用配合还原反萃取法从P204有机相中去除Fe(Ⅲ)
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摘要
P204萃取剂对Fe~(3+)选择性高,生成的萃合物稳定,但有机相中的Fe~(3+)难以反萃取。研究了采用配合还原反萃取法从P204有机相中反萃取Fe~(3+),考察了几种配合离子及还原剂对Fe~(3+)反萃取的影响。强酸性条件下,Cl-易与Fe~(3+)配位形成FeCl_4~-,硫代硫酸钠对Fe~(3+)的反萃取有明显促进作用,因此,探索了以盐酸为配合剂,硫代硫酸钠为还原剂,通过还原反萃取从P204有机相中去除Fe~(3+)。试验结果表明:在常温、相比Vo/Va=3/1、盐酸浓度5 mol/L、一次振荡时间4 min、硫代硫酸钠加入量为理论量的4倍、二次间歇振荡12min条件下,Fe~(3+)反萃取率达88.6%。该方法可有效去除P204有机相中的Fe~(3+),使有机相得到净化。
P204 can high selectivity extract Fe~(3+) in solution,so the extraction complex is difficult to be stripped.The stripping Fe~(3+) from P204 by the process of complexation and reducing was investigated.The effects of several complexation ions and reducing agents on stripping of Fe~(3+) in the P204 organic phase were examined.Under the conditions of high acid concentration,Cl-complexes Fe~(3+)to form FeCl_4~-.The sodium thiosulfate is good reduction agent for stripping the Fe~(3+) in the P204.The influences of some factors on stripping of Fe~(3+)from the P204 organic phase were examined.The results show that under the conditions of room temperature,Vo/Vaof 3/1,hydrochloric acid concentration of 5 mol/L,once oscillation time of 4 minutes,the 4 times theoretical amount of sodium thiosulfate and second intermittent oscillation time of 12 minutes,the stripping rate of Fe~(3+) can reach88.6%.Fe~(3+)can effectively be removed from the P204 by the method.
P204 can high selectivity extract Fe~(3+) in solution,so the extraction complex is difficult to be stripped.The stripping Fe~(3+) from P204 by the process of complexation and reducing was investigated.The effects of several complexation ions and reducing agents on stripping of Fe~(3+) in the P204 organic phase were examined.Under the conditions of high acid concentration,Cl-complexes Fe~(3+)to form FeCl_4~-.The sodium thiosulfate is good reduction agent for stripping the Fe~(3+) in the P204.The influences of some factors on stripping of Fe~(3+)from the P204 organic phase were examined.The results show that under the conditions of room temperature,Vo/Vaof 3/1,hydrochloric acid concentration of 5 mol/L,once oscillation time of 4 minutes,the 4 times theoretical amount of sodium thiosulfate and second intermittent oscillation time of 12 minutes,the stripping rate of Fe~(3+) can reach88.6%.Fe~(3+)can effectively be removed from the P204 by the method.
引文
[1]刘会州,于淑秋,陈家镛.P204-正辛烷萃取和反萃取Fe(Ⅲ)机理的研究[J].化工学报,1991,42(3):283-287.
[2]杨合,荣宜,薛向欣,等.包头稀土尾矿回收铁的直接还原研究[J].中国稀土学报,2012,30(4):470-475.
[3]李华昌,符斌.实用化学手册[M].北京:化学工业出版社,2007.
[4]金鑫,汪庭语,赵松,等.二-(2-乙基己基)磷酸萃取剂中铁离子的洗脱与萃取剂的再生[J].湿法冶金,2012,31(6):396-398.
[5]肖纯,唐谟堂,杨声海,等.用铁粉和稀硫酸还原反萃取P204中Fe3+[J].中南大学学报(自然科学版),2007,38(4):663-668.
[6]LAN Qiaofa,HUANG Zhenhua,XIE Fanghao,et al.Removal of Fe(Ⅲ)from P507-N235System by Complexing Method[J].Journal of Chinese Society of Rare Earths,2015,33(2):188-195.
[7]邓志敢,魏昶,李雯廷,等.石煤氧压酸浸液萃钒除铁工艺研究[J].稀有金属,2009,33(2):290-294.
[8]郁强,滕藤,於静芬.界面化学反应控制的萃取动力学研究[J].有色金属(冶炼部分),1981(5):29-36.
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[10]吴瑾光,陈滇,高宏成,等.酸性磷萃取剂在皂化过程中的结构变化与萃合物的组成[J].高等学校化学学报,1980,1(2):14-221.
[11]冯雪茹,吕国志,张廷安,等.P204萃取硫酸体系中的V(Ⅳ)、Fe(Ⅲ)的分离性能研究[J].钢铁钒钛,2017,38(2):23-29.
