硫化铅精矿和废铅膏泥同时浸出过程研究
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摘要
研究了硫化铅精矿和废铅膏泥同时浸出过程。同时浸出过程涉及两个阶段:(1)在盐酸溶液中,铅精矿中的PbS和废铅膏泥中的PbO、PbO_2、Pb被转化为固体PbCl_2;(2)固体PbCl_2和废铅膏泥中的PbSO_4与MgCl_2反应生成可溶性的配合物MgPbCl_4。第一阶段中的一个关键技术是PbO_2用作PbS的氧化剂,或PbS用作PbO_2的还原剂。两个阶段的总结果是产出了浸出渣和浸出液。从浸出液中可结晶出PbCl_2。第二阶段的过程是铅氯化-湿法冶金中的成熟技术,本研究的重点集中在第一阶段的条件试验。第二阶段采用固定试验条件:浸出温度95℃,溶液中MgCl_2浓度5.5mol/L,浸出时间3h。通过试验确定的第一阶段最佳试验条件:废铅膏泥与铅精矿的质量比3.5∶1,液固比4∶1,溶液pH2.0,转化温度55℃,转化时间4h。试验结果表明,在上述试验条件下,硫化铅精矿和废铅膏泥同时浸出过程的浸出渣含铅达到1.8%,铅浸出率为99.44%。
A process for simultaneous leaching of lead concentrate and spent lead paste was investigated.The process involved two stages:The first is in hydrochloric acid solution,PbS in lead concentrate and PbO、PbO_2、Pb in spent lead paste were converted to solid PbCl_2;The second is the solid PbCl_2 and PbSO_4 in spent lead paste reacted with MgCl_2 to produce soluble complex compound MgPbCl_4.As a key technology in the first stage,PbO_2 was used as oxidant of PbS,or PbS was used as reductant of PbO_2.The total result of two stages was to produce leach residue and leach solution,from which PbCl_2 can be crystallized.The second stage is a mature technology in the chloride hydrometallurgy of lead and focus of this study was centred on condition experiments of the first stage.The second stage used fixed experiment conditions:leaching temperature 95℃,concentration of MgCl25.5 mol/L and leaching time 3 h.The optimal conditions of the first stage determined by experiments:the mass ratio of spent lead paste and lead concentrate3.5∶1;the ratio of liquid and solid 4∶1;solution pH 2.0;conversion temperature 55℃;conversion time4 h.Experiment results indicated that lead content in leach residue from process for simultaneous leaching of lead concentrate and spent lead paste reached 1.8%,leach efficiency of lead 99.44%under the above experimental conditions.
A process for simultaneous leaching of lead concentrate and spent lead paste was investigated.The process involved two stages:The first is in hydrochloric acid solution,PbS in lead concentrate and PbO、PbO_2、Pb in spent lead paste were converted to solid PbCl_2;The second is the solid PbCl_2 and PbSO_4 in spent lead paste reacted with MgCl_2 to produce soluble complex compound MgPbCl_4.As a key technology in the first stage,PbO_2 was used as oxidant of PbS,or PbS was used as reductant of PbO_2.The total result of two stages was to produce leach residue and leach solution,from which PbCl_2 can be crystallized.The second stage is a mature technology in the chloride hydrometallurgy of lead and focus of this study was centred on condition experiments of the first stage.The second stage used fixed experiment conditions:leaching temperature 95℃,concentration of MgCl25.5 mol/L and leaching time 3 h.The optimal conditions of the first stage determined by experiments:the mass ratio of spent lead paste and lead concentrate3.5∶1;the ratio of liquid and solid 4∶1;solution pH 2.0;conversion temperature 55℃;conversion time4 h.Experiment results indicated that lead content in leach residue from process for simultaneous leaching of lead concentrate and spent lead paste reached 1.8%,leach efficiency of lead 99.44%under the above experimental conditions.
引文
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[16]李淑梅,刘凯华,丛自范.用氯化铅制取氧化铅试验研究[J].当代学术发展研究,2012,(10):29-31.
