Sulfur Tantalite

Akimov and Chernyak [452] investigated and reported on the mechanism of the interaction between columbite and tantalite and sulfuric acid. The said interaction is presented as comprising two steps. The first step is related to the formation of iron and manganese sulfates and of tantalum and niobium hydroxides ... 

The results of a thermodynamic analysis of the interactions in Equations (127) and (128), as presented in [452], show that a coherent shell of tantalum and niobium hydroxides is formed on the surface of the columbite or tantalite during the interaction with sulfuric acid. The formation of the shell drives the process towards a forced thermodynamic equilibrium between the initial components and the products of the interaction, making any further interaction thermodynamically disadvantageous. It was also shown that, from a thermodynamic standpoint, the formation of a pseudomorphic structure on the surface of columbite or tantalite components is preferable to the formation of tantalum and niobium oxysulfates. Hence, the formation of the pseudomorphic phases catalyzes the interaction described by Equation (127) while halting that described by Equation (128). 

This approach explains the experimental fact that the complete decomposition of columbite or tantalite by sulfuric acid yields hydroxides of tantalum and niobium according to the first step of Equation (127). 

Analysis of the volumetric effects indicates that as a result of such mechanical activation, iron and manganese are concentrated in the extended part of the crystal, while tantalum and niobium are predominantly collected in the compressed part of the distorted crystal structure. It is interesting to note that this effect is more pronounced in the case of tantalite than it is for columbite, due to the higher rigidity of the former. Akimov and Chernyak [452] concluded that the effect of redistribution of the ions might cause the selective predominant dissolution of iron and manganese during the interaction with sulfuric acid and other acids. 

The digestion of columbite, tantalite and other raw materials containing tantalum and niobium using both hydrofluoric acid and a mixture of hydrofluoric and sulfuric acids is widely applied in the industiy. The main advantage of the method is its simplicity. The method has, nevertheless, several disadvantages that should be noted, as follows. 

An initial solution was prepared by the hydrofluoride method, i.e. melting of a mixture of ammonium hydrofluoride and tantalite, followed by the digestion of soluble components with water and separation of the solution by filtration. The prepared initial solution contained no free HF or any other acid, and had a pH 3. In order to obtain an optimal acidity level, sulfuric acid was added to the solution. Concentrations of Ta2Os (50-60 g/1) and Nb205 ( 30 g/1) were kept approximately constant during the preparation of the solutions. Extraction was performed using a polypropylene beaker and a magnetic stirrer. 

Carlson and Nielsen (C3) described the pilot and full-scale plant separation of an ore containing more than 30% combined columbium and tantalum oxide using a sulfuric-hydrofluoric acid leach and methyl isobutyl ketone (MIBK) as solvent in pulsed columns. The —200 mesh columbite-tantalite ore was digested with 70% HF until the combined (Ca + Ta)20s in the leach liquid reached 3 Ib/gal at which time it was diluted to 15N free acid and clarified by filtration. This solution was contacted countercurrently in the pulsed column where Ta and Cb were extracted by MIBK. Columbium was stripped from the organic with demineralized water which diluted the free acid in the solvent, making possible the transfer of all the Cb the Ta-loaded solvent was then stripped with demineralized water causing the transfer of Ta to the aqueous phase. The oxides were then precipitated with 28% ammonium hydroxide solution. Conversion to the respective oxides was by calcination of the precipitates. 

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