The adsorption efficiency of treatment of wastewater from a chemical enterprise containing high concentrations of heavy metals Fe3+, Mn2+, Ti3+, Cr3+, Zn, Ni (9300–7.3 mg/l) in combination with acid (up to 180,000 mg/l), as well as additional treatment of wastewater from a machine-building enterprise containing Cd, Cu, Cr, Zn was studied. Inorganic (based on natural materials) and carbon sorbents were used as sorbents, including those obtained by the original technology of coal activation (high-efficiency low-temperature dispersion—Nanocoal (NC)) and carbon nanotubes (CNT) (method of catalytic thermolysis of hydrocarbon fractions). It is shown that the most effective sorbents for concentrated effluents are dolomite < serpentinite < composite sorbent diatomite-serpentinite < trepel < diatomite < shungite. For model solutions with medium concentration (892–0.5 mg/L): NC < diatomite < BAU < zeolite < opoca (dilution by a factor of 10); model solutions diluted 50 times (heavy metal concentrations 358–3 mg/L): zeolite < diatomite < opoca < NC < BAC (50 times); for the most dilute solutions (5–0.2 mg/L)—Nanocoal and birch activated carbon (traditional technology) adsorption increases in the series CNT < NC < BAC.