FIELD: chemistry.
SUBSTANCE: invention relates to a method of producing manganese (II) n-aminobenzoate through direct reaction of metal with carboxylic acid in the presence of an oxidising agent. The oxidising agent used is manganese peroxide in molar ratio to metal equal to 1:1-1:3 in total molar load of metal-containing reagents equal to 0.75-1.25 mol/kg and in molar ratio with acid equal to 1:(1.95-2.0). The liquid-phase solvent used is butyl acetate. The stimulating additive used is molecular iodine and solid manganese n-aminobenzoate, taken in amount of 0.01-0.10 mol/kg and 0-0.035 mol/kg respectively. Loading is done successively: glass beads in weight ratio to the rest of the load equal to 1.5:1, butyl acetate, carboxylic acid, metal, peroxide thereof and molecular iodine, after which the components are stirred and solid manganese carboxylate is added. The process is carried out with spontaneously increasing temperature in the range of 20-45°C and monitoring via sample collection and analysing the samples for content of the end product until achieving output of the calculated value of 98% or more. The process is then stopped, the reaction mixture is separated from the glass beads, cooled to 10-15°C, kept at that temperature for 1.5-2.0 hours and then filtered. The residue is then removed from the filter and taken for purification through recrystallisation. The filtrate then accumulates and then undergoes simple distillation; the distilled solvent is then returned to the reverse process and an additional amount of the end product is then extracted from the still after cooling and filtration.
EFFECT: high output of the end product, improved environmental properties of the process and low power consumption.
2 cl, 16 ex, 1 tbl
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Authors
Dates
2011-03-20—Published
2009-07-17—Filed