铜烟灰浓硫酸熟化—浸出提铟工艺研究
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摘要
针对株洲冶炼厂硫酸浸出铜烟灰提铟工艺,采用电感耦合等离子体光谱仪(ICP)与X射线衍射仪(XRD)对铜烟灰进行化学组成及物相分析,发现浸出率较低的主要原因是常规酸浸时,被石英和部分硫化物包裹的铟不能被有效浸出。根据吉布斯自由能变化及E-pH图等热力学计算,基于现有技术参数,以铟的浸出率为指标,探索浓硫酸熟化浸出工艺。通过单因素实验,重点考察了酸矿比、熟化时间、浸出时间对铟浸出效果的影响。结果表明,酸矿比1.5、熟化时间2h、水浸温度90℃、水浸时间2h、高锰酸钾添加量为0.3%、水浸过程保持液固比6∶1的条件下,铟的浸出效果最优。利用最优工艺参数条件进行综合实验,铟浸出率由原工艺的65.73%提高到88%以上,同时浓硫酸熟化实验浸出液中铟及其他金属离子的浸出率较常规酸浸高。研究结果对指导企业生产有重要意义。
In order to analyze the chemical composition and phase of copper soot by inductively coupled plasma spectrometer(ICP)and X-ray diffraction(XRD),the infiltration of copper soot in the sulfuric acid leaching process of Zhuzhou Smelter was found to be the main reason for the low leaching rate.In the case of conventional acid leaching,indium encapsulated by quartz and partial sulfide cannot be effectively leached.According to the thermodynamic calculations such as Gibbs free energy change and E-pH map,based on the existing technical parameters,the leaching rate of indium was characterized,and the concentrated sulfuric acid ripening and leaching process were explored.The effects of acid oreratio,curing time and leaching time on the indium infiltration leaching were investigated by single factor experiment.The results show that when the acid oreratio is 1.5,the curing time is 2 h,the water leaching temperature is 90 ℃,the water immersion time is 2 h,the potassium permanganate addition is 0.3%,and the water immersion process maintained the liquid-solid ratio of 6∶1,the leaching effect is optimal.Comprehensive experiments using the optimum process parameters show that the indium leaching rate increases from 65.73% to 88%,and the indium and other metal ions leaching rate in the sulfuric acid ripening leaching solution arerelatively higher than that of the conventional acid leaching,which is of great significance to enterprise production.
In order to analyze the chemical composition and phase of copper soot by inductively coupled plasma spectrometer(ICP)and X-ray diffraction(XRD),the infiltration of copper soot in the sulfuric acid leaching process of Zhuzhou Smelter was found to be the main reason for the low leaching rate.In the case of conventional acid leaching,indium encapsulated by quartz and partial sulfide cannot be effectively leached.According to the thermodynamic calculations such as Gibbs free energy change and E-pH map,based on the existing technical parameters,the leaching rate of indium was characterized,and the concentrated sulfuric acid ripening and leaching process were explored.The effects of acid oreratio,curing time and leaching time on the indium infiltration leaching were investigated by single factor experiment.The results show that when the acid oreratio is 1.5,the curing time is 2 h,the water leaching temperature is 90 ℃,the water immersion time is 2 h,the potassium permanganate addition is 0.3%,and the water immersion process maintained the liquid-solid ratio of 6∶1,the leaching effect is optimal.Comprehensive experiments using the optimum process parameters show that the indium leaching rate increases from 65.73% to 88%,and the indium and other metal ions leaching rate in the sulfuric acid ripening leaching solution arerelatively higher than that of the conventional acid leaching,which is of great significance to enterprise production.
引文
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[17]胡一平.复杂转炉渣中铟的浸出工艺研究[D].长沙:中南大学,2010.HU Yiping.Study on leaching technology of indium from a complex converter slag[D].Changsha:Central South University,2010.
[18]王洪琼.关于浓硫酸和稀硫酸氧化性的探讨[J].四川师范学院学报(自然科学版),1999(3):301-302.WANG Hongqiong.Probing into oxidation of concentrated sulfuric acid and dilute sulfuric acid[J].Journal of China West Normal University(Natural Sciences),1999(3):301-302.
[19]马保中,金炳界,裴彦林,等.褐铁型红土镍矿硫酸熟化过程及其机制研究[J].稀有金属,2017,41(10):1159-1166.MA Baozhong,JIN Bingjie,PEI Yanlin,et al.Process and mechanism study on activation pretreatment of limonitic lateriteOres at Low Temperature[J].Chinese Journal of Rare Metals,2017,41(10):1159-1166.
[2]王树楷.铟的应用与提取进展[J].中国工程科学,2008(5):85-94.WANG Shukai.Progress of extraction and application of indium[J].Engineering Sciences,2008(5):85-94.
