Abstract:The red mud sample was dissolved with nitric acid, hydrofluoric acid and sulfuric acid followed by passing strongly acid exchange resin (Dowex50W-X8, H+ type) column. After elution with 2 mol/L hydrochloric acid for several times, the scandium in ion exchange resin was eluted and enriched with 5 mol/L hydrochloric acid. The solution was evaporated to dryness by heating. Then, the perchloric acid was added and the solution was heated to dryness. The residue was dissolved with 10 mol/L of hydrogen peroxide and 6 mol/L of hydrochloric acid followed by drying, respectively. The residue was dissolved with 2 mol/L hydrochloric acid and the solution was transferred into separating funnel. The sulfosalicylic acid and bromocresol green was added successively. Then, the solution was adjusted with ammonia water and hydrochloric acid to yellow. The chlorophosphonazo-PN (CPA-PN) was added for coloring and reacting with scandium to form α complex, which was then extracted with 20 mL of 0.02 mol/L 1-phenyl-3-methyl-4- benzoyl-5-pyrazolone (PMBP-benzene). The absorbance was measured on spectrophotometer at 680 nm. The content of scandium could be obtained from the calibration curve. Therefore, the determination method of scandium in red mud by spectrophotometry after separation with ion exchange resin was established. The results showed that the mass concentration of scandium in solution in range of 0.01-0.48 μg/mL was linear to the absorbance. The linear correlation coefficient of calibration curve was r=0.998 9. The apparent molar absorptivity was 3.86×104 L·mol-1·cm-1. The detection limit of scandium in this method was 0.42 μg/g. The interference tests indicated that for 5.0 μg of Sc (III) in solution, the tolerant amount of co-existing ions was defined as resulting in error of no more than ±5 %, and was listed as following (in fold): BO33- (600), NH4 (I) (200), Ca (II) (100), RE2O3 (60), Be (II) (30), Fe (III)(25), Al (III)(25), Mn (II) (25), Zr (IV) (4), Ti (IV)(2), Ta (V) (2). The content of scandium in actual red mud sample was determined according to the experimental method. The relative standard deviations (RSD, n=6) were between 2.5% and 3.9%. The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry.
林筑, 孔凡军, 郑美娟, 何锦林. 离子交换树脂分离-分光光度法测定赤泥中钪[J]. 冶金分析, 2016, 36(8): 73-77.
LIN Zhu, KONG Fan-jun, ZHENG Mei-juan, HE Jin-lin. Determination of scandium in red mud by spectrophotometry after separation with ion exchange resin. , 2016, 36(8): 73-77.
廖春发,卢惠明,邱定蕃,等.从赤泥中综合回收有价金属工艺的研究进展[J].轻金属,2003,15(10):18-22.LIAO Chun-fa,LU Hui-ming,QIU Ding-fan,et al.Recovering valuable metals from red mud generation during alumina production[J].Light Metals,2003,15(10):18-22.
[2]
朱军,兰建凯.赤泥的综合回收与利用[J].矿产保护与利用,2008,12(2):52-54.ZHU Jun,LAN Jian-kai.Comprehensive recovery and utilization of red mud[J].Conservation and Utilization of Mineral Resources,2008,12(2):52-54.
[3]
唐晓宁,陈肖虎,薛安.赤泥中钪的浸出动力学研究[J].湿法冶金,2010,29(3):155-158.TANG Xiao-ning,CHEN Xiao-hu,XUE An.Research on leaching kinetics of scandium from red mud[J].Hydrometallurgy of China,2010,29(3):155-158.
[4]
Yatsenko S P,Pyagai I N.Red mud pulp carbonization with scandium extraction during alumina production[J].Theoretical Foundations of Chemical Engineering,2010,44(4):563-568.
[5]
王克勤,于永波,王浩,等.从赤泥中提取钪的工艺现状[J].轻金属,2008,3(10):16-19.WANG Ke-qin,YU Yong-bo,WANG Hao,et al.Current situation of recovering scandium from red mud[J].Light Metals,2008,3(10):16-19.
[6]
姚宁.钪的提取及应用[J].黎明化工,1990,10(8):27-30.
[7]
魏正贵,李德谦,王春,等.HBTMPTP与Cyanex 925协同萃取Sc(Ⅲ)的研究[J].高等学校化学学报,1997,18(8):1281-1285.WEI Zheng-gui,LI De-qian,WANG Chun.Studies on synergistic extraction of Sc(Ⅲ)with HBTMPTP and cyanex 925[J].Chemical Research in Chinese Universities,1997,18(8):1281-1285.
[8]
王喜全.用P204作萃取剂分离富集钪[J].辽宁化工,1998,27(6):320-322.WANG Xi-quan.The separation and enrichment of Sc by P204 solvent extraction[J].Liaoning Chemical Industry,1998,27(6):320-322.
[9]
孙静,李德谦,叶伟贞.异丙基膦酸单(1-已基-4-乙基)辛酯从硫酸介质中萃取分离钪、铁和镥[J].中国稀土学报(Journal of the Chinese Rare Earth Society),1994,12(4):298-302.
[10]
傅玉琴,周移,李龙泉.PMBP萃淋树脂分离钪中微量锆[J].化学试剂,1999,21(1):44-46.FU Yu-qin,ZHOU Yi,LI Long-quan.Separating microamounts of zirconium from scandium with levextrel resin PMBP[J].Chemical Reagents,1999,21(1):44-46.
卢业玉,罗宗铭,刘铠霞.钪(Ⅲ)-乳酸-埃络青R-溴化十六烷基三甲基铵的显色反应及其应用[J].理化检验:化学分册,2002,38(10):497-499.LU Ye-yu,LUO Zong-ming,LIU Kai-xia.Study on the mixed micellar ligand color reaction of scandium(Ⅲ)with eriochrome cyanine R and lactic acid in the presencn of ctmab and its application[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2002,38(10):497-499.
[13]
林维明,张培兴.甲基百里酚蓝光度法测定高温氯化收尘渣中钪[J].分析试验室(Chinese Journal of Analysis Laboratory),1986 (11):56-59.
[14]
余荣旻,杨涛,邓志军,等.铬天青S光度法测定赤泥-钛白废水综合回收中的微量钪[J].冶金分析,2015,35(1):63-67.YU Rong-min,YANG Tao,DENG Zhi-jun,et al.Determination of micro scandium in the comprehensive recovery of red mud-titanium dioxide wastewater by chromeszurol S spectrophotometry[J].Metallurgical Analysis,2015,35(1):63-67.
[15]
周锦帆,王慧,吴骋,等.离子交换分离的试验技巧及研究方法[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis).2010,46(8):960-964.
[16]
于永波.赤泥浸出萃取钪的工艺研究[D].山西:太原理工大学,2009.
[17]
王秋泉,杨利民,彭春霖.PMBP 萃取色谱法分离钪和镧系元素及钇的研究[J].沈阳化工学院学报(Journal of Shenyang Institute of Chemical Technology),1991,3(5):159-167.