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Preparation of High-Purity Lead Chloride and Lead Oxide from Spent Lead Paste by Crystallization

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Abstract

Compared with conventional pyrometallurgical recycling, hydrometallurgical recycling offers distinct advantages by mitigating emissions of waste gas and lead-containing dust; however, it also encounters challenges in effectively eliminating metal impurities from spent lead paste. This study presents a novel hydrometallurgical process for the recovery of spent lead paste, which entails the production of high-purity lead chloride through crystallization, coupled with the recovery of lead oxide via dechlorination, thereby realizing the preparation of high-purity recovered products. First, sulfated lead paste was leached using a sodium chloride solution. Lead could be completely leached when the solid–liquid ratio was 40 g·L−1, the concentration of sodium chloride solution was 250 g·L−1, the reaction temperature was 80 °C, and the leaching time was 20 min. Subsequently, the leachate was filtered and further treated through dilution with distilled water (at 1.6 times) at 0 °C, thereby yielding high-purity lead chloride through the crystallization process, wherein metal impurities were effectively prevented from precipitating out. Finally, the lead chloride product was dechlorinated using sodium hydroxide solution. The dechlorination conditions were as follows: the solid–liquid ratio was 136.09 g·L−1, the crystallization temperature was 0 °C, and the concentration of sodium hydroxide solution was 11.51 mol·L−1. α-PbO was obtained under these conditions. In this study, spent lead paste was recycled with the advantages of low energy consumption and no harmful gas emissions, thereby providing a new idea for recycling lead-containing waste.

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References

  1. May GJ, Davidson A, Monahov B (2018) Lead batteries for utility energy storage: a review. J Energy Storage 15:145–157. https://doi.org/10.1016/j.est.2017.11.008

    Article  Google Scholar 

  2. Zou C, Zhang L, Hu X et al (2018) A review of fractional-order techniques applied to lithium-ion batteries, lead-acid batteries, and supercapacitors. J Power Sources 390:286–296. https://doi.org/10.1016/j.jpowsour.2018.04.033

    Article  CAS  Google Scholar 

  3. He Y, Zheng Y, Wu Y et al (2019) Tracking flows of secondary vehicle batteries in China. Resour Conserv Recycl 142:34–36. https://doi.org/10.1016/j.resconrec.2018.11.016

    Article  Google Scholar 

  4. Zhang W, Yang J, Wu X et al (2016) A critical review on secondary lead recycling technology and its prospect. Renew Sust Energ Rev 61:108–122. https://doi.org/10.1016/j.rser.2016.03.046

    Article  CAS  Google Scholar 

  5. Rada S, Cuibus D, Vermesan H et al (2018) Structural and electrochemical properties of recycled active electrodes from spent lead acid battery and modified with different manganese dioxide contents. Electrochim Acta 268:332–339. https://doi.org/10.1016/j.electacta.2018.02.135

    Article  CAS  Google Scholar 

  6. Li M, Yang J, Liang S et al (2019) Review on clean recovery of discarded/spent lead-acid battery and trends of recycled products. J Power Sources 436:226853. https://doi.org/10.1016/j.jpowsour.2019.226853

    Article  CAS  Google Scholar 

  7. Li Y, Yang S, Taskinen P et al (2019) Novel recycling process for lead-acid battery paste without SO2 generation - Reaction mechanism and industrial pilot campaign. J Clean Prod 217:162–171. https://doi.org/10.1016/j.jclepro.2019.01.197

    Article  CAS  Google Scholar 

  8. Xing P, Wang C, Wang L et al (2019) Hydrometallurgical recovery of lead from spent lead-acid battery paste via leaching and electrowinning in chloride solution. Hydrometallurgy 189:105134. https://doi.org/10.1016/j.hydromet.2019.105134

    Article  CAS  Google Scholar 

  9. Huang K, Liu H, Dong H et al (2021) A novel approach to recover lead oxide from spent lead acid batteries by desulfurization and crystallization in sodium hydroxide solution after sulfation. Resour Conserv Recycl 167:105385. https://doi.org/10.1016/j.resconrec.2020.105385

