| 摘要 |
FIELD: chemistry. ^ SUBSTANCE: invention relates to an improved method of producing basic phthalate of iron (III), which is used in chemical practice, analytical control and scientific research, through direct reaction of iron with atmospheric oxygen and phthalic acid in the presence of organic solvent, where the stimulating additive used is hydrochloric acid and inorganic chlorides in amount ranging from 0.013 to 0.062 mol/kg of the load. The liquid phase solvent is n-butyl alcohol iron which is crushed and moved in the reaction zone in form of steel balls with diametre ranging from 2.2 to 3.7 mm, alone or in combination with crushed cast iron in any mass ratio. Initial content of phthalic acid is varied from 1.0 to 1.5 mol/kg of the load. The reactor used is a vertical type bead mill with the grinding agent in form of steel balls and crushed alloy of iron together with glass beads in mass ratio of iron-containing reagent, beads and the rest of the load equal to 1:1:0.6 with a spill pipe as a bubbler during the process. Loading is done in the following sequence: grinding agent and moved metal, liquid phase solvent, phthalic acid, chlorine-containing stimulating agent, and the process itself starts with heating contents of the reactor to 35, is carried out with self-heating in the range 35 to 50C while stirring continuously, bubbling air at a rate of 2.3 to 3.1 l/(min kg of load), while maintaining temperature using a cooling liquid bath and controlling the process using a sampling method until exhaustion of all loaded acid, after which bubbling is stopped. Suspension of the reaction mixture is let to flow under gravity through a net lying in the field of a permanent magnet into the receiving tank of a vacuum filter, after which it is filtered. The residue is washed with the liquid phase solvent and taken for purification, and the primary filtrate and washing solvent are returned to the repeated process. ^ EFFECT: non-waste method at low temperature; wastes from other industries can be used as reagents; desired products can be separated by simple filtration. ^ 2 cl, 8 ex |
