Preparation of Bismuthyl (III) Fumarate Microspheres from Chloric Acid Solutions
K. V. MISHCHENKO, E. E. LUNEVA, YU. M. YUKHIN
Institute of Solid State Chemistry and Mechanochemistry, Siberian Branch of the Russian Academy of Sciences, Novosibirsk, Russia
Keywords: bismuthyl (III) fumarate, microspheres, oxide, hydrochloric solutions, precipitation
Pages: 79-85
Abstract
The spherical microstructures of bismuthyl (III) fumarate with the composition (BiO)2С4H2O4 were obtained using the standard method of precipitation from solutions at 23 and 60 ºС. The composition of the reaction product and its properties were studied using a complex of physicochemical methods. At 60 oC, the degree of bismuth precipitation in the product is not less than 99.8 % for the molar ratio of bismuth to fumarate ion equal to 1.5. According to IR and Raman spectroscopy data, both acidic residues of fumaric acid are deprotonated in the resulting compound, while the carboxylic groups have bidentate coordination to bismuthyl cation. The effect of temperature on the morphology of obtained compounds was studied by scanning electron microscopy and small-angle laser light scattering. According to scanning electron microscopy data, (BiO)2С4H2O4 obtained at 23 ºC is composed of spherical particles about 10-12 µm in size, consisting of thin nanoplates about 0.1 μm thick. The data of sedimentation analysis of the powder indicate a symmetric particle size distribution with the average particle size equal to 11.7 μm. With an increase in precipitation temperature to 60 oC, particle size decreases to 3-7 µm; an asymmetric function of particle size distribution is observed, and the average size of the aggregates is 30.9 µm. A possible mechanism for the formation of (BiO)2С4H2O4 spherical microstructures is described as a process combining Ostwald ripening and self-assembling. According to the data of thermal and XRD analyses, the product of thermal decomposition of bismuthyl fumarate at a temperature of 450 ºC is a monoclinic modification of Bi2O3.
DOI: 10.15372/CSD2021280
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