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Lead sulfate, lead oxides and lead metal are the main component of lead paste in spent lead acid battery. When lead sulfate was desulfurized and transformed into lead carbonate by sodium carbonate, lead metal and lead oxides remained unchanged. Lead carbonate is easily decomposed to lead oxide and carbon dioxide under high temperature. Namely, vacuum thermal process is the reduction reaction of lead oxides. A compatible environmental process consisted of hydrometallurgical desulfurization and vacuum thermal reduction to recycle lead was investigated in this research. Lead paste was firstly desulfurized with sodium carbonate, by which, the content of sulfur declined from 7.87% to 0.26%. Then, the desulfurized lead paste was reduced by charcoal under vacuum. Under the optimized reaction conditions, i.e., vacuum thermal reduction at temperature 850 °C under 20 Pa for 45 min, a 22.11 × 10 −2 g cm −2 min −1 reduction rate, and a 98.13% direct recovery ratio of fine lead (99.77%) had been achieved, respectively. [ABSTRACT FROM AUTHOR]

• A novel technology, for atomic economic recovery of lead paste, is proposed. • Direct recovery ratio of Pb reaches 99.29%, which means that Pb-loss is very little. • Sb-content in crude Pb-Sb alloy decreased from 46% to 0.98%. • The technology has advantages of lower cost and less pollution, etc. Until today, there are still many problems that must be solved through innovative research to make the recycling of spent lead-acid batteries and the separation of Pb-Sb alloy more environmentally friendly and energy-saving. In this paper, a novel method for regenerating lead paste, by vacuum reduction reaction coupling with separation of Pb-Sb alloy, was developed. In this process, antimony from Pb-Sb alloy is used to reduce desulfurized lead paste into lead under vacuum, while it is oxidized into volatile Sb 2 O 3 as by-product. The results showed that direct recovery ratio of Pb from desulfurized lead paste reached 99.29% and Sb-content in Pb-Sb alloy decreased from 46% to 0.98% under following conditions: the mass ratio of desulfurized lead paste to Pb-Sb alloy of 1.50, residual gas pressure of 30 Pa, reduction temperature of 810 °C for 50 min. By this method, not only the lead paste can be recovered with high atom economy, but also the Pb-Sb alloy can be separated efficiently at zero cost and without "three wastes" generation. Therefore, this method is very useful for the recycling of spent lead-acid battery and the separation of Pb-Sb alloy. [ABSTRACT FROM AUTHOR]