Method and mechanism for the formation of sulfur compounds during the process of sulfur electrochemical dissolution has been studied, including a technique for the production of composite sulfur-graphite electrode. Along with these, a 3D design is presented in the unit that was used to perform electrolytic reduction, using composite sulfur-graphite electrode. For the first time, a study was carried out for the simultaneous reactions of electroreduction and electrooxidation of sulfur at the sulfur-graphite electrode in sulfurous environment in the same electrolytic bath, with separate electrode spaces. Influences of current density, acid concentration and electrolyte temperature were studied, and it was demonstrated that sulfur is reduced in cathode chamber with formation of hydrogen sulfide gas, and is oxidized in the anode chamber with formation of sulfite and sulfate ions. It has been shown that the methods we propose can be used to produce important sulfur compounds through electrochemical dissolution of specially designed sulfur-graphite electrode.