Abstract: | The electrochemical preparation of NaClO has been widely used for the production of industrial disinfectant. To reduce the cost of electrode preparation using the brushing method, this paper introduces a method for the electrodeposition for RuO2/Ti and RuO2‐IrO2/Ti preparation and NaCl solution electrolysis. The deposition of Ir improves the uniformity and stability of the RuO2/Ti electrode. The optimum preparation conditions and additive concentrations were investigated in detail through the orthogonal experiment. By adjusting the electroplating time, temperature and voltage, the electrode with a high content of available chlorine was synthesized successfully. The physicochemical properties of the as‐prepared RuO2/Ti and RuO2‐IrO2/Ti were determined by XRD, SEM‐EDS, and XPS, and the electrochemical performance and lifetime of the RuO2/Ti and RuO2‐IrO2/Ti was verified via an electrochemical workstation. Uniform and stable RuO2/TiO2 and RuO2‐IrO2/TiO2 were synthesized successfully for the electrolysis of the NaCl solution. |