[3]ZHU G C,ZHENG M D,FAN G L,et al.Recovering indium with sulfating roasting from copper-smelting-ash[J].Rare Metals,2007,26(5):488-491.
[4]KOLEINI S M J,MEHRPOUYA H,SABERYAN K,et al.Extraction of indium from zinc plant residues[J].Minerals Engineering,2010,23(1):51-53.
[5]ZHANG K,WU Y,WANG W,et al.Recycling indium from waste LCDs:A review[J].Resources Conservation&Recycling,2015,104:276-290.
[6]王建芳,徐杰,王君,等.从铟浮渣碱渣中回收铟的工艺研究[J].中国有色冶金,2018,47(1):65-67.WANG Jianfang,XU Jie,WANG Jun,et al.Process study on indium recovery from indium dross and alkaline residue[J].China Nonferrous Metallurgy,2018,47(1):65-67.
[7]曹笑,郭学益,李栋,等.从二次资源中回收铟的研究现状[J].金属材料与冶金工程,2015,43(2):42-47.CAO Xiao,GUO Xueyi,LI Dong,et al.Status of indium recovery from secondary resources[J].Metal Materials and Metallurgy Engineering,2015,43(2):42-47.
[8]周玉琳.提高锌精矿中铟回收率的实践[J].有色金属(冶炼部分),2015(1):50-53.ZHOU Yulin.Plant practice to improve indium recovery rate from zinc concentrate[J]. Nonferrous Metals(Extractive Metallurgy),2015(1):50-53.
[9]SAWAI H,RAHMAN I M M,TSUKAGOSHI Y,et al.Selective recovery of indium from lead-smelting dust[J].Chemical Engineering Journal,2015,277:219-228.
[10]PEREIRA E B,SULIMAN A L,TANABE E H,et al.Recovery of indium from liquid crystal displays of discarded mobile phones using solvent extraction[J].Minerals Engineering,2018,119:67-72.
[11]吴军,宋祥莉,姜国敏.铜闪速炉烟灰硫酸化焙烧后焙砂浸出试验研究[J].有色金属(冶炼部分),2012(5):5-7.WU Jun,SONG Xiangli,JIANG Guomin.Study on leaching of calcine from sulphating roasting dust of copper flash smelting furnace[J].Nonferrous Metals(Extractive Metallurgy),2012(5):5-7.
[12]严浩.一种处理富铟渣的工艺[J].世界有色金属,2017(15):11-12.YAN Hao.Treatment process for rich indium residue[J].World Nonferrous Metals,2017(15):11-12.
[13]薛永建,翟爱萍,尹荣花.从氧化锌中回收铟的工艺改进[J].江西有色金属,2010,24(增刊1):124-125.XUE Yongjian, ZHAI Aiping, YIN Ronghua.Technology improvement of indium recovery out of zinc oxide[J].Nonferrous Metals Science and Engineering,2010,24(s1):124-125.
[14]周正华.铜烟灰回收铟工艺研究[J].稀有金属,2007(增刊1):118-121.ZHOU Zhenghua.Study of indium reclaiming technology from copper-smelting dust[J].Chinese Journal of Rare Metals,2007(s1):118-121.
[15]饶兵,戴惠新,高利坤.冶炼废渣中铟回收技术进展[J].化工进展,2016,35(12):4042-4052.RAO Bing,DAI Huixin,GAO Likun.Metallurgical progress of recovery indium from smelt residues[J].Chemical Industry and Engineering Progress,2016,35(12):4042-4052.
[16]李路路.提高高铟烟灰中铟浸出率的研究[D].西安:西安建筑科技大学,2018.LI Lulu.Study on increasing indium leaching rate in indium ash[D].Xi'an:Xi'an University of Architectural and Technology,2018.
[17]胡一平.复杂转炉渣中铟的浸出工艺研究[D].长沙:中南大学,2010.HU Yiping.Study on leaching technology of indium from a complex converter slag[D].Changsha:Central South University,2010.
[18]王洪琼.关于浓硫酸和稀硫酸氧化性的探讨[J].四川师范学院学报(自然科学版),1999(3):301-302.WANG Hongqiong.Probing into oxidation of concentrated sulfuric acid and dilute sulfuric acid[J].Journal of China West Normal University(Natural Sciences),1999(3):301-302.
[19]马保中,金炳界,裴彦林,等.褐铁型红土镍矿硫酸熟化过程及其机制研究[J].稀有金属,2017,41(10):1159-1166.MA Baozhong,JIN Bingjie,PEI Yanlin,et al.Process and mechanism study on activation pretreatment of limonitic lateriteOres at Low Temperature[J].Chinese Journal of Rare Metals,2017,41(10):1159-1166.