锌置换渣加压酸性浸出过程铁的物相转化及其影响
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摘要
研究了锌置换渣的加压酸浸过程Fe矿物相的浸出行为和浸出料浆过滤性能。利用OM、SEM-EDS、XRD、FTIR、XPS等检测手段,对原料和典型浸出渣的成分及结构进行表征分析。结果表明:Fe在锌置换渣中主要呈三价,以多孔疏松的ZnFe_2O_4形式存在;在低酸浸出渣中主要呈三价,是以外层包覆硅胶的密实ZnFe_2O_4形式存在;在高酸条件下,二价和三价共存,摩尔比约为27:23,主要以铁硅氧化物(Fe O-y SiO_2)形态存在。加压浸出可使原料中以ZnFe_2O_4形态存在的Fe大部分进入溶液,促使渣中残余Fe转化为铁硅氧化物形态,避免渣中胶质Si、Fe共存、协同恶化浸出矿浆的过滤性能,并最终与渣中的Pb沉淀重构,形成具有孔道结构的物质FeO-x Pb O-y SiO_2,有效改善了料浆的过滤性能。
T the leaching behavior of ferrous phase and the filtration performance of leaching slurry of zinc replacement residue under oxygen pressure acidity leaching process were explored. The composition and structure of raw material and typical leaching residues under different sulfuric acid concentrations were analyzed and characterized in more detail by element analysis, OM, SEM-EDS, XRD, FTIR, XPS, and etc. The results show that, in the zinc replacement residue, the iron exists as trivalent ion in the form of porous ZnFe_2O_4, and in the low acid leaching residue it presents as trivalent ion in the form of dense ZnFe_2O_4 coated with silica gel, and in the high acid leaching residue the bivalent and trivalent ion coexisted(n(Fe2+):n(Fe3+)=27:23) in the form of a kind of complex silicon/iron oxide(FeO-y SiO_2). The pressure leaching process can make most of iron elements, in form of ZnFe_2O_4, enter the solution, and at the same time the residual iron elements in the slag are transformed into Fe O-y SiO_2, and then the deterioration of the leaching slurry filtration performance can be avoided due to the absence of the coexistence of colloidal Si and Fe in the slag. Finally, the silicon/iron oxide with the lead precipitation is reorganized into a kind of material with pore structure(FeO-x Pb O-y SiO_2),which effectively improves the filtration performance of the leaching slurry.
T the leaching behavior of ferrous phase and the filtration performance of leaching slurry of zinc replacement residue under oxygen pressure acidity leaching process were explored. The composition and structure of raw material and typical leaching residues under different sulfuric acid concentrations were analyzed and characterized in more detail by element analysis, OM, SEM-EDS, XRD, FTIR, XPS, and etc. The results show that, in the zinc replacement residue, the iron exists as trivalent ion in the form of porous ZnFe_2O_4, and in the low acid leaching residue it presents as trivalent ion in the form of dense ZnFe_2O_4 coated with silica gel, and in the high acid leaching residue the bivalent and trivalent ion coexisted(n(Fe2+):n(Fe3+)=27:23) in the form of a kind of complex silicon/iron oxide(FeO-y SiO_2). The pressure leaching process can make most of iron elements, in form of ZnFe_2O_4, enter the solution, and at the same time the residual iron elements in the slag are transformed into Fe O-y SiO_2, and then the deterioration of the leaching slurry filtration performance can be avoided due to the absence of the coexistence of colloidal Si and Fe in the slag. Finally, the silicon/iron oxide with the lead precipitation is reorganized into a kind of material with pore structure(FeO-x Pb O-y SiO_2),which effectively improves the filtration performance of the leaching slurry.
引文
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[2]杨海龙,李存兄,魏昶,李旻廷,李兴彬,邓志敢,樊刚.压力场下纯异极矿高温酸转化研究[J].昆明理工大学学报(自然科学版),2015,40(5):10-16.YANG Hai-long,LI Cun-xiong,WEI Chang,LI Min-ting,LIXing-bin,DENG Zhi-gan,FAN Gang.Research on high temperature acid conversion of pure hemimorphite under pressure[J].Journal of Kunming University of Science and Technology(Natural Science Edition),2015,40(5):10-16.
[3]XU Hong-sheng,WEI Chang,LI Cun-xiong,FAN Gang,DENGZhi-gan,ZHOU Xue-jiao,QIU Shuang.Leaching of a complex sulfidic,silicate-containing zinc ore in sulfuric acid solution under oxygen pressure[J].Separation and Purification Technology,2012,85:206-212.
[4]LI Cun-xiong,XU Hong-sheng,DENG Zhi-gan,LI Xing-bin,LIMin-ting,WEI Chang.Pressure leaching of zinc silicate ore in sulfuric acid medium[J].Transactions of Nonferrous Metals Society of China,2010,20(3):913-928.
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[6]贺山明,王吉坤,闫江峰,张向阳,巨佳.氧化铅锌矿加压酸浸试验研究[J].湿法冶金,2010,29(3):159-162.HE Shan-ming,WANG Ji-kun,YAN Jiang-feng,ZHANGXiang-yang,JU Jia.Experimental study on pressure acid leaching of lead-zinc oxide ore[J].Hydrometallurgy of China,2010,29(3):159-162.
[7]贺山明,王吉坤,闫江峰,包崇军.高硅氧化铅锌矿加压酸浸中锌的浸出动力学[J].中国有色冶金,2011,40(1):63-66.HE Shan-ming,WANG Ji-kun,YAN Jiang-feng,BAOChong-jun.Leaching kinetics of zinc extracted from pressure leaching of high silica Pb-Zn oxide ore in sulfuric acid medium[J].China Nonferrous Metallurgy,2011,40(1):63-66.
