FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing manganese (II) m-nitrobenzoate by reacting metal with acid in the presence of an oxidising agent, organic liquid phase and stimulating additive in a bead mill. The oxidising agent used is manganese peroxide taken in amount of 0.25-0.50 mol/(kg of the initial charge) and in molar ratio to metal equal to 1:1-1:3. The acid is taken in amount of (2.05÷2.15) where nMn and is content (mol/(kg of the initial charge)) of the metal and its peroxide in the initial charge. The main component of the liquid phase is isobutyl alcohol, ethylcellosolve, butylacetate, o-xylene or white spirit, i.e. solvent in which at least acid is partially dissolved and salt - the product, is least dissolved. Molecular iodine, potassium iodide, potassium bromide, calcium chloride or barium chloride are used a stimulating additive, taken in amount of 0.01-0.05 mol/(kg of the initial charge). Loading is done successively: glass beads, liquid phase solvent, m-nitrobenzoic acid, stimulating additive, metal and peroxide thereof. The process starts at room temperature and is carried out while cooling in the range of achieved maximum temperature of 35-53°C while controlling via a sampling method until virtually complete conversion of manganese peroxide and metal to salt, after which the process is stopped, the suspension of the reaction mixture is separated from the glass beads and filtered, the residue is washed with liquid phase on a filter, thoroughly pressed and taken for purification via recrystallisation, as well as the process filtrate.
EFFECT: method provides virtually quantitative conversion of metal-containing components to the end product.
17 ex, 2 tbl
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Authors
Dates
2011-02-20—Published
2009-01-19—Filed