    Article  CAS  Google Scholar 

  10. Zhu X, Yang J, Gao L et al (2013) Preparation of lead carbonate from spent lead paste via chemical conversion. Hydrometallurgy 134–135:47–53. https://doi.org/10.1016/j.hydromet.2013.01.018

    Article  CAS  Google Scholar 

  11. Zhu X, Zhang W, Zhang L et al (2019) A green recycling process of the spent lead paste from discarded lead–acid battery by a hydrometallurgical process. Waste Manage Res 37:508–515. https://doi.org/10.1177/0734242X19830175

    Article  CAS  Google Scholar 

  12. Ye L, Duan L, Liu W et al (2020) Facile method for preparing a nano lead powder by vacuum decomposition from spent lead-acid battery paste: leaching and desulfuration in tartaric acid and sodium tartrate mixed lixivium. Hydrometallurgy 197:105450. https://doi.org/10.1016/j.hydromet.2020.105450

    Article  CAS  Google Scholar 

  13. Zhu X, He X, Yang J et al (2013) Leaching of spent lead acid battery paste components by sodium citrate and acetic acid. J Hazard Mater 250–251:387–396. https://doi.org/10.1016/j.jhazmat.2013.02.018

    Article  CAS  Google Scholar 

  14. Yu W, Yang J, Li M et al (2019) A facile lead acetate conversion process for synthesis of high-purity alpha-lead oxide derived from spent lead-acid batteries. J Chem Technol Biot 94:88–97. https://doi.org/10.1002/jctb.5748

    Article  CAS  Google Scholar 

  15. Li M, Yang J, Liang S et al (2020) A closed-loop ammonium salt system for recovery of high-purity lead tetroxide product from spent lead-acid battery paste. J Clean Prod 250:119488. https://doi.org/10.1016/j.jclepro.2019.119488

    Article  CAS  Google Scholar 

  16. Deng X, Liu W, Zhang D et al (2021) Hydrothermal desulfurization of spent lead paste based on comproportionation reaction. Sep Purif Technol 259:118115. https://doi.org/10.1016/j.seppur.2020.118115

    Article  CAS  Google Scholar 

  17. Hu G, Zhang P, Yang J et al (2022) A closed-loop acetic acid system for recovery of PbO@C composite derived from spent lead-acid battery. Resour Conserv Recycl 184:106391. https://doi.org/10.1016/j.resconrec.2022.106391

    Article  CAS  Google Scholar 

  18. Wu Y, Chen Z, Yu Q et al (2022) Preparation of high-purity lead carbonate and lead oxide from spent lead paste. J Clean Prod 372:133786. https://doi.org/10.1016/j.jclepro.2022.133786

    Article  CAS  Google Scholar 

  19. Wang J, Yang J, Hou H et al (2021) A green strategy to synthesize two-dimensional lead halide perovskite via direct recovery of spent lead-acid battery. Resour Conserv Recycl 169:105463. https://doi.org/10.1016/j.resconrec.2021.105463

    Article  CAS  Google Scholar 

  20. Pan J, Zhang X, Sun Y et al (2016) Preparation of high purity lead oxide from spent lead acid batteries via desulfurization and recrystallization in sodium hydroxide. Ind Eng Chem Res 55:2059–2068. https://doi.org/10.1021/acs.iecr.5b04221

    Article  CAS  Google Scholar 

  21. Shu Y, Ma C, Zhu L, Chen H (2015) Leaching of lead slag component by sodium chloride and diluted nitric acid and synthesis of ultrafine lead oxide powders. J Power Sources 281:219–226. https://doi.org/10.1016/j.jpowsour.2015.01.181

    Article  CAS  Google Scholar 

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Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (No.51464021).

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Correspondence to Qiang Yu or Zhen Chen.

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Wu, Y., Wang, M., Yu, Q. et al. Preparation of High-Purity Lead Chloride and Lead Oxide from Spent Lead Paste by Crystallization. J. Sustain. Metall. 9, 1777–1789 (2023). https://doi.org/10.1007/s40831-023-00764-4

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