从氧氯化锆母液中分离制备氧化锆的研究

采用有机协同萃取剂将氧氯化锆母液中的锆萃取到有机相中得到含锆萃取物, 锆萃取物经洗涤、反萃、氨沉和灼烧得到核能级氧化锆产品。试验结果表明:当料液中游离酸酸度为5 mol/L, 有机相组成为20%TOPO+10%Cynex272+70%磺化煤油, 萃取相比为2〖DK〗∶1时, 锆铪分离效果较好, 锆萃取率达到98.68%;有机相洗涤试验中铪反洗率为97.33%, 锆损耗率仅1.25%;盐酸酸度为0.5 mol/L时, 锆反萃效果较佳, 达到98.90%。最终制得的氧化锆产品纯度达到99.90%, 铪含量仅为0.0030%。

Separation and Preparation of Zirconium Oxide from Mother Liquor Containing Zirconium Oxychloride

Zirconium-bearing extract was obtained by extracting Zr from the mother liquor containing zirconium oxychloride into an organic phase using organic synergistic extractant. Nuclear grade zirconium oxide was obtained after washing, re-extraction, ammonia precipitation and ignition of the extracts. The test results showed, with free acidity at 5 mol/L, organic phase composed of 20%TOPO+10%Cynex272+70% sulfonated kerosene and O/A rate of 2〖DK〗∶1, the best Zr-Hf separation result was obtained with Zr extraction rate of 98.68%. And the experiment of organic phase washing resulted in the backwashing rate of hafnium at 97.33% and the loss rate of zirconium just at 1.25%. With hydrochloric acid acidity of 0.5 mol/L, the best Zr re-extraction effect could be obtained, reaching 98.90%. The final product of zirconium oxide has 99.90% purity, with hafnium content of only 0.0030%.