[17] Kumar R V,Sonmez M S,Kotzeva V P.Lead Recycling[P].British Pat.:GB0622249.1,2006-08-11.
[18] Sonmez M S,Kumar R V.Leaching of Waste Battery Paste Components:Part 1.Lead Citrate Synthesis from PbO and PbO2[J].Hydrometallurgy,2009,95:53-60.
[19] Sonmez M S,Kumar R V.Leaching of Waste Battery Paste Components:Part 2.Leaching and Desulphurisation of PbSO4by Citric Acid and Sodium Citrate Solution[J].Hydrometallurgy,2009,95:82-86.
[2]李卫锋,蒋丽华,湛晶,张传福.废铅酸蓄电池铅再生技术现状及进展[J].中国有色冶金,2011,(6):53-56.
[3]陈曦,祁国恕,惠怀胜,张正洁.我国废铅酸蓄电池火法冶炼污染防治最佳可行技术研究[J].资源再生,2012,(6):54-56.
[4]杜新玲,王国富.废旧铅酸蓄电池密闭短窑熔炼的生产实践[J].中国有色冶金,2013,42(4):34-38.
[5]焦志良,陈为亮,张旭,朱玉平,许康,齐妍洁.从二次含铅物料中湿法回收铅的研究现状[J].湿法冶金,2014,33(2):90-92.
[6]王玉,王刚,马成兵,刘树军,于少明,黄宪法.废铅蓄电池铅膏湿法回收制取氯化铅技术的研究[J].安徵化工,2010,36(6):24-27.
[7]齐美富,郑园芳,桂双林.废铅酸蓄电池中铅膏氯盐体系浸取铅的动力学研究[J].矿冶工程,2010,30(6):61-64.
[8]周鸿燕,马旭.氟硼酸浸出电解法回收高纯度铅[J].腐蚀与防护,2014,35(12):1274-1277.
[9]尹文新,韩跃新,王德全.湿法炼铅研究进展[J].矿冶,2005,14(3):49-52.
[10]何东升,朱新锋,刘建文,高林霞,杨家宽.废铅酸蓄电池铅膏柠檬酸浸出动力学研究[J].环境工程学报,2012,6(2):623-626.
[11]朱新锋,王现丽,聂鹏茹,张伟,胡雨辰,杨家宽,汪潇,郭一飞.湿法回收废铅膏中间产物柠檬酸铅Pb3(C6H5O7)2·3H2O的热分解[J].中国有色金属学报,2016,26(12):2686-2693.
[12]马琳亭,李玉.铅酸蓄电池拆解分选新工艺研究[J].甘肃冶金,2014,36(1):111-112.
[13]李淑梅,张福生,丛自范,于文圣.固体氯化铅直接低温熔炼生产粗铅的研究[J].有色矿冶,2011,27(2):28-30.
[14] Das S C,Subbaiah T,Sahoo P K.Electrowinning of lead from its chloride bath containing organic additives[J].Hydrometallurgy,1989,21(3):373-383.
[15]Wang Xiang wen,Martioins,Gerard P.Electrochemical aspects of electrowinning lead metal from brine lead chloride electrolytes in the temperature range 55~80℃proceedings of the 1993EPD congress[C].TMS,1993,21-25.
[16]李淑梅,刘凯华,丛自范.用氯化铅制取氧化铅试验研究[J].当代学术发展研究,2012,(10):29-31.
[17] Kumar R V,Sonmez M S,Kotzeva V P.Lead Recycling[P].British Pat.:GB0622249.1,2006-08-11.
[18] Sonmez M S,Kumar R V.Leaching of Waste Battery Paste Components:Part 1.Lead Citrate Synthesis from PbO and PbO2[J].Hydrometallurgy,2009,95:53-60.
[19] Sonmez M S,Kumar R V.Leaching of Waste Battery Paste Components:Part 2.Leaching and Desulphurisation of PbSO4by Citric Acid and Sodium Citrate Solution[J].Hydrometallurgy,2009,95:82-86.
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