| At present,there is a sharp decline in the reserves of lead ores and it is impossible to meet the production demand simply by relying on native lead ores.However,the disposal of lead wastes can cause serious pollution to the environment,so it is very important to realize the recycling of lead.The purpose of this study is to find the efficient and clean technology to convert the lead paste of lead waste storage battery and chlorinated lead slag into available lead resources.With the rapid development of energy storage industry,lead acid batteries need to improve their performance to meet the demand of energy storage market,and the research of new type of lead acid battery materials is very urgent.First of all,the lead paste of lead waste storage battery this study was used as the raw materials to prepare the high performance PbO2 materials by liquid phase for the first time in this study.And the?NH4?2S2O8 was used as oxidant.The results in this study prove that the content of Pb O2 can be up to 99.07%when the reaction temperature is 80?,the ratio of?NH4?2S2O8 dosage and the theoretical value is 2.5 to 3,the quality ratio of ammonia and distilled water is 2 to 3 and the reaction time is 6 to 8hours.The XRD spectra shows that there are two kinds of crystal type which is?-PbO2and?-Pb O2 in the products.And the products have a smaller particle size and a porous shape on the surface.Secondly,the desulphurization lead paste was used as lead source and the ethylene glycol was used as carbon source to prepare lead carbon composite materials by solvent heat method for the first time in this study.The research shows that the products is mainly a complex of the elemental lead and carbon when the quality ratio of ethylene glycol and desulfurization lead paste is 15 to 20,the reaction temperature is 230?to 240?and the reaction time is 10 to 12 hours.The recycling process of chlorinated lead slag is a difficult problem in the hydrometallurgical process of chlorination.It is the first time that chlorinated lead slag which produced in the process of electrolytic copper anode slime was dechlorinated under the system of ammonia and carbon dioxide.The research shows that the dechlorination rate can be up to 99.02%when the dosage of ammonia is 2 to 3 times as much as the theory,the ratio of liquid and solid is 3 to 4,the reaction time is 4 to 5hours and the reaction temperature is 35?to 45?.Then the dechlorination products were calcined in the muffle furnace to prepare yellow lead?Pb O?and red lead?Pb3O4?.The research shows that the content of Pb O in the yellow lead can be up to99.5%when the calcination temperature is 620?and the calcination time is 3 hours.The XRD spectrum shows that the major component of the products are?-PbO.The content of Pb O2 in the red lead can reach 32.72%when the calcination temperature is480?and the calcination time is 3 hours.This study tried to improve the yield of red lead by adding the?NH4?2S2O8 to oxidate divalent lead ion in the dechlorination process.And the content of Pb O2 in the product of red lead can reach 34.26%when the dosage of?NH4?2S2O8 is 1.5 to 2 times as much as the theoretical value.This paper explored the method of preparing high purity Pb O2 powder and lead carbon composite materials by using lead paste of waste lead-acid battery as materials and the reach of chlorinated lead residue's dechlorination process and the process of preparing red and yellow lead.It provides new methods for the recovery and utilization of solid waste containing lead. |
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