Commercial bleach (3.6 wt% active chlorine) is prepared by diluting highly concentrated industrial solutions of sodium hypochlorite (about 13 wt% active chlorine) obtained mainly by bubbling chlorine gas into dilute caustic soda. The chlorine and soda used are often obtained by electrolyzing a sodium chloride solution in two-compartment cells (chlorine-soda processes). On a smaller scale, small units used for swimming pool water treatment, for example, allow the production of low-concentration bleach (0.3 to 1 wt% active chlorine) by use of a direct electrolysis of sodium chloride brine. The oxidation and degradation reaction of hypochlorite ion (ClO−) at the anode is the major limiting element of this two-compartment process. In this study, we have developed a new process to obtain higher levels of active chlorine up to 3.6%, or 12° chlorometric degree. For this purpose, we tested a device consisting of a zero-gap electrolysis cell, with three compartments separated by a pair of membranes that can be porous or ion-exchange. The idea is to generate in the anode compartment hypochlorous acid (HClO) at high levels by continuously adjusting its pH to a value between 4.5 and 5.5. In the cathodic compartment, caustic soda is obtained, while the central compartment is supplied with brine. The hypochlorous acid solution is then neutralized with a concentrated solution of NaOH to obtain bleach. In this work, we studied several membrane couples that allowed us to optimize the operating conditions and to obtain bleach with contents close to 1.8 wt% of active chlorine. The results obtained according to the properties of the membranes, their durability, and the imposed electrochemical conditions were discussed.