Separation of niobium and tantalum using continuous multistage counter-current solvent extraction with trioctyl amine

Abstract

Niobium and tantalum are valued for their uses in nuclear, steel, aviation and electronics industries. This paper elucidates the development of a multistage counter-current separation process for obtaining pure niobium and tantalum from the hydrofluoric acid solution of Coumbite-Tantalite ore (leach liquor), with trioctyl amine (TOA) as the extractant solvent. Contrary to the conventionally used multistage process this novel route does not use any other acid in addition to hydrofluoric acid, resulting in the elimination of the generation of mixed fluoride waste. Reaction equilibrium constants for the reactions involving the extraction of hydrofluoric acid, niobium and tantalum have been determined and were used to generate equilibrium distribution curve of niobium and tantalum in the organic and aqueous phase. The number of counter-current stages required for an appropriate organic to aqueous phase volume (O/A) ratio was determined using McCabe-Thiele calculations. Selective extraction of 99% of tantalum from the leach liquor was achieved using 5 v/v% TOA and two counter-current stages for an O/A ratio of four. The tantalum lean raffinate was treated with commercial grade hydrofluoric acid to form the niobium feed solution having 16 M free acidity. Near complete extraction of niobium was achieved using a three stage counter-current process with O/A ratio of two and 10 v/v% TOA as the organic extractant. The calculations for the stage-wise variation of concentrations were validated by batch experimental simulation of counter-current processes.