[8]XU Hong-sheng,WEI Chang,LI Cun-xiong,FAN Gang,DENGZhi-gan,LI Min-ting,LI Xing-bin.Sulfuric acid leaching of zinc silicate ore under pressure[J].Hydrometallurgy,2010,105(1/2):186-190.
[9]XU Hong-sheng,WEI Chang,LI Cun-xiong,DENG Zhi-gan,FAN Gang,LI Min-ting,LI Xing-bin.Selective recovery of valuable metals from partial silicated sphalerite at elevated temperature with sulfuric acid solution[J].Journal of Industrial and Engineering Chemistry,2014,20(4):1373-1381.
[10]徐志峰,江庆政,王成彦.铁闪锌矿低温加压浸出过程中锌、硫、铁的行为[J].有色金属(冶炼部分),2012(7):6-11.XU Zhi-feng,JIANG Qing-zheng,WANG Cheng-yan.Behavior of zinc,sulfur and iron in low temperature pressure leaching process of marmatite[J].Nonferrous Metals of China(Metallurgy division),2012(7):6-11.
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[12]徐志峰,邱定蕃,王海北.铁闪锌矿加压浸出动力学[J].过程工程学报,2008,8(1):28-34.XU Zhi-feng,QIU Ding-fan,WANG Hai-bei.Pressure leaching kinetics of marmatite[J].The Chinese Journal of Process Engineering,2008,8(1):28-34.
[13]刘述平,李博,王昌良,唐湘平.从铜铅锌复杂多金属精矿中两段加压浸出锌铜铁试验研究[J].湿法冶金,2013,32(5):297-301.LIU Shu-ping,LI Bo,WANG Chang-liang,TANG Xiang-ping.Study on two stages pressure leaching of Zn,Cu and Fe from Cu-Pb-Zn complex polymetallic ore[J].Hydrometallurgy of China,2013,32(5):297-301.
[14]杨凡,邓志敢,魏昶,李存兄,李兴彬.采用赤铁矿去除高铁闪锌矿浸出液中的铁[J].中国有色金属学报,2014,24(9):2387-2392.YANG Fan,DENG Zhi-gan,WEI Chang,LI Cun-xiong,LIXing-bin.Iron-removal by hematite from leaching liquor of high iron sphalerite[J].The Chinese Journal of Nonferrous Metals,2014,24(9):2387-2391.
[15]DUTRIZAC J E,CHEN T T.Precipitation of hematite directly from ferric sulphate solutions[J].World of Metallurgy-Erzmetall,2011,64(3):134-150.
[16]杨凡,邓志敢,魏昶,李兴彬,李存兄,邱伟佳,朱如龙.高铁闪锌矿赤铁矿法除铁中锌离子和镁离子的影响及存在机理[J].中国有色金属学报,2014,24(11):2906-2913.YANG Fan,DENG Zhi-gan,WEI Chang,LI Xing-bin,LICun-xiong,QIU Wei-jia,ZHU Ru-long.Effect and existence mechanism of zinc ion and magnesium ion in iron removal from high iron sphalerite by hematite process[J].The Chinese Journal of Nonferrous Metals,2014,24(11):2906-2912.
[17]FLEURIAULT C M,ANDERSON C G,SHUEY S.Iron phase control during pressure oxidation at elevated temperature[J].Minerals Engineering,2016,(98):161-168.
[18]王益昭,李存兄,魏昶,邓志敢,李兴彬,樊刚,易烁文.湿法炼锌过程中赤铁矿生成及硫的吸附转化[J].中国有色金属学报,2017,27(10):2145-2153.WANG Yi-zhao,LI Cun-xiong,WEI Chang,DENG Zhi-gan,LIXing-bin,FAN Gang,YI Yue-wen.Production of hematite and conversion of adsorption S in zinc hydrometallurgy process[J].The Chinese Journal of Nonferrous Metals,2017,27(10):2145-2153.
[19]李存兄,魏昶,邓志敢,李兴彬,樊刚,王益昭,易烁文,李旻廷.Fe SO4-H2O体系中水热赤铁矿沉铁及亚稳态铁物相转变行为[J].中国有色金属学报,2018,28(3):628-635.LI Cun-xiong,WEI Chang,DENG Zhi-gan,LI Xing-bin,FANGang,WANG Yi-zhao,YI Yue-wen,LI Ming-ting.Hydrothermal hematite precipitation and conversion behavior of metastable iron phase in FeSO4-H2O system[J].The Chinese Journal of Nonferrous Metals,2018,28(3):628-635.
[20]艾进,申星梅,李辽沙.Fe3+离子对硅酸体系聚合行为的影响[J].过程工程学报,2013,13(6):998-1002.AI Jin,SHEN Xing-mei,LI Liao-sha.Effect of Fe3+ion on polymerization behavior of silicic acid system[J].The Chinese Journal of Process Engineering,2013,13(6):998-1002.
[21]HUANG Fei-rong,LIAO Ya-long,ZHOU Juan,WANG Yi-yang,LI Hui.Selective recovery of valuable metals from nickel converter slag at elevated temperature with sulfuric acid solution[J].Separation and Purification Technology,2015,156:572-581.
[22]LIU Fu-peng,LIU Zhi-hong,LI Yu-hu,WILSON B P,LUNDSTR?M M.Recovery and separation of gallium(III)and germanium(Ⅳ)from zinc refinery residues:Part I:Leaching and iron(Ⅲ)removal[J].Hydrometallurgy,2017,169(3):564-570.
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