FIELD: technological processes.
SUBSTANCE: invention relates to a simple process for the preparation of tin (II) carboxylates by reacting a metal with an oxidant in the presence of a stimulating iodine additive in a vertical bead mill in a white spirit with a glass bead as a grinding agent in a weight ratio with a charge (without metal) of 1:1. In this case, the appropriate tin (IV) carboxylate in the amount of 0.15–0.50 mol/kg in the molar ratio with tin 1:(1.4÷2.0), which is 3.56–8.31 % of the mass of the rest of the load. Iodine is dosed in an amount of 0.03÷0.05 mol/kg. As an additional stimulating additive, an acid with an anion of tin (IV) carboxylate in an amount of 0.01÷0.05 mol/kg. Loading is carried out in sequence: glass beads, solvent, molecular iodine, carboxylic acid, then metal. Process starts with stirring and is carried out at room temperature in the absence of external heat input and (or) forced cooling of the reaction mixture while monitoring the accumulation of tin (II) compounds until the oxidant is almost completely consumed. Upon reaching this point, the process is stopped, the product suspension is separated from the grinding agent and the excess metal, then it is filtered, the filter cake is washed from the excess acid with a small amount of a solvent, well wring out, remove from the filter and dry or direct to additional purification by recrystallization. Following tin (IV) carboxylates are used as the oxidizing agent: formate, propionate, benzoate, anthranilate, salicylate, 5-aminosalicylate, p-aminobenzoate, p-oxybenzoate, p-nitrobenzoate, phenylanthranilate, gallate, 3-methoxy-4-oxycinnamic or hydrocinnamic acid normal salt, m-nitrobenzoate, acetylsalicylate, o-nitrobenzoate chlorobenzoate, or stearate.
EFFECT: simple process for the preparation of tin (II) carboxylates is provided.
3 cl, 3 tbl, 27 ex
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Authors
Dates
2018-10-19—Published
2017-11-15—Filed