RU2674178C2 - Production of high-grade manganese from ferromanganese by means of vaporisation in vacuum induction plant - Google Patents

Abstract

FIELD: metallurgy.

SUBSTANCE: invention relates to the field of metallurgy and can be used to obtain industrially pure manganese by vaporizing carbon-containing ferromanganese in an induction vacuum unit. Pan containing liquid carbon-containing ferromanganese is inserted into an induction vaporizer, pressure is controlled in the range of 10–900 mbar using a system of vacuum pumps and a filter system, manganese is vaporized at a temperature above the manganese liquidus temperature of 1,248 °C and is purged with an inert gas, obtained manganese vapour is cooled in a steam pipe tightly connected to the induction vaporizer and a movable condensation chamber, manganese vapour is collected in the mobile condensation chamber at a temperature of 1,350 to 1,400 °C in a liquid aggregation state and continuously discharged from said chamber through a siphon heated tray into a filling machine and cast into the target product. In the installation, the induction vaporiser and the mobile condensation chamber are tightly connected to each other by the steam line to cool the manganese vapour by means of a primary water cooler enclosing the steam line outside, and a secondary water cooler is located inside the steam line in the vapour flow above the chamber, wherein the chamber has a siphon warmed fly for the continuous release of industrially pure manganese to the filling machine.

EFFECT: invention allows to continuously obtain industrially pure manganese by evaporation of cheap raw materials.

13 cl, 3 dwg

Description

The present invention relates to a method for producing technically pure manganese by evaporation of carbon-containing ferromanganese in an induction vacuum tank.

Manganese is one of the most important alloying elements in steel production. It is characterized by high strength and a large tensile strength. Obtaining different grades of steel using manganese is achieved as a result of the use of manganese-containing alloying additives in the process of its smelting. These include those produced in blast furnaces or reduction furnaces with high carbon manganese alloys such as FeMnHC (HCFeMn) and medium carbon alloys such as FeMnMC (MCFeMn) and low carbon alloys such as FeMnLC (LCFeMn), obtained in secondary metallurgy plants.

In addition to carbon in the indicated amounts, manganese alloys also contain other elements, such as phosphorus and sulfur, due to which the use of materials is limited.

However, the demand for technically pure manganese is constantly expanding to meet the increasing demands for the production of high quality steel. Currently, technically pure manganese is produced only by the electrolytic method, since it is technically impossible to obtain pure manganese by reduction with carbon, since in this case, in addition to manganese, stable carbides are also formed, in particular, Mn ₇ C ₃ .

To do this, use as pure a solution of manganese sulfate as possible, which is subjected to electrolysis using stainless steel electrodes at a voltage of 5-7 Volts. In this case, pure manganese is formed on the cathode, oxygen is formed on the anode, which then reacts with manganese ions to form pyrolusite:

2MnSO ₄ + 2H ₂ O → 2Mn + 2H ₂ SO ₄ + O ₂ .

Along with this, it is also known to obtain manganese by reducing its oxides with aluminum (aluminothermy) or silicon.

Another possibility of producing manganese consists in heating the aforementioned manganese compounds to the evaporation temperature of manganese.

However, pure manganese is formed only at temperatures above 1600 ° C, since only at this temperature part of the manganese begins to evaporate, as a result of which this method of production has so far been unprofitable.

The objective of the present invention is to provide a method for the continuous production of manganese by evaporation of the feedstock, which would not be expensive and, therefore, economical.

This problem is solved by the features described in paragraph 1 of the claims, in particular, as a result of the fact that the method is carried out in vacuum at temperatures above the liquidus temperature of manganese, and the ladle with liquid carbon-containing ferromanganese is placed in an induction evaporator, the metal is obtained in vacuum, and vacuum pump systems and filter systems at 10-900 mbar and temperatures above 1248 ° C, while blowing with an inert gas, evaporate it and cool it during subsequent operation of the unit with water, while the vapor Manganese is condensed in a movable condensation chamber at a temperature of 1350 to 1400 ° C and continuously released through a heated siphon into a filling machine.

The installation and method according to the invention is an innovation not only in the sense of continuous production of manganese, but also in relation to casting.

The following is a description of the metallurgical properties of manganese.

The two-component Mn-Fe system represents the different phases of the transition of the manganese – iron solution. As can be seen from FIG. 2 diagrams, the liquidus temperature of pure manganese is 1246 ° С.

When the manganese content is from 65 to 92%, which is typical for ferroalloys, the liquidus temperature is from 1246 to 1280 ° C. This is the lowest temperature at which liquid material begins to evaporate. The vapor pressure, depending on temperature, has an exponentially increasing curve (see Fig. 3).

To clearly explain the physical conditions for implementing the method according to the invention, the kinetics of the evaporation of manganese is described below.

The kinetics of the evaporation of manganese is a function of pressure, temperature and the amount of inert gas. The evaporation process itself occurs as a result of a phase transition of a liquid into a gas (vapor) at a given temperature and pressure according to the first-order law, as presented in equation (1):

,

,

where: (-dMn / dt) is the evaporation rate,% / min.,

τ is the phase transition constant, in minutes,

[Μn] is the current concentration of manganese,

[Μn ^* ] is the equilibrium concentration Μn at the current stage of the process (p, T, inert gas).

At phase equilibrium (liquid - gas):

,

,

expressed through a temperature-dependent constant K (T),

,

,

the pressure upon evaporation of pMn, and also through the activity coefficient fMn as a function of the composition of the metal, the equilibrium concentration of manganese [Μn ^* ] has the following form:

,

,

Where:

Moreover, they mean:

1. ΝΜn: volumetric flow Μn in a vacuum vessel, normal m ³ / min., Directly proportional to the evaporation rate, expressed in terms of k (-dMn / dt).

2. uАr: argon volume flow blown into the vacuum vessel, normal m ³ / min.

3. p: pressure inside the evaporation tank.

Equations (4) and (5) together with equation (1) give the following dependence:

Equation (6) reproduces the principle of regulation in relation to the following values:

- metal temperature Τ, adjustable in the temperature range over 1246 ° C by inductive heating,

- pressure p in the tank, adjustable in the range from 10 to 900 mbar through a system of vacuum pumps,

- inert gas flow uAr, adjustable in the range from 0.05 to 0.5 normal m ³ / (t metal per min.) using the discharge system.

From this, all the basic parameters necessary for implementing the method according to the invention using the device according to the invention are derived.

According to the invention, it is provided that the condensation of manganese vapor occurs continuously using a secondary cooler installed in the vapor stream inside the steam pipe and having a conical shape to improve the dripping.

Additionally, the vacuum pump system is equipped with a secondary water cooling system, a condenser and a filter. The evaporation process is additionally supported by argon as an inert gas, forming a kind of protective gas atmosphere.

Technically pure manganese is continuously cooled by water, discharged and supplied in a protective atmosphere from argon to a filling machine, where it is cast into the appropriate desired formats.

It is envisaged to adjust during the process the evaporation rate, temperature, the amount of vacuum and the inert gas flow. Evaporated material may have a different concentration of manganese, affecting the rate of evaporation, temperature and inert gas flow.

It is also necessary to ensure that the material to be vaporized continuously or periodically enters the induction evaporator.

Another objective of the present invention is to provide a device for implementing the method according to the invention.

This additional problem is solved by means of a device in accordance with the characteristics described in paragraph 9 of the claims, in particular by means of an evaporator in which a manganese alloy is used, which produces metal under vacuum, which is used with a vacuum pump system and a filter system at a pressure of 10 to 900 millibars and a temperature above 1248 ° C, when purged with argon as a protective gas, is evaporated and cooled using primary and secondary water coolers, while the manganese vapor is collected They are in a liquid state of aggregation in a mobile condensation chamber at a temperature of 1350 to 1400 ° С and are continuously discharged through a heated siphon into a filling machine.

According to another embodiment, the evaporator is an induction evaporator mounted on a hydraulic platform configured for vertical movement.

According to a preferred embodiment of the device according to the invention, the movable condensation chamber is arranged to move horizontally.

According to another embodiment, the induction evaporator and the condensation chamber are tightly interconnected by means of a steam line containing primary and secondary water coolers.

According to a particularly preferred embodiment of the device according to the invention, the secondary water cooler is located inside the steam line in a steam stream above the condensation chamber.

It is envisaged that the steam line is connected to the supply pipe of the protective (inert) gas and that the protective (inert) gas circulates through the steam pipe and the supply pipe, while the vaporous manganese can be separated using a secondary condenser belonging to the supply pipe, and the protective (inert) gas again fed through the inlet pipe to the induction evaporator and, therefore, into the steam stream. At the same time, it is envisaged that an additional inert gas could be supplied to the circuit through the make-up supply to make up for losses caused by the process and thus to control the concentration inside the circulation system.

To maintain as constant a concentration of protective (inert) gas in the circuit as possible, additional protective gas can be supplied through the feed line to the supply pipe, from which, having passed the secondary filter, it can again enter the induction evaporator.

Below, an apparatus according to the invention for carrying out the method according to the invention is explained in more detail using an exemplary embodiment with reference to the attached drawing.

In this case, figure 1 shows:

FIG. 1 is a schematic diagram of a device for implementing the method, a model of the process.

As shown in figure 1, the device 18 essentially contains an induction evaporator 1, inside of which is loaded FeMn at a temperature of 1600-1700 ° C in a liquid state of aggregation. According to this embodiment, the induction evaporator 1 is placed on a hydraulic platform 9, allowing it to be raised and lowered.

At the bottom of the induction evaporator 1, it is provided that at least one connecting element 19 for the purge pipe is connected to the supply pipe 15, through which the protective gas, in this case argon, enters the induction evaporator 1. Through the FeMn melt, the protective gas rises, where, together with the evaporated fraction of manganese, it is collected at a pressure of 100-200 mbar in the steam line 14 and then discharged in the form of a vapor stream 17 shown by the arrow. While the steam line 14 is hermetically connected with the induction evaporator 1.

The steam stream 17 located in the steam line 14 passes by the primary water cooler 4, covering the steam pipe outside, and is cooled. In the secondary water cooler 5, the steam stream 17 is cooled so much that the aggregate state of manganese changes from gaseous to liquid. In order to ensure this as efficiently and as quickly as possible, an arrangement of the secondary water cooler 5 inside the steam line 14 in the steam stream 17 is provided.

At the same time, the secondary water cooler 15 is conical in shape and its tapering side is oriented towards the incoming steam stream 17. In the figure it is depicted as an isosceles triangle.

A horizontally movable condensation chamber 2 is arranged under the secondary water cooler 15. In addition, the condensation chamber 2 can be hermetically connected to the steam line 14.

Condensed high-purity manganese is collected in a horizontally mobile condensation chamber 2 and maintained at a temperature of 1350-1400 ° C in a liquid state of aggregation.

The movable condensation chamber 2 is equipped with a siphon groove 13. Through this groove 13 manganese is released and fed to the filling machine 8. The filling machine is divided into chambers and is also in the atmosphere 7 of the protective gas (argon) and equipped with the appropriate technical means to create and maintain shielding gas atmosphere. In a filling machine, manganese is cast into the target product 11 of the appropriate desired format. Target product 11 consists of manganese with a purity of 99.9%.

While the manganese-containing vapors in the vapor stream 17 are condensed by a secondary water cooler 5, the protective atmosphere gas is sucked out through the outlet 20 by means of a vacuum pump 3 and again fed into the supply pipe 15. The evaporated manganese still contained in the protective gas is cooled in the secondary condenser 12 and is separated from the protective atmosphere. For this, the secondary condenser 12 is equipped with a vacuum pump and a water cooler 6.

The shielding gas purified from manganese vapor is circulated through the supply pipe 15 and through the feed supply 16 and the secondary filter 10 again enters the induction evaporator. Through the supply line 16, the protective gas again enters the circuit to compensate for its losses during the process, as a result of which a stable atmosphere from argon is constantly maintained as a protective gas.

List of items

1 induction evaporator

2 condensation chamber

3 vacuum pump

4 primary water cooler

5 secondary water cooler

6 vacuum pump with water cooling system

7 argon protective atmosphere

8 filling machine

9 hydraulic platform

10 secondary filter

11 target product

12 secondary capacitor

13 year old

14 steam line

15 inlet pipe

16 make-up feed

17 steam flow

18 device

19 purge pipe connector

20 conclusion

Claims (13)

1. A method of producing technically pure manganese by evaporation of carbon-containing ferromanganese in an induction vacuum installation, characterized in that a container with liquid carbon-containing ferromanganese is placed in an induction evaporator (1), the pressure is regulated in the range of 10-900 mbar using a system (3) of vacuum pumps and a filter systems (10), carry out the evaporation of manganese at a temperature above the liquidus temperature of manganese 1248 ° C and purge it with an inert gas, cool the resulting manganese vapor in a hermetically sealed When a steam line is connected with an induction evaporator and a movable condensation chamber, manganese vapors are collected in a movable condensation chamber (2) at a temperature of 1350 to 1400 ° C in a liquid state of aggregation and continuously discharged from the chamber (2) through a siphon heater to a filling machine (8 ) and cast into the target product (11). 2. The method according to p. 1, in which the condensation of manganese vapor is carried out continuously using a secondary water cooler (5) located in the steam stream inside the steam pipe and having a conical shape to improve the flow of droplets into the chamber (2). 3. The method according to p. 1, in which the evaporation process is supported by argon as an inert gas, which forms an atmosphere of a protective gas. 4. The method according to p. 1, in which technically pure manganese is continuously cooled with water, discharged from the chamber (2) and supplied in a protective gas atmosphere from argon to a filling machine (8). 5. The method according to p. 1, in which the evaporation rate of manganese is controlled by temperature, the degree of vacuum in the capacity of the induction evaporator and the inert gas flow rate. 6. The method according to p. 1, in which the evaporated carbon-containing ferromanganese has a different concentration of manganese. 7. The method according to p. 6, in which the evaporated carbon-containing ferromanganese is continuously or periodically loaded into an induction evaporator (1). 8. An induction vacuum installation for producing technically pure manganese by vaporizing carbon-containing ferromanganese according to any one of claims 1 to 7, characterized in that it contains an induction evaporator (1) for liquid carbon-containing ferromanganese, a movable condensation chamber (2) for collecting manganese vapor and maintaining manganese at a temperature from 1350 to 1400 ° C in a liquid state of aggregation, while the induction evaporator and the movable condensation chamber (2) are hermetically connected to each other by a steam line (14) To cool manganese vapors by means of a primary water cooler (4), covering the steam pipe outside, and a