Scalable S/N Co-Functionalized Activated Carbon for Targeted Recovery of Multiple Precious Metals from Industrial Waste Streams

• Engineered S/N network with in situ hierarchical porosity. • Selective recovery of Au, Pd, and Pt from sub-ppb to industrial waste leachates. • Synergistic multi-functionality of imine/polysulfide/amine/thioamide groups. • One-pot, kilogram-scale synthesis with low cost and reduced life-cycle impacts. The recovery of precious metals (PMs) from industrial waste streams is constrained by the scarcity of adsorbents that reconcile scalable production, multi-metal selectivity, and cost-effectiveness. Here, we engineered S/N co-functionalized activated carbon to overcome these challenges by combining hierarchical porosity with an electron-enhanced surface of a multifunctional S/N network. The optimal S/N co-functionalized activated carbon (AC2) is synthesized via a scalable one-pot solvothermal method (92% yield, 0.532 kg·batch −1 ), immobilizing thioamide, polysulfide, imine, and amine functionalities onto a micro-mesoporous carbon matrix. This design enables ultra-trace PM uptake (1 μg·L −1 ) with exceptional residual levels (<0.001 μg·L −1 ) and remarkable adsorption capacities (1750, 940, and 270 mg·g −1 for Au, Pd, and Pt, respectively). Practical validation in e-waste and catalyst leachates (>96% recovery) and spiked surface water (92%–97% PM uptake with 10000 fold competing metal concentrations) demonstrates robust performance in real-world hydrometallurgical and ecological contexts. The adsorbent’s techno–economic viability is further underscored by acid-resistant reusability (>15 cycles), a 34 fold cost reduction at scale (370 CNY·kg −1 ), and over 90% lower life cycle environmental impacts. This work establishes a paradigm for resource-efficient urban mining, integrating scalable material design with critical metal recovery to address global resource circularity challenges.