用磷酸三丁酯从硝酸体系中萃取分离锆铪试验研究Separation of Zirconium and Hafnium From Nitric Acid Solution by Solvent Extraction Using Tributyl Phosphate
李大炳;赵凤岐;支梅峰;周志全;张永明;舒祖骏;
摘要(Abstract):
以含铪的氯化锆酰工业产品为原料,经水溶、碱沉、洗涤、硝酸溶解等工序制备ρ(Zr(Hf))为7580g/L的硝酸锆(铪)酰溶液;再以φ(TBP)=40%的煤油溶液萃取锆,含锆有机相经硝酸锆酰溶液洗涤除铪、水反萃取后,得到硝酸锆酰溶液;硝酸锆酰溶液经氨水沉淀,沉淀物经干燥、煅烧得到ZrO2粉末,其ZrO2纯度达99.5%,铪质量分数<1.0×10-5,产品质量优于原子能级二氧化锆标准(铪质量分数<1.0×10-4);萃取锆后的萃余水相中,铪占锆、铪总质量的96.7%,满足原子能级铪对杂质锆的要求。
关键词(KeyWords): 锆;铪;分离;TBP;溶剂萃取
基金项目(Foundation):
作者(Authors): 李大炳;赵凤岐;支梅峰;周志全;张永明;舒祖骏;
DOI: 10.13355/j.cnki.sfyj.2016.06.012
参考文献(References):
- [1]张力.锆铪分离的湿法工艺比较及分析[J].稀有金属快报,2007,26(1):115-119.
- [2]张平伟.溶剂萃取分离锆铪[J].稀有金属,1992,16(4):286-292.
- [3]徐欣,杨新伟,邬元旭,等.P507萃取锆和铪及分离性能[J].稀有金属,2008,32(3):355-359.
- [4]TAGHIZADEH M,GHASEMZADEH R.Determination of optimum process conditions for the extraction and separation of zirconium and hafnium by solvent extraction[J].Hydrometallurgy,2008,90(2/3/4):115-120.
- [5]邬安华.法国原予能级锆冶炼新方法[J].稀有金属,1991,15(5):385-387.
- [6]林振汉.用甲基异丁基酮萃取分离锆铪的工艺评价[J].稀有金属快报,2007,26(4):93-96.
- [7]BISWAS R K,HAYAT M A.Solvent extraction of zirconium(Ⅳ)from chloride media by D2EHPA in kerosene[J].Hydrometallurgy,2002,63(2):149-158.
- [8]WANG Qiuquan,TSUNODA K I,AKAIWA H.Separation of zirconium(Ⅳ)and hafnium(Ⅳ)by extraction chromatography using di(1-methylheptyl)methyiphosphonate as a stationary phase[J].Analytical Sciences,1997,13(1):27-31.
- [9]吕标起,徐志高,张力,等.MIBK-HSCN体系萃取分离锆铪影响因素的研究[J].稀有金属,2008,32(6):754-757.
- [10]侯嵩寿,尤曙彤,张平伟,等.改进的N235-H2SO4流程萃取分离锆铪制取原子能级氧化锆[J].稀有金属,1991,15(6):405-409.
- [11]林振汉.用TBP萃取分离锆和铪的工艺研究[J].稀有金属快报,2004,23(11):21-25.
- [12]蒋竹筠.混合酸系统磷酸三丁酯萃取分离锆铪[J].稀有金属与硬质合金,1996(6):55-61.
- [13]杨传芳,洪滨,陈家镛.磷酸三丁酯-煤油从浓酸溶液中萃取Zr的第三相行为[J].化学与粘合,1995(2):66-69.