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The new material polypyrrole/MoS₄²⁻(MoS₄‐Ppy), prepared by ion‐exchange of NO₃‐ of NO₃‐Ppy with MoS₄²⁻, displays high acid stability and excellent uptake for heavy metal ions such as Hg²⁺, Ag⁺, Cu²⁺, and Pb²⁺. The different maximum adsorption capacities (q_m) for Cu²⁺, Pb²⁺, Hg²⁺, and Ag⁺depend on the various binding modes arising from the different thiophilicity of these metal ions. The removals of Ag⁺and Pb²⁺reach >99.6% within 5 min, and for highly toxic Hg²⁺, >98% removal achieves at 1 min. At strong acid limit, the exceptionalq_m(Ag⁺) of 725 mg g⁻¹places the MoS₄‐Ppy at the top of materials for such removal. Uptake kinetics of Ag⁺, Hg²⁺, and Pb²⁺is extremely fast: >99.9% removal rates at wide pH range (0.5–6) within 1–5 min. Also, at strongly acidic conditions (pH ≈ 1), for highly toxic Hg²⁺, <2 ppb concentration can be achieved, accepted as safe limit. The MoS₄‐Ppy demonstrates an outstanding ability to separate low‐concentrated Ag⁺from high concentrated Cu²⁺especially under strong acidic conditions (pH ≈ 1), showing a large separation factor SF_Ag/Cu(K_d^Ag/K_d^Cu) of 10⁵(>100). MoS₄‐Ppy is a superior and novel sorbent material for water remediation applications as well as precious metals recovery.