School of Environmental Science and Engineering, Huazhong University of Science and Technology (HUST), 1037 Luoyu Road, Wuhan, Hubei, 430074, PR China.
J Hazard Mater. 2012 Feb 15;203-204:274-82. doi: 10.1016/j.jhazmat.2011.12.021. Epub 2011 Dec 14.
As part of contribution for developing a green recycling process of spent lead acid battery, a nanostructural lead oxide was prepared under the present investigation in low temperature calcination of lead citrate powder. The lead citrate, the precursor for preparation of this lead oxide, was synthesized through leaching of spent lead acid battery paste in citric acid solution. Both lead citrate and oxide products were characterized by means of thermogravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD), and scanning electron microscope (SEM). The results showed that the lead citrate was sheet-shape crystal of Pb(C(6)H(6)O(7)) · H(2)O. When the citrate was calcined in N(2) gas, β-PbO in the orthorhombic phase was the main product containing small amount of Pb and C and it formed as spherical particles of 50-60 nm in diameter. On combusting the citrate in air at 370°C (for 20 min), a mixture of orthorhombic β-PbO, tetragonal α-PbO and Pb with the particle size of 100-200 nm was obtained, with β-PbO as the major product. The property of the nanostructural lead oxide was investigated by electrochemical technique, such as cyclic voltammetry (CV). The CV measurements presented the electrochemical redox potentials, with reversibility and cycle stability over 15 cycles.
作为开发废铅酸电池绿色回收工艺的贡献之一，本研究在低温下煅烧柠檬酸铅粉末，制备了纳米结构的氧化铅。柠檬酸铅是制备这种氧化铅的前体，通过浸出废铅酸电池膏在柠檬酸溶液中合成。柠檬酸铅和氧化物产物均通过热重-差热分析（TG-DTA）、X 射线衍射（XRD）和扫描电子显微镜（SEM）进行了表征。结果表明，柠檬酸铅为 Pb(C6H6O7)·H2O 的片状晶体。当柠檬酸在 N2 气体中煅烧时，主要产物为正交相的β-PbO，含有少量 Pb 和 C，它形成直径为 50-60nm 的球形颗粒。在空气（370°C，20min）中燃烧柠檬酸时，得到了正交相β-PbO、四方相α-PbO 和 Pb 的混合物，粒径为 100-200nm，其中β-PbO 为主要产物。通过电化学技术，如循环伏安法（CV），研究了纳米结构氧化铅的性能。CV 测量结果表明，具有电化学氧化还原电位，在 15 个循环中具有可逆性和循环稳定性。
