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filingDate 1956-02-29-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationDate 1959-12-16-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-825604-A
titleOfInvention Process for extracting and separating niobium and tantalum
abstract Niobium oxychloride and tantalum pentachloride are separated by extraction with an inert solvent in the absence of water. The initial mixture is prepared by converting an oxide material such as an ore, concentrate, slag or mixture of oxides with chlorine and a reducing agent, to a mixture containing niobium at least to a major extent as oxychloride and tantalum at least to a major extent as pentachloride. The chlorination may be performed at 400-1000 DEG C. in a shaft or horizontal tube furnace, and it is necessary in order to prevent reaction of the resultant vapours with the waste chlorination gases, to permit contact therebetween for at most a few seconds, e.g. by diluting with chlorine-freed spent reaction gas or by providing a conduit which is very short or of very small cross-section, between the chlorinator and the condenser. Other elements which may be present in the oxide material and which are chlorinated are titanium, tin, manganese and silicon: these may be separated at different temperatures. In the selective solution of the chloride-oxychloride mixture, solvents referred to are aliphatic and aromatic compounds, preferably halogenated and containing up to three carbon atoms, e.g. bromoethane, chlorethane and carbon tetrachloride: titanium tetrachloride, silicon tetrachloride, tin tetrachloride, phosphorous trichloride, carbonyl chloride, thionyl chloride, sulfuryl chloride and liquid sulphur dioxide. A mixture of solvents may be used. The dissolution may be effected under atmospheric or superatmospheric pressure and at room or raised temperature, e.g. the boiling point of the solvent employed, and may be performed in a grinding apparatus or continuously in a counter-current method. After separation of the solution from the residue the tantalum pentachloride may be obtained by distilling off the solvent or by cooling and crystallization. Both the soluble and the residual substances may be purified by sublimation. Examples illustrate the chlorination of briquettes of sugar charcoal, niobium and tantalum pentoxides at 550-600 DEG C. or at 1000 DEG C. followed by precipitation of the chlorides in an air-cooled condenser, pulverization and multiple extraction. In some of the examples, the insoluble portion (mainly niobium) may be sublimed in vacuo to give a residue rich in tantalum and a sublimate rich in niobium. French Specification 973,896 and U.S.A. Specifications 2,537,316, 2,481,584, 2,443,254 and 2,427,360 are referred to in connection with the prior art.
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