| Under the situation that mineral resources are gradually exhausted,it is of great economic and social benefit to strengthen the comprehensive recovery and utilization of valuable metals from the secondary resources such as waste circuit board,waste catalyst and waste power battery.Due to the high grade of valuable metal components in these secondary resources,the industrial sulfuric acid leaching system without selectivity results in the coexistence of multiple metal components in the leachate,which brings great difficulties for subsequent separation and recovery.In this paper,the separation of valuable metal ions from waste hydrogenation catalyst and sulfuric acid leaching solution of waste lithium ion battery was studied,and the separation behavior of valuable metal ions was systematically studied by solvent extraction method.The main research contents and conclusions are as follows:（1）The extraction separation of Ni,Mo,V and Al from sulfuric acid leachates of waste hydrogenation catalyst was studied.Based on molecular interaction,selective co-extraction of Mo and V was achieved,and then the selective separation of V from the loaded organic phase was achieved by reducing stripping.The selective separation of Ni in the raffinate could be achieved by commercial extractant HBL110.The effects of p H,time,and composition of extractant on the extraction separation were investigated.When the concentration of TOA and Cyanex272 in mixed extractant was 0.5 mol·L-1 and 0.5 mol·L-1,the extraction time was 5 min,and the extraction ratio was 1:1（O/A）,the extraction efficiencies of Ni,Mo,V and Al at 25℃and p H=1 were 0%,99.98%,97.5%and 0%,respectively.The removal efficiency of V in the organic phase was 83%by using 1mol·L-1 H2SO4+0.75 mol·L-1 Na2SO3,and 98%of Mo can be stripped from the organic phase by using 1 mol·L-1 Na OH+0.5 mol·L-1Na Cl.The extraction efficiency of 98.5%can be achieved for Ni by using50%（v/v）HBL110 at equilibrium p H=3.81,and 1 mol·L-1 H2SO4 can completely strip Ni from organic phase.Furthermore,the molybdenum and vanadium species in the leachate were studied by UV-vis and Raman spectroscopies,and the reduction stripping mechanism of vanadium was revealed.FT-IR,NMR,and ESI-MS spectra were combined to reveal the interaction of extraction agent and its influence on separation.（2）The extraction separation of Li,Co,Ni and Mn in the sulfuric acid leachates of spent lithium ion battery was studied.Based on the interaction between the molecules,the simultaneous extraction of Co and Mn was achieved and the complexation stripping was used to selectively separate Co in the loaded organic phase.The effects of p H,time,saponification rate,and composition of extractant on the extraction separation were investigated.Under the conditions of 25℃,p H=2.66,0.1 mol·L-1Cyanex272 and 0.1 mol·L-1P507 in the mixed extractant,saponification rate of 50%,extraction ratio of 1:1（O/A）,the extraction efficiency of Li,Co,Ni and Mn were 0.75%,99.59%,2.5%and 99.91%,respectively.The stripping effeciency of Co in the loaded organic phase was 86%with 2mol·L-1（NH4）2CO3.The residual Mn can be completely stripped from the organic phase by 0.1 mol·L-1 H2SO4.Ni in the raffinate can be selectively separated by 0.5 mol·L-1 Cyanex302 with an extraction percentage of 99.95%at equilibrium p H=6.4.Ni in the loaded organic phase can be completely removed by 0.5 mol·L-1 H2SO4.FT-IR,NMR,and ESI-MS spectra were used to disclose the interaction of the mixed extractants and its influence on metal separation.This paper includes 34 figures,5 tables and 156 references... |
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