[12]张廷安,牟望重,豆志河,等.转炉钒渣氧压酸浸过程V-FeH2O系的电位—pH图[J].中国有色金属学报,2011,21(11):2936-2945.
[13]SINGH D K,MISHRA S L,SING H.Stripping of iron(Ⅲ)From the D2EHPA+TBP extract produced during uraniun recovery from phosphoric acid by oxalic acid[J].Hydrometallurgy,2006,81(3/4):214-218.
[14]NISHIHAMA S,HIRAI T,KOMASAWA I.Mechanism of photoreductive stripping of iron(Ⅲ)in a liquid-liquid extraction system and its application for a hydrometallurgical process[J].Industrial&Engineering Chemistry Research,1999,38(10):4850-4856.
[15]张雪梅,汪徐春,邓军,等.草酸配合除石英砂中铁的研究[J].硅酸盐通报,2012,31(4):852-860.
[16]印春生,赵巍,杨兴华,等.影响镧系金属离子的结构参数与配合物稳定常数的关系研究[J].湘潭大学自然科学学报,2001,23(1):44-48.
[17]马涌,路殿坤,金哲男,等.P204萃取含铜酸性废水中铁的研究[J].有色矿冶,2010,26(2):24-27.
[18]王洪星.P204对Sc3+、Fe3+和Al 3+萃取过程的基础研究[J].科技展望,2016,26(14):84.
[2]杨合,荣宜,薛向欣,等.包头稀土尾矿回收铁的直接还原研究[J].中国稀土学报,2012,30(4):470-475.
[3]李华昌,符斌.实用化学手册[M].北京:化学工业出版社,2007.
[4]金鑫,汪庭语,赵松,等.二-(2-乙基己基)磷酸萃取剂中铁离子的洗脱与萃取剂的再生[J].湿法冶金,2012,31(6):396-398.
[5]肖纯,唐谟堂,杨声海,等.用铁粉和稀硫酸还原反萃取P204中Fe3+[J].中南大学学报(自然科学版),2007,38(4):663-668.
[6]LAN Qiaofa,HUANG Zhenhua,XIE Fanghao,et al.Removal of Fe(Ⅲ)from P507-N235System by Complexing Method[J].Journal of Chinese Society of Rare Earths,2015,33(2):188-195.
[7]邓志敢,魏昶,李雯廷,等.石煤氧压酸浸液萃钒除铁工艺研究[J].稀有金属,2009,33(2):290-294.
[8]郁强,滕藤,於静芬.界面化学反应控制的萃取动力学研究[J].有色金属(冶炼部分),1981(5):29-36.
[9]傅洵,傅有君.P538与P204从盐酸介质中萃取Fe(Ⅲ)[J].应用化学,1991,8(4):43-47.
[10]吴瑾光,陈滇,高宏成,等.酸性磷萃取剂在皂化过程中的结构变化与萃合物的组成[J].高等学校化学学报,1980,1(2):14-221.
[11]冯雪茹,吕国志,张廷安,等.P204萃取硫酸体系中的V(Ⅳ)、Fe(Ⅲ)的分离性能研究[J].钢铁钒钛,2017,38(2):23-29.
[12]张廷安,牟望重,豆志河,等.转炉钒渣氧压酸浸过程V-FeH2O系的电位—pH图[J].中国有色金属学报,2011,21(11):2936-2945.
[13]SINGH D K,MISHRA S L,SING H.Stripping of iron(Ⅲ)From the D2EHPA+TBP extract produced during uraniun recovery from phosphoric acid by oxalic acid[J].Hydrometallurgy,2006,81(3/4):214-218.
[14]NISHIHAMA S,HIRAI T,KOMASAWA I.Mechanism of photoreductive stripping of iron(Ⅲ)in a liquid-liquid extraction system and its application for a hydrometallurgical process[J].Industrial&Engineering Chemistry Research,1999,38(10):4850-4856.
[15]张雪梅,汪徐春,邓军,等.草酸配合除石英砂中铁的研究[J].硅酸盐通报,2012,31(4):852-860.
[16]印春生,赵巍,杨兴华,等.影响镧系金属离子的结构参数与配合物稳定常数的关系研究[J].湘潭大学自然科学学报,2001,23(1):44-48.
[17]马涌,路殿坤,金哲男,等.P204萃取含铜酸性废水中铁的研究[J].有色矿冶,2010,26(2):24-27.
[18]王洪星.P204对Sc3+、Fe3+和Al 3+萃取过程的基础研究[J].科技展望,2016,26(14):84.