Simultaneous recovery and value-added conversion of hazardous heavy metal ions from complex wastewater sources is of great significance yet challenging. Herein, we demonstrate that highly toxic antimonite Sb(III) could be effectively recovered from antimony (Sb) mine flotation wastewater and converted into high-value-added metallic Sb using a novel facile atomic H* enhanced electrochemical reduction avenue coupled with thermal reduction by H₂ gas. The high production of atomic H* generated from the electrochemical cathode with an optimum reduction potential of –1.2 V vs. Ag/AgCl, which is lower than the Sb(III) reduction potential of –1.0 V, might be attributable to the superior Sb recovery capabilities. Furthermore, the metallic Sb concentration at –1.2 V was 14.43 times greater than at –1.0 V due to the strong reductivity of atomic H*. In addition, Sb(III) removal efficiency was found to be as high as 98.52%, with a metallic Sb recovery rate of up to 1.67 mg min^–1. The efficiency of Sb(III) recovery was demonstrated throughout a wide pH range, with metallic Sb being the main product, independent of the presence of multiple coexisting ions. Economic analysis also indicated that treating Sb mine flotation wastewater per ton may yield a net profit of $40.09. This research contributes to the advancement of an atomic H* enhanced electrochemical technology for high-valued heavy metal recovery from complex heavy metal-polluted wastewater.

从复杂的废水源中同时回收和增值有害重金属离子具有重要意义但也具有挑战性。在此，我们证明了使用新型简便的原子 H* 增强电化学还原途径与热还原相结合，可以有效地从锑 (Sb) 矿浮选废水中回收剧毒的锑矿 Sb(III) 并将其转化为高附加值的金属 Sb。 H ₂气。电化学阴极产生大量原子 H*，最佳还原电位为 –1.2 V vs. Ag/AgCl 低于 –1.0 V 的 Sb(III) 还原电位，这可能归因于 Sb 的出色回收能力。此外，由于原子 H* 的强还原性，–1.2 V 下的金属 Sb 浓度是–1.0 V 下的 14.43 倍。此外，发现 Sb(III) 去除效率高达 98.52%，金属 Sb 回收率高达 1.67 mg min ^–1. 在很宽的 pH 范围内证明了 Sb(III) 的回收效率，金属 Sb 是主要产物，与多种共存离子的存在无关。经济分析还表明，每吨处理 Sb 矿浮选废水可产生 40.09 美元的净利润。这项研究有助于推进原子 H* 增强的电化学技术，用于从复杂的重金属污染废水中回收高价值的重金属。