Raw material decomposition

The purpose of the decomposition of raw materials is to convert tantalum and niobium compounds into a soluble form and prepare the solution for use in subsequent procedures. Fig. 116 presents the process flow chart. The most typical and frequently used raw materials are columbite-tantalite concentrates with the general formula (Fe, Mn)(Nb, Ta)206. 

Two types of digestion solutions are usually used for the chemical decomposition of the raw material hydrofluoric acid, HF, or a mixture of hydrofluoric and sulfuric acids, HF and H2SO4 [32]. The process is performed using solutions with relatively high acid concentrations, at elevated temperatures and under intensive stirring for several hours to ensure effective digestion. The raw material is nearly completely dissolved. 

A residual phase, usually consisting of insoluble fluorides and oxyfluorides of alkali earth and rare earth metals, is separated from the solution by filtration. The mechanism of the chemical decomposition of raw materials of the tantalum- and niobium-containing oxide type seems to be complicated, and unfortunately, the process has yet to be adequately investigated. 

It was proposed [445 - 447] that the dissolution of tantalum and niobium oxides in mixtures of hydrofluoric and sulfuric acids takes place through the formation of fluoride-sulfate complexes, at least during the initial steps of the interaction and at relatively low acid concentrations. Nevertheless, it was also assumed that both tantalum and niobium fluoride-sulfate complexes are prone to hydrolysis yielding pure fluoride complexes and sulfuric acid. No data was provided, however, to confirm the formation of fluoride sulfate complexes of tantalum and niobium in the solutions. 

Nevertheless, Ta5+ and Nb5+ interact with aqueous media containing fluorine ions, such as solutions of hydrofluoric acid. On the other hand, as was clearly shown by Majima et al. [448 - 450], the increased hydrogen ion activity can also significantly enhance the dissolution rate of oxides. The activity of hydrogen ions can be increased by the addition of mineral salts or mineral acids to the solution. 

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Another method of raw material decomposition is based on the fluorination of the raw material by the hydrofluoride method. No published data exists on hydrofluoride decomposition of columbite or tantalite concentrates. The interaction can, nevertheless, be discussed based on available information on the decomposition of lithium tantalate, LiTaC>3, and lithium niobate, LiNb03, using the hydrofluoride method [113,118,122]. 

In general, the process flow chart of raw material decomposition by the hydrofluoride method can be represented as shown in Fig. 117. 

The main advantages of the method can be formulated as follows. First, hydrofluoric acid is not needed for the decomposition stage the amount of fluorine required for the raw material decomposition can be calculated and adjusted as closely as possible to the stoichiometry of the interaction. Since the leaching of the fluorinated material is performed with water, a significant fraction of the impurities are precipitated in the form of insoluble compounds that can be separated from the solution, hence the filtrated solution is essentially purified. There is no doubt that solutions prepared in this way can be of consistent concentrations of tantalum and niobium, independent of the initial raw material composition. 

Nevertheless, current processes of raw material decomposition that are based on digestion of the material by highly concentrated hydrofluoric and sulfuric acids yield highly acidic solutions. 

The unique advantage of the plasma chemical method is the ability to collect the condensate, which can be used for raw material decomposition or even liquid-liquid extraction processes. The condensate consists of a hydrofluoric acid solution, the concentration of which can be adjusted by controlling the heat exchanger temperature according to a binary diagram of the HF - H20 system [534]. For instance, at a temperature of 80-100°C, the condensate composition corresponds to a 30-33% wt. HF solution. 

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