Method of disposal of waste from the production of ferromanganese in the composition of the ore part of the charge

 

(57) Abstract:

The invention relates to metallurgy manganese and can be used in the hydrometallurgical processing of vysokofosforistye carbonate and manganese ore and waste from the production of ferromanganese to obtain manganese concentrate. Method of disposal of waste from the production of ferromanganese in the composition of the ore part of the charge (RCS) includes obtaining the mn containing solutions, additives thereto of an alkaline reagent, filtering, washing and heat treatment RCS. With the addition of an alkaline reagent to impose an additional wastes from the production of ferromanganese in relation RCS waste, equal to 1: (0,10-1,10), and maintains the slurry with stirring 0.2 to 1 hour, and heat treatment RCS carried out in two stages at 70-105C and at 200-250C. the Invention will dispose of wastes from the production of manganese ferroalloys, which will expand the raw material base deficit mn containing raw materials, to increase the filtration rate of the slurry, and also to reduce the loss of manganese in the smelting of manganese alloys by reducing the removal of fines from the flue gases and, ultimately, to increase the degree of extraction of manganese and reduce toxic waste. In addition, prego filtration equipment. table 4.

The invention relates to metallurgy manganese and can be used in the hydrometallurgical processing of vysokofosforistye carbonate and mixed ore and waste from the production of ferromanganese to obtain scarce manganese concentrate required for the production of manganese alloys.

The well-known "Method of obtaining the mn containing briquettes" (A. C. 1698305 USSR MKI5C 22 B 1/24) publ.15.12.91, bull. N 46, which is proposed as the mn containing component of the ore part of the charge to use carbonate of manganese concentrate with the introduction of fluxing additive hydrated lime. Concentrate and lime are mixed in a mass ratio. (3.5 to 5) : 1 and after mixing them carry out the drying in two stages: first at 140-160oC for 0,58 - 1.2 hours, and then 380-420oC in the course of 0.43 - 0.55 hours.

The disadvantages of the method are:

1. Use to harden the briquettes expensive commercial product - lime;

2. High energy costs - drying at a temperature of 140 - 420oC;

3. The inability to obtain a homogeneous mixture, because it is mixing of solid products.

A method of obtaining pelletized ore cha is klaverbank pellets and melt with their use of high-carbon ferromanganese". In Proc. of Theory and practice of metallurgy manganese". - M.: Nauka. 1990, S. 114). As a source of raw materials used concentrate the following chemical composition in %: 44,2 Mn; 13,6 SiO2; 1,4 CaO; 3,3 MgO and cloddy quicklime.

Technological scheme includes: grinding manganese concentrate to fraction minus 0,074 mm, and lime to a fraction of 0.08 mm, dosing and mixing of fine powders, pelletizing and heat-moisture treatment in an autoclave at a gauge pressure of 1.3 MPa and a temperature of 182 - 190oC for 3.5 hours. Thus was obtained pelletized ore part of the mixture with a moisture content of 2 to 5.7 %, a manganese content 32,37 - 34,74% and the output of the fine fraction is 5 mm 0.3 to 3.7 per cent.

The disadvantage of this method is:

1. Use for work is a commodity lime:

2. The need for fine grinding of the original components of the charge (0,074 and 0.08 mm), which complicates the technological scheme, increases the power consumption and complexity of processes;

3. The complexity of the hardware design, the use of autoclaves, which entails higher capital and labor.

4. The inability to obtain a homogeneous mixture, because it is solid-phase mixing of the materials.

5. Naesb is usnote and received results is a flow chart, including the processing of finely ground manganese ore, slimes or low-grade concentrates at atmospheric pressure or autoclaves hot acid leaching of manganese, filter, additive to the filtrate reagent emitting manganese in the form of a hydroxide, or the receipt of manganese sulfate or carbonate and fired at 800-1000oC to obtain compounds of manganese in the form of an agglomerate, i.e., the ore part of the charge. (C. I. anoosh and other "Getting low-phosphorus manganese concentrates", Kiev, Tekhnika, 1969, S. 146-149).

The disadvantage of this method is the low filtration rate of the slurry during the precipitation of manganese concentrate component 100-120 l/m2hour, and the low yield of fractions: +3.0 mm, resulting in losses of manganese and frustration mode furnaces in the smelting of manganese ferroalloys.

The aim of the invention is the utilization of waste from the production of manganese ferroalloys, the expansion of raw materials scarce mn containing raw materials through the use of waste production, increase the rate of filtration of the pulp during the precipitation of manganese, the reduction of losses in the smelting manganese manganese alloys by reducing removal IU the surface discharge, the reduction of areas under samoatel and capex extra filtration equipment.

This objective is achieved in that in the known method the ore part of the charge (RCS), including the production of mn containing solutions, Supplement to the mn containing solutions of alkaline reagent with the addition of waste from the production of ferromanganese in respect of the ore part of the charge to waste, equal to 1: (0,10 - 1,10) and exposure of the pulp in the mixing 0.2 to 1 hour, filtering, washing and heat treatment received ore part of the charge in two stages at 70-105oC in the first stage and at 200-250oC - in the second stage.

Additional introduction of waste from the production of ferromanganese on stage deposition RCS and conducting two-stage heat treatment RCS allows you to increase the filtration rate 1.2 to 2.4 due to the coagulating properties of waste from the production of ferromanganese, which will reduce operational, labor and energy costs and reduce the cost of additional equipment and capital construction. There is a decrease in the content of manganese in the filtrate with 0,306 g/l to 0,099 - traces, which increases the degree of extraction of manganese in the composition RCS, reduces stratums strength characteristics of conglomerates at the expense of the binding properties of the waste, fall in alkaline medium, with two-stage heat treatment yield small fraction minus 3 mm 1.3 - 17,8 times less than in the experiments without the addition of waste production of ferromanganese. Increases the strength of the resulting conglomerates RCS - after testing them for strength small fraction minus 3 mm is formed in the 1,4 - 25,8 times less, and when testing for thermal stability of its output is reduced 1.3 - 4 times.

The improvement of these characteristics allows to reduce losses RCS metallurgical transformations, ultimately, to increase the degree of extraction of manganese in the metal and to improve the environment by reducing the removal of fines.

As starting materials for carrying out laboratory tests used carbonate ore Midnight Deposit (sample 1), product enrichment concentrate received on its enrichment (sample 2), the gas cleaning sludge from the production of ferro-manganese (sample 3).

Table 1 shows the composition of the original sample.

The impact of the introduction of waste from the production of ferro-manganese in the settings for the ore part of the charge and its properties were studied by the following method: raw materials - carbonate manganese ore (sample 1, that is was hyperoval in 2.0 l of water. In the resulting slurry was injected hydrochloric acid to pH 1.7 and withstood the slurry under stirring for 7 hours at 70oC. Then, the slurry was injected calcium reagent (lime milk, lime and others), adjust the pH of the slurry within pH 2.8 - 3.2, and kept under stirring for 0.5 hours and perform filtering.

The filtrate, representing the basis of the chloride of manganese, divided into portions of 0.3 l and conducted experiments to obtain RCS.

Example 1.

Of carbonate manganese ore (sample 2, table. 1) spent leaching of manganese by the method described above, adjusting the PH of the spent limestone, crushed to a fraction of minus 0.16 mm and after filtering the received filter containing, g/l: 54 manganese, 0,004 - phosphorus, 0.01 to iron and 0.15 - silicon oxide.

The experience of the prototype was conducted without the addition of waste from the production of ferro-manganese (PL. 2. experience 1 prototype), when introduced in 0.3 l of filtrate of the suspension of calcium hydroxide with a concentration of CaO 150 g/l to pH 10 and stirring for 0.5 hours. The following experiments 2-8 (see tab.2) held with the introduction of a certain amount of waste - sludge (sample 3, see table. 1), with the addition of calcium hydroxide (150 g/l CaO) to pH 10. After mixing the extracts of the pulp is carried out her first drying at 90oC for 1 hour and then at 200oC for 0.5 hours.

After that RCS was a durable baked conglomerates. Characteristics of their strength in example 1 was determined by the exit mass fraction fraction -3,0 mm immediately after drying, and then in examples 2-4 after the dissolution of a particular sample of conglomerates with a height of 1.5 m (again determined the presence of a fraction is 3.0 mm). In addition, it was determined thermal resistance conglomerates with their quick heating up to 850oC in the definition of output fractions -3 mm and after the test.

The dependence of these characteristics on the conditions of the experiments are given in table. 2 (examples 2-8).

The results of the experiments are given in table. 2, from which it follows that the introduction of the sludge within the relationship 1: (0,1 - 1,1) RCS waste from the production of ferromanganese, the filtration rate is increased in comparison with the experience of the prototype 1.2 - 2.4 times, which will reduce operational, labor and energy costs, and reduce the cost of purchasing additional filtration equipment and capital construction.

When the ratio is less (1:0,05) this effect is negligible, because the insufficient action of the slurry, as coagulating dobie change in strength characteristics of conglomerates, formed during drying (experience 3-7).

With the introduction of the pulp upon receipt RCS waste reduced content of manganese in the filtrate with 0,306 g/l to 0,099 - traces, which allows not only to increase the degree of extraction of manganese in the composition RCS, but also reduce cleaning solutions and to improve the environment by reducing toxic effluents. In addition, the additive waste changes this characteristic RCS as vaccum RCS: after filtering in the present limits of the relationship between 0.1 and 1 humidity sediment below 1.05-1.28 times that reduced power consumption during heat treatment and reduction of water consumption in the process.

Example 2

Study of the influence of the stage of heat treatment RCS on its granulometric composition (exit faction -3 mm) was performed according to the method described in example 1.

Characteristics RCS obtained depending on the parameters I and II stages of heat treatment are given in table. 3.

At stage I is the physical destruction of moisture. At temperatures below 70oC the process is very slow and RCS the second stage heat treatment comes with high humidity from 20 to 7.8%, so when heated conglomerates 200oC is the boiling Fe 105oC. Exposure RCS at stage I when 70-105oC after exposure at stage II for 0.5 hour at 200oC provides the output fraction minus 3 mm in the range of 0.5 to 1.7%, Rel. in comparison with the experience of the prototype of 8.9% Rel., ie 5.2 - 17.8 percent times less. After dropping the received conglomerates (research strength) from a height of 1.5 m output detail by the present method is 0.5 - 1.5% Rel. or 12-36,2 times lower than in the experience of the prototype. The same holds when tested for thermal stability conglomerates output fraction -3 mm within the proposed method is 0.6 to 1.3% Rel. or 5.3 to 2.5 times less than in the experience of the prototype.

Example 3.

Study of the influence of the conditions of the second stage heat treatment RCS on granulometric composition was performed according to the method described in example 1, and the ratio and the heat treatment for stage I conducted according to the experience of 2.3 (see tab. 3).

The temperature of the second stage was changed from 190 to 260oC, soaking the samples RCS at a given temperature for 0.5 hours. Experiments have shown (PL. 4), that exposure to second-stage heat treatment in the range from 200 to 250oC allows you to receive the output of the fine fraction -3 mm after the second heat treatment in a 1.3 to 17.8 times less than in epinasty below 1.3 - 4 times. Heat treatment in the second stage at a temperature below 200oC does not allow to obtain figures, exceeding the results of the prototype, because the residual moisture content under these conditions in the conglomerates is at the level of 11.2 5.5 percent, thereby reducing the quality of conglomerates RCS. The exposure at 260oC is impractical, because the quality indicators RCS worse.

Example 4.

With optimal parameters is carried out the processing of 1 kg of manganese concentrate, obtained during the concentration of ore (sample 2, see tab. 1). The concentrate was ground to a fraction of -0,315 mm and was added 2 liters of water, heated slurry to 70oC. Under stirring to the slurry introduced hydrochloric acid to pH 1.7 and kept for 5 hours. Then introduced the calcium hydroxide with a concentration of 150 g/l CaO to pH 3.0 and withstand the pulp for 0.5 hour with stirring. After filtering received of 3.25 liters of mn containing solution with content, g/l: 71,8 manganese, 0,002 - phosphorus 0,011 of silicon oxide.

To obtain RCS to the solution was added until a pH of 9.9 suspension of calcium hydroxide with a concentration of 150 g/l CaO and 53,9 g of waste sludge from the production of ferro-manganese (sample 3, see table. 1). The slurry was kept under stirring 0.7 hours and posively 90oC for 1 hour, and then raised the temperature to 220oC and kept for 0.5 h at the same temperature.

After the two-stage heat treatment and cooling RCS output fraction -3 mm amounted to 0.3%, after a drop of 2.7%, and after testing, thermal resistance of 1.1%.

The manganese content in air-dry RCS after stage filtration to 38.5%. After calcining the mass loss amounted to 26.0% and the manganese content in RCS became 52,0%.

The use of the proposed method when processing 70.0 thousand tons of manganese ore beneficiation of low-grade carbonate ore Russia to dispose of up to 40 thousand tons of waste - sludge blast furnace ferromanganese production concentrate, suitable for the production of manganese alloys in an amount of about 60 thousand tons/year containing an extra 6 thousand tons of manganese.

Expanding resource base at the expense of waste disposal while also improving such technological parameters as filtration rate (an increase of 1.1 - 2.4 times), which reduces the capital cost of installing additional filtration equipment, buildings to install them. In addition, reduced labor and energy costs on the giving of waste - of gas-cleaning sludge from the production of ferro-manganese improves the strength of the conglomerates manganese concentrate (output trivia -3 mm less than 1.3 at 17.8 times) and their resistance during thermal shock (output trivia -3 mm less than 1.3 to 4.0 times), thereby improving the environmental performance of the process of smelting of manganese alloys, increasing the degree of extraction at the stage of obtaining manganese alloys.

Method of disposal of waste from the production of ferromanganese in the composition of the ore part of the charge, including the production of mn containing solutions, Supplement to the mn containing solution of an alkaline reagent, filtering, washing and heat treatment received ore part of the charge, characterized in that with the addition of an alkaline reagent to impose an additional wastes from the production of ferromanganese in respect of the ore part of the charge to waste, equal to 1 : (0,10 - 1,10), and maintain the slurry with stirring 0.2 to 1 h, the heat treatment of the ore part of the charge is carried out in two stages at 70 - 105oWith the first stage and at 200 - 250oWith the second stage.

 

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