The method for extracting and separating Ta and Nb by using the solvent extaction system, hydrofluoric acid-sulphuric acid-tributyl phosphate (TBP), was investigated. The extractability of fluotantalates and fluoniobiates from HF-H
2SO
4 solution into TBP was found to be a function of HF acidity, H
2SO
4 acidity, TBP concentration, oxide concentration, organic solvent ratio, and number of extraction operation. The results obtained can be summarized as follows: (1) %Ta extracted and Ta distribution coefficient increased with an increase of H
2SO
4 acidity at constant HF acidity, but decreased with increasing HF acidity at constant H
2SO
4 acidity. They diminished with a decrease of TBP concentration. %Nb extracted and Nb distribution coefficient augmented with increasing HF acidity, H
2SO
4 acidity, and TBP concentration. (2) In general, the separation factor was superior in low HF acidity-low H
2SO
4 acidity, but inferior in high HF acidity-high H
2SO
4 acidity. It varied little by change in TBP concentration. (3) Both %Ta and %Nb extracted fell in opposition of rising oxide concentration in aqueous solution. (4) Augmenting solvent ratio and number of extraction operation caused increase of both %Ta and %Nb extracted. (5) The extract made with TBP included little impurity. (6) HF-H
2SO
4-TBP system had larger extraction efficiency of Ta and Nb, particulary in extracting Nb, and higher purity of organic extract than HF-H
2SO
4-Hexone system, which is used as the industrial extractive and separative system in liquid-liquid extraction of Ta and Nb at present.
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