of a strong-acid sulfonated
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Selective recovery of gold from cyanide leach liquors is hindered by the co-dissolution of iron minerals that generate ferrocyanide complexes which strongly compete with [Au(CN)
2]
− at ion-exchange sorbents. Here, we investigate mixed-bed interpolymer systems (IPS) composed of a strong-acid sulfonated polystyrene–divinylbenzene cation exchanger (TC007, Na
+ form) and a strong-base quaternary ammonium anion exchanger (AV-17-8, Cl
− form) as a charge-selective platform for gold cyanide recovery. IPS compositions spanning cation-to-anion molar ratios from 6:0 to 0:6 were evaluated in batch contact with binary model solutions containing 30 mg L
−1 each of [Au(CN)
2]
− and [Fe(CN)
6]
4− at pH 10 and 25 °C. The optimal 1:5 IPS achieved an [Au(CN)
2]
− extraction degree of 79.88% and a selectivity coefficient β = D
Au/D
Fe = 4.95 at 48 h, whereas the pure AV-17-8 anion exchanger (0:6) reached only 37.55% Au extraction at 48 h, following an atypical delayed-uptake kinetic profile rather than the rapid, near-quantitative capture expected of an unmodified strong-base resin. Sorption kinetics were best described by a pseudo-second-order model (R
2 = 0.9992), confirming ion exchange at quaternary ammonium sites as the dominant rate-controlling step, with a ~30-fold increase in k
2 for [Au(CN)
2]
− in the 1:5 IPS relative to AV-17-8 alone. FTIR spectroscopy and TGA-DSC revealed the incorporation of metal cyanide complexes into the IPS matrix, with diagnostic C≡N stretching bands at 2108.7 and 2034.1 cm
−1 and an additional thermal event at 200–280 °C. These findings establish compositionally tunable IPS based on commercially available resins as a charge-selective sorbent platform demonstrating a capacity to regenerate under single-cycle elution conditions for gold cyanide recovery from ferrocyanide-containing process streams while highlighting the need for further evaluation under industrial Fe:Au ratios.
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