Solid-Liquid Reactions in the Synthesis of High-Purity Bismuth Compounds
Y. M. YUKHIN1, E. S. KOLEDOVA1, A. S. DAMINOV2, K. V. MISHCHENKO1, L. I. AFONINA1, E. V. TIMAKOVA1, O. A. LOGUTENKO1
1Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk, Russia
2LLC Rare Metals Plant, Novosibirsk Region, Russia
Keywords: металлический висмут, оксид, азотнокислые растворы, гидролитическая очистка, оксогидроксонитрат висмута, обработка растворами кислот, соединения висмута, metal bismuth, oxide, nitrate solutions, hydrolytic purification, bismuth oxohydroxonitrate, treatment with acid solutions, bismuth compounds
Pages: 96-104
Abstract
Processing of the nitric solutions from the production of bismuth compounds by adding water was studied by means of X-ray phase and chemical analyses, and electron microscopy. It is shown that bismuth gets precipitated from solutions at the process temperature of 65±5 °C and pH 0.7-1.0 in the form of oxohydroxonitrate [Bi6O4(OH)4](NO3)6•H2O, and washing with water causes hydrolysis with the formation of high-purity [Bi6O5(OH)3](NO3)5•3H2O compound. These compounds are used as precursors for obtaining high-purity bismuth compounds through a solid-liquid reaction. It is demonstrated that the treatment of bismuth oxohydroxonitrate with the solutions of citric, gallic, tartaric, salicylic, nitric acids and ammonium carbonate may result in obtaining bismuth citrate BiС6Н5О7, bismuth oxogallate trihydrate C6H2(OH)3COOBiO•3H2O, bismuth ditartrate trihydrate [Bi(C4H4O6)(C4H5O6)]•3H2O, bismuth oxide salicylate Bi(C7H5O3)O, bismuth nitrate pentahydrate Bi(NO3)3•5H2O, bismuth oxocarbonate (BiO)2CO3, respectively. The powders of metal bismuth with particle size 1-5 and 10-50 mm were obtained by the reduction of oxohydroxonitrates of the compositions [Bi6O4(OH)4](NO3)6•H2O and [Bi6O5(OH)3](NO3)5•3H2O, respectively, in the solution of benzyl alcohol. The reduction of these oxohydroxonitrates in ethylene glycol solution in the presence of hydrazine hydrate in the case of [Bi6O4(OH)4](NO3)6•H2O results in the formation of bismuth glycolate, while in the case of [Bi6O5(OH)3](NO3)5•3H2O - in the formation of metal bismuth with particle size 10-50 mm. The powders of metal bismuth with particle size 1-5 and 10-50 mm were obtained by means of the reduction of the compounds [Bi6O4(OH)4](NO3)6•H2O and [Bi6O5(OH)3](NO3)5•3H2O, respectively, in the aqueous medium with sodium borohydride as the reducing agent, with the molar ratio of bismuth/sodium borohydride = 1, pH 12 and a temperature of 25 °C.
DOI: 10.15372/CSD2020208
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