Method of processing manganese carbonate ore

FIELD: chemistry.

SUBSTANCE: method involves leaching alkali and alkali-earth metals with a solution of a chlorine-containing reagent and separating the insoluble residue containing manganese dioxide. The ore undergoes preliminary decarboxylation via thermal treatment at temperature 750-1000°C for 2-4 hours to obtain coal tar. The chlorine-containing reagent used when leaching the coal tar is 10-40% aqueous ammonium chloride solution, taken in weight ratio ore: ammonium chloride equal to 1:1-2. Leaching is carried out at temperature 20-100°C for 1-2 hours. After separating the insoluble residue, the filtrate is carbonised with exhaust gases from the ore decarboxylation step, followed by separation of the obtained calcium carbonate and return of the aqueous ammonium chloride solution to the coal tar leaching step.

EFFECT: obtaining quality end product - manganese dioxide concentrate and a by-product - calcium carbonate using a zero-discharge process scheme.

1 dwg, 1 tbl, 1 ex

 

The invention relates to a method of chemical enrichment of carbonate manganese ores and can be used for processing depleted in manganese ores.

A method of refining manganese raw material [A.S. No. 1518400, CL SW 47/00, publ. Bull. No. 40, 1989], including the leaching of the raw material containing manganese dioxide circulating solution of sulfuric acid and ammonium sulfate in the presence of ferromanganese as a reducing agent to achieve a pH of 1.8-2.0, separating the insoluble residue from the solution by filtration, and purification of the filtrate from the impurities of iron and phosphorus by precipitation with ammonia at pH of 4.5-5.0. The allocation of manganese from a purified filtrate is carried out by electrolysis, the circulating sulfuric acid return to the stage of leaching.

The disadvantage of this method of enrichment of carbonate manganese ore is high corrosiveness of the reaction medium due to the use of sulphuric acid for leaching and the need for ferromanganese.

There is a method of enrichment of manganese carbonate ores [U.S. Pat. Of the Russian Federation No. 2090641, CL SW 47/00, publ. Bull. No. 3, 1997], comprising grinding the ore to a particle size of 0.1 mm, autoclave leaching of manganese saturated aqueous chlorine-containing reagent, separating the solution from the residue and precipitation of manganese from solution in the form of its compounds. As the chlorine-containing reagent IP is result calcium chloride. The leaching solution of calcium chloride is carried out in a ratio of 1:3.0 to 3.5 with subsequent heating of the pulp within 0.5 to 1.0 h and its pumping through battery autoclave, heated to 200-220°C. Then, to the slurry is added calcium chloride in the amount of 40-60% by weight solids and iron chloride until the concentration in the solution 2,02-2.5% and pumping the mixture through a second battery autoclave heated to 240-260°C; then the slurry is cooled to 90-100°C., separating a solid residue, precipitated manganese from solution by pushenkoj, filtered, washed, calcined and doused or bitteroot. The final product after calcination contains up to 60-64% manganese content of impurities of calcium oxide 3-4%, calcium chloride 3-5%, of silicon oxide to 1%. Extraction of manganese in the final product - 92-95,5%.

The disadvantage of this method is the complexity of the technological process associated with the use of two systems battery autoclaves, high temperature leaching process (200-260°C), the use of chloride of iron, a significant consumption of reagent is calcium chloride.

Closest to the claimed method is [A.S. No. 2222624, CL SW 47/00, SW 3/10, publ. Bull. No. 3, 2004], including leaching from ore alkali and alkaline earth metals with a solution of chlorine - containing reagent hydrochloric acid at a controlled pH value of the medium and separating the insoluble precipitate, terasawa manganese oxide. As the chlorine-containing reagent is used a solution of hydrochloric acid. Leaching of lead abgaznaya hydrochloric acid concentration 5-18% at pH of 6.0-6.5 and at a temperature of 15-45°C. In the process of leaching the ore with hydrochloric acid at elevated temperatures is allocated chlorine gas for absorption using sodium hydroxide solution. The filtrate is directed to obtaining a co-product is calcium chloride. In the resulting insoluble precipitate the manganese content is increased by 3-4 times. The departure process is the absorption solution phase absorption of exhaust gases containing hypochlorite, chloride and sodium carbonate.

The disadvantage of this method of enrichment of carbonate manganese ore is high corrosiveness of the reaction medium due to the use of hydrochloric acid, the presence of a large volume of wastewater. As a result of processing ore with hydrochloric acid is secreted chlorine gas, which adds cost and complexity to the process of ore.

The task, which is aimed by the invention is the development of industrially-applicable method for processing manganese carbonate ores with a low manganese content of from 7 to 25 wt.%, and waste schema enrichment of manganese ore. When using the invention can be obtained by technical financial p is tat, which is expressed in the possibility of obtaining high-quality target product is a concentrate of manganese dioxide and a co-product of calcium carbonate.

This technical result in the implementation of the invention is achieved by a method for processing manganese carbonate ores, including pre-decarboxylation ore by heat treatment at 750 to 1000°C for 2-4 hours with obtaining peck, leaching of coal tar pitch at a temperature of 20-100°C for 1-2 hours chlorine-containing reagent is 10-40%aqueous solution of ammonium chloride, taken in a mass ratio of ore:ammonium chloride is 1:1-2, separating the insoluble precipitate containing manganese dioxide; the filtrate after separation of the insoluble precipitate carbonizing flue gases from stage decarboxylation of ore, followed by the separation of the obtained calcium carbonate and magnesium and further return generated an aqueous solution of ammonium chloride on stage leaching pitch. In the process controlling the concentration of ammonium chloride, if necessary add crystalline ammonium chloride.

The invention consists in the following.

Heat treatment is subjected to ore having the following composition, wt.%: Caso3- 70-80; Mno2- 7-25; MP2About3is 0.3 to 1.5; Fe2 About3- 2-5; And2About3- 1-2; SiO2- 4-7; MgSO3- 1-3. During heat treatment at a temperature of 750 to 1000°C source of manganese carbonate ore within 2-4 hours the process of decarboxylation of carbonates of alkaline earth metals with carbon dioxide and the formation of the corresponding oxides of calcium and magnesium:

Further chilled peck is subject to leaching 10-40%ammonium chloride solution for 1-2 hours. The leaching process proceeds with evolution of heat, due to which the temperature of the reaction mixture increases from 20 to 100°C. leaching of coal tar alkaline and alkaline earth metals into solution. The oxides of alkaline earth metals pass into solution in the form of chlorides of calcium and magnesium

The reaction mixture is sent to the stage of separation of the insoluble precipitate. The precipitate is washed with water and dried. The resulting product is a concentrate of manganese dioxide. The filtrate containing the chlorides of calcium, magnesium and ammonium hydroxide is subjected to carbonization of the waste gas phase thermal decarboxylation containing carbon dioxide. The carbonisation formed carbonates of calcium, magnesium and chloride is ammonium

Carbonates of calcium and magnesium extracted precipitated and separated by filtration. The liquid phase is a 10-40%solution of ammonium chloride, which is returned to the step of leaching peck.

The leaching process takes place in a neutral aqueous solution of ammonium chloride, which malcolmsonii that does not require selection of special materials for the manufacture of equipment for the leaching step. When using the invention in addition to the target product is obtained calcium carbonate of high quality. The processing of manganese ores closed, as the resulting solution of ammonium chloride is returned to the process cycle leaching.

Schematic diagram of processing of carbonate manganese ore shown in the drawing.

Example 1. 1000 g of the original carbonate manganese ore, containing (wt.%) 10.73 Mno2, 0.42 MP2About3, 77.05 caso3, 2.13 MgCO3, 3.73 Fe2O3, 1.19 Al2About3and 4.75 SiO2. subjected to heat treatment at a temperature of 900°C for 3 hours. Get peck in the number 649,8 g containing (in wt.%) 16.51 Mno2, 0.65 MP2O3, 66.40 Cao, 1.57 MgO, 5.74 Fe2O3, 1.83 Al2About3and 7.30 SiO2. Allocated 350,2 g of carbon dioxide, to which were referred to the stage of carbonization. Peck (649,8 g) subjected to leaching 5000 g reverse a 20%aqueous solution of ammonium chloride for 1.5 hours at 70°C. the Mass ratio of ore:ammonium chloride is 1:1. The precipitate was separated by filtration, washed with water and dried to obtain the target product in the amount of 208,15, the Concentrate contains (in %): 51.55 Mno2, 2.02 MP2O3, 17.92 Fe2O3, 5.72 Al2O3and 22.79 SiO2. The filtrate contains 17.05% l2, 0.48% MgCl2, 11.1% NH4OH. Next, the filtrate in the number 5440,6 g is subjected to carbonization exhaust gases from the stage decarboxylation. The result is a pulp in the amount of 5790,85 g containing carbonates of calcium and magnesium in the form of a solid phase and ammonium chloride in the liquid phase. Filtering the pulp produce precipitates of carbonates of calcium and magnesium, after washing and drying receive 790,85 g of calcium carbonate content of 97.3% of the basic substance. The filtrate in the amount of 5000 g, representing a 20%solution of ammonium chloride, return to the stage leaching peck.

The appropriateness of the ranges of processing carbonate manganese ores are presented in table 1.

The process in the specified ranges of process parameters provides for the recycling of depleted manganese carbonate ores with obtaining a concentrate of manganese dioxide and the carb is Nata calcium high quality, ore processing waste-free and environmentally friendly scheme.

2 900
Table 1
Influence of technological parameters on the processing of carbonate manganese ores
no experienceDecarboxylationLeachNote
Temperature, °CDuration, hThe concentration of R-RA NH4Cl%Duration, hTemperature, °CThe ratio of ore: NH4Cl
19003251,5701:1,5high quality manganese concentrate
27003202701:1 partial decarboxylation, reduction in the quality of the concentrate
311003202701:1sintering ore
49001202701:1partial decarboxylation, reduction in the quality of the concentrate
59005202701:1irrational use of energy resources, the cost of product
6900372701:1incomplete leaching, degradation concentrate
7900345701:1the excess reagent (ammonium chloride)
89003200,5701:1incomplete leaching, degradation concentrate
99003202,5701:1slow performance
109003202151:1the necessity of cooling the reaction mixture stage leach
1190032021051:1the necessity of heating the reaction mixture under leach
123202701:0,8incomplete leaching, degradation concentrate
1390032020701:2,2the excess reagent

Method for processing manganese carbonate ores, including leaching of alkali and alkaline earth metals with a solution of chlorine-containing reagent, separating the insoluble precipitate containing manganese dioxide, wherein the pre-ore is subjected to decarboxylation by heat treatment at a temperature of 750 to 1000°C for 2-4 h with obtaining pitch, as the chlorine-containing reagent leaching of pitch use 10-40%aqueous solution of ammonium chloride, taken in a mass ratio of ore:ammonium chloride is 1:1-2, the leaching is carried out at a temperature of 20-100°C for 1-2 h, the filtrate after separation of the insoluble precipitate carbonizing exhaust gases from the stage decarboxylation of ore, followed by the separation of the obtained calcium carbonate and returning the aqueous solution of chlorine is IDA ammonium on stage leaching pitch.



 

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