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In this work, the alkaline refining of arsenic in crude lead was studied with a mixture of sodium hydroxide and sodium carbonate as alkaline refining agents. Taking the arsenic removal rate as the research object, the effects of reaction temperature, holding time, Na2CO3:NaOH, the dosage of refining agent were investigated. The arsenic removal rate is 79.09% under the optimum experimental conditions as follows: reaction temperature 823 K, holding time 60 min, Na2CO3:NaOH 1:4, refining agent dosage 10%. The oxidation purification mechanism of arsenic was studied by XPS, SEM-EDS, XRD and FT-IR. The results show that arsenic in the crude lead is gradually oxidized by oxygen and lead oxide during arsenic removal process, and the arsenic trioxide is eventually converted into sodium arsenate (Na3AsO4) and lead arsenate (Pb2As2O7) in the slag.

Studies on the effective extraction and separation of zinc-iron from spent pickling solution using tri-n-octylamine (TOA) with solvent extraction were investigated. Single extraction efficiency of 83.75% is obtained under the optimal conditions (organic phase consisting of 30% (v/v) extractant TOA, 20% (v/v) modifier iso-octanol, and 50% (v/v) diluent sulfonated kerosene, organic phase volume: aqueous phase volume of 2:1, and extraction time 10 min), while only 1.8% iron is co-extracted. McCabe-Thiele diagram is employed to analyze the number of theoretical stages needed for the effective extraction of zinc, and it is found that under five-stage counter-current extraction, almost all the zinc ions are extracted. A stripping efficiency of more than 90% from the loaded organic phase is achieved by 2.0 mol/L NH3·H2O and organic phase volume: aqueous phase volume of 1:2. Furthermore, the extraction mechanism of zinc with TOA accompanied by anion exchange is demonstrated by FT-IR spectra analysis and ESI-MS analysis, and the structure of the extracted complex is confirmed as [ R 3 N H Z n C l 3 ] .