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New techniques were developed for the synthesis of monolithic highly porous composite aerogels (hydrogels) from reduced graphene oxide and carbon nanotubes, as well as graphene-containing composites based on mesoporous activated carbon. Simple operations for hydrophilization of synthesized samples were proposed. New electrode materials for electrosorption and deionization of water were fabricated. The resulting materials were investigated and tested in electrochemical cells for membrane capacitive deionization (MCDI).