ABSTRACT In this study, an efficient method of lead recovery from lead sulfate in spent lead-acid batteries assisted by ultrasonic is developed using the citric acid–sodium citrate solution. Ultrasonic-assisted technology is employed to enhance the kinetics of lead sulfate leaching. Initially, the predominance area of the lead citrate complexes was analyzed. The study was conducted to evaluate the effect of ultrasonic-assisted technology on the kinetic behavior of lead sulfate within the citric acid–sodium citrate solution, thereby unveiling the differences between ultrasonic-assisted leaching and the non-ultrasonic-assisted leaching. Kinetic study indicated that the employment of ultrasonic-assisted technology could effectively reduce the apparent activation energy during the desulfurization process, decreasing the energy initially required from 43.27 kJ/mol to 35.15 kJ/mol. Furthermore, the ultrasonic-assisted leaching led to successful preparation of lead citrate precursor, characterized by a smaller particle size and larger specific surface area. Systematic investigations were performed on the thermal decomposition process of these precursors and the effects of calcination temperature and holding time on the properties of calcination products. It was revealed that pure porous lead oxide powder with a purity of 99.9% could be produced successfully under the conditions of calcination temperature at 350°C and holding time of 1 h. The research provides an innovative process for the efficient recovery of lead from spent lead acid batteries.