FIELD: inorganic synthesis.
SUBSTANCE: invention relates to preparation of niobium and/or tantalum pentachlorides from niobium and/or tantalum oxides and/or oxychlorides and comprises reaction of oxide or oxychloride compounds with chlorination agent, namely double aluminum chloride-phosphorus pentachloride compound AlCl3·PCl5. Process is carried out at 100 to 400° C. Exhausted chlorination agent is then regenerated by chlorinating it in presence of sulfur at 500-600° C or in presence of carbon at 800-900° C. After chlorination of oxide or oxychloride compounds with AlCl3·PCl5 chlorination is continued using AlCl3·POCl5. In another embodiment of invention, chlorination is accomplished using, as chlorination agent, melts based on formulations similar to eutectics formed by AlCl3·PCl5 or AlCl3·POCl5 and sodium and/or potassium chloroaluminates or chloroferrates. Resulting niobium and/or tantalum pentachlorides are recovered from reaction mixture via rectification.
EFFECT: achieved environmental safety of reactants and reaction products and fullness of chlorination, lowered temperature, accelerated process, and reduced expenses.
6 cl, 5 ex
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Authors
Dates
2005-06-10—Published
2004-05-18—Filed