FIELD: technological processes.
SUBSTANCE: invention relates to a process for the preparation of tin (II) carboxylates by reacting a metal, its dioxide and a carboxylic acid in the presence of an organic solvent and a stimulating iodine additive in a vertical bead mill with a glass bead as a milling agent, where at the beginning the reactor is loaded with a wiping agent in a weight ratio with the remaining charge of 1:1, a liquid phase solvent and an acid in an amount of 1.68 mol/kg, include mechanical stirring and a slurry of acid is prepared, then 0.4 mol/kg of tin dioxide is introduced and, in some cases, 10-2 mol/kg p-aminoazobenzene as a tribochemical catalyst, and with the current control of the consumption of the acid, a tin (IV) salt and an introduced acid are obtained, 10 % of the rest of the metal charge and 0.05 mol/kg of molecular iodine are introduced, and the desired carboxylate is obtained by monitoring the accumulation of tin (II) compounds, and then the mechanical stirring is stopped, the grinding agent and the unreacted metal are extracted from the product slurry separated by subsequent filtration, washing the precipitate with a liquid phase solvent, drying it and purification by recrystallization. As an acid, benzoic, salicylic, p-oxybenzoic, anthranilic, p-aminobenzoic, o-chlorobenzoic, m-nitrobenzoic, 5-aminosalicylic, gallic, p-nitrobenzoic, anisic, acetic, propionic, trichloroacetic, benzene propionic are used.
EFFECT: method makes it possible to obtain the product in high yield.
4 cl, 4 tbl, 18 ex
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Authors
Dates
2018-10-30—Published
2017-11-15—Filed