| 摘要 |
FIELD: chemistry. ^ SUBSTANCE: invention relates to an improved method for synthesis of lead (II) acetate through direct reaction of a metal, its dioxide with a carboxylic acid in the presence of an organic liquid phase and a stimulating iodine additive in a vertical bead mill, where the oxidising agent and the reagent in deficit are lead dioxide taken in amount of 0.4-0.6 mol/kg, metal and acetic acid are taken in amount of 0.6-1.5 mol/kg and respectively so as to obtain mol/kg of a salt product, where nPbO2 is amount of lead dioxide in mol/kg. The stimulating additive used is iodine taken in amount of 0.01-0.05 mol/kg liquid phase, the base of which is initially composed of an organic solvent and acetic acid and iodine dissolved in the said solvent. Components of the reaction mixture are loaded in the following sequence: liquid phase solvent, acetic acid, metal, its dioxide, molecular iodine. Mass ratio of the components and glass beads is at least 1:1.5; the process starts at room temperature and is carried out at maximum temperature of 30-50C under forced cooling conditions and while controlling using a sampling method and determining content of accumulated salt and unreacted lead dioxide and acetic acid in the said samples until the oxidising agent is virtually exhausted, after which the process is stopped. The suspension of the reaction mixture is separated from the glass beads and thin films of unreacted metal by passing through netting with cell size of 0.3ù0.3 mm as a filter partition. The beads and unreacted metal are returned to the reactor where together with the housing, mixer and other components of the reactor are washed with the liquid phase solvent from reaction mixture remaining after discharge thereby obtaining a washing solvent; the suspension of the reaction mixture is filtered, the residue on the filter is treated with the washing solvent, pressed well and taken for cleaning through recrystallisation, and the obtained filtrate in a mixture with the washing solvent is returned to the repeated process. Output the filtered off product is 93-98% of the theoretical output. ^ EFFECT: design of an improved method of obtaining lead acetate. ^ 2 cl, 15 ex |
