Studies of the sorption process of extracting Fe3+ and Al3+ ions from aqueous solutions of sodium chloride, nitrate and sulfate salts in a static mode on an industrial powder sorbent of the OU-A brand have been carried out. The influence of Cl-, NO3- and SO42- anions on the value of sorption of metal cations was determined. By the nature of the adsorption isotherms of metal ions, an assumption about the mechanisms of the process was made. The values of the electrokinetic potential of coal particles in salt solutions were obtained, on the basis of which flocculants were selected and their effect on the efficiency of the electroflotation process for extracting spent carbon sorbent was evaluated. It was found that the spent sorbent with Fe3+ ions in an amount of up to 1 g/l, and the sorbent with Al3+ ions – up to 1.6 g/l within 10 minutes can be extracted from solutions of nitrate and sodium chloride salts by adding flocculants of cationic and nonionic types. The experimental studies have shown that the use of a combined method, including sorption treatment with subsequent extraction of the spent sorbent in the process of electroflotation, will not only reduce the duration of wastewater treatment, but also provide a high degree of their purification.