The method of producing reagent collector on the basis of oxyalkylation acids for flotation of ores disulfidnykh

 

(57) Abstract:

Usage: mineral processing, flotation of ores. The inventive mixture of carboxylic acids with 6-18 carbon atoms reacts with phosphorus trichloride at 120-150oC. carry out the hydrolysis of the resulting reaction mass at 80-110oC. as the source reagent impose additional phosphorous acid. The molar ratio of phosphorous acid, phosphorus trichloride and the mixture of carboxylic acids is from 1.0: 0.5 to: 1.0 to 1.3:0.8 to 1.0 second. Use of phosphorous acid, obtained by hydrolysis of phosphorus trichloride hydrochloric acid or by hydrolysis VAT residue production dimethylphosphite. 2 C.p. f-crystals.

The invention relates to chemical technology for reagent collector on the basis of oxyalkylation acids intended for the enrichment of phosphate ores and oxidized ores of non-ferrous metals.

A method of obtaining a flotation reagent for enrichment of oxidized ores of non-ferrous metals, which is that of aliphatic acids containing from 6 to 10 carbon atoms, or mixtures thereof is subjected to interaction with phosphorus trichloride and water, with tempini processing hydrolyzate miscible with water, an organic solvent and sodium hydroxide [1]

The disadvantages of the method are the use of flammable liquids and having stage filtering fine suspension Dimitrievich salts 1-oxyalkylation 1,1-acids.

A method of obtaining higher Axelmannstein acid interaction6-C18-carboxylic acids with water trichloride and phosphorus when heated to 120-150oWith subsequent hydrolysis of the resulting reaction mixture with water at 80-110oAnd the selection of the target product by successively added to the hydrolysate miscible and non-polar solvents [2] (the prototype).

The main disadvantage of this method is the use of a large number of solvents, the volume of which amounts to 4-7 volume of the hydrolysate, and their regeneration requires significant energy costs. Another disadvantage of this method is very rapid interaction of phosphorus trichloride with water, complicating the process.

The aim of the invention is the elimination of the technological process is energy intensive and explosion-fire processing stage hydrolysate of organic solvents. An additional aim of the invention is, who on receipt of flotation reagent interaction of a mixture of carboxylic acids with 6 to 18 carbon atoms with phosphorus trichloride at 120-150oC, followed by hydrolysis at 80-110oWith as a source of reagent addition use of phosphorous acid and phosphorous acid, phosphorus trichloride and the mixture of carboxylic acids take in a molar ratio of from 1.0:0.5 to:1.0 to 1.3:0,8:1,0.

An additional objective is achieved by the use of phosphorous acid, obtained by hydrolysis of phosphorus trichloride with hydrochloric acid or by hydrolysis VAT residue production dimethylphosphite.

Common indicators of ways to get diphosphonic acid is the molar ratio of the amount of the compound of trivalent phosphorus to the amount of carboxylic acids. This ratio stoichiometry should be 2:1. In the known methods the synthesis is conducted at a molar ratio of 2:2, i.e., when the twofold excess of carboxylic acids. In the proposed method, this ratio is 2: 1,1, allowing you to get flotation without labor-intensive extraction and regeneration of the excess carboxylic acid.

Below are examples of the proposed method.

Example 1. In h is coy, download 63,14 g (0.77 mol) of phosphorous acid and 100,38 g (0.66 mol) of a mixture of synthetic fatty acids (C6C18. In the resulting mixture is metered 57,53 g (0.41 mol) of phosphorus trichloride. The molar ratio of phosphorous acid:phosphorus trichloride: carboxylic acid is 1,18:0,62:1. Raise the temperature to 140oWith and lead synthesis within 6 hours. Then the reaction mass is then cooled, poured 80 g (of 4.44 mol) of water and carry out hydrolysis for 3 hours at a temperature of 103oC. Get 256,6 g of flotation reagent containing 55,11% Axelmannstein acids, 7,68% synthetic fatty acids.

Example 2 (comparative). In chetyrehosnuju flask is charged with 100,36 g (0.66 mol) of a mixture of synthetic fatty acids, 41,54 g (2,31 mol) of water. In the resulting mixture is metered 165,56 g (1.18 mol) of phosphorus trichloride. Further synthesis and hydrolysis are the conditions of example 1. Obtain 240 g of a viscous non-conforming product is yellow, stratifying during storage. Because 2,31 mole of water hydrolyzing of 0.77 mole of phosphorus trichloride with the formation of 0.77 mole of phosphorous acid, the molar ratio of the reactants is the same as example 1.

Example 3. In the flask is charged with 70,52 g (0.86 mol) of phosphorous acid, 100,38 g (0.66 mol) cosines and hydrolysis are in accordance with example 1. Obtain 242 g of flotation reagent containing 45,3% of the basic substance, 15.2% of fatty acids.

Example 4. In the flask is charged with 54,12 g (0.66 mol) of phosphorous acid, 100,38 g (0.66 mol) of a mixture of fatty acids and dispense 74,36 g (of 0.53 mol) of phosphorus trichloride. The molar ratio of reagents 1,0:0,8:1. Further synthesis and hydrolysis are in accordance with example 1. Get 245 g of product containing 45.6% of the basic substance, 13.3% of the fatty acids.

Example 5. Into the flask is poured 64,9 g abgaznaya hydrochloric acid and dosed 106,63 g (0,76 mol) of phosphorus trichloride. In the resulting phosphorous acid load 100,38 g (0.66 mol) of a mixture of fatty acids and dispense 57,53 g (0.41 mol) of phosphorus trichloride. The molar ratio of reagents 1,15:0,62: 1. Further synthesis and hydrolysis are in accordance with example 1. Get 259 g of flotation reagent containing 56.9% of the basic substance, 8,96% fatty acids.

Example 6. In the flask is charged with 61,93 g (of 0.68 mol) of phosphorous acid obtained by hydrolysis of VAT residue production dimethylphosphite, 100,38 g (0.66 mol) of a mixture of fatty acids and dispense 63,80 g (0.46 mol) of phosphorus trichloride. The molar ratio of reagents 1,02:0,7:1. Further synthesis and hydrolysis are in accordance with example 1. Get 246 g of flotation reagent containing a synthesis step ready phosphorous acid allows to obtain flotation of the required quality at low excess carboxylic acid and thereby eliminate labor-intensive stage of separation of the reaction mixture with the use of solvents. In the known methods of phosphorous acid is also involved in chemical processes, however, it is formed by the hydrolysis of phosphorus trichloride with water in the environment carboxylic acid, which is accompanied, obviously, other reactions.

The proposed method also has advantages:

several times reduced thermal effect of reaction that makes hazard the boot process trichloride phosphorus;

reduces the viscosity of the reaction mixture entering the hydrolysis, which provides intensive mixing and accelerates stage hydrolysis;

allows you to utilize agathou hydrochloric acid or waste production dimethylphosphite.

1. The method of producing reagent collector on the basis of oxyalkylation acids for flotation disulfidnykh ores, including the interaction of a mixture of carboxylic acids with 6 to 18 carbon atoms with phosphorus trichloride at 120 150oWith subsequent hydrolysis of the resulting reaction mass at 80 110o, Characterized in that as starting reagent addition use of phosphorous acid and phosphorous acid, phosphorus trichloride and the mixture of carboxylic acids take in a molar ratio of 1,0 0,5 0,8 1,0 1,3 1,0.

is asfora hydrochloric acid.

3. The method according to p. 1, characterized in that the use of phosphorous acid, obtained by hydrolysis of the cubic residue production dimethylphosphite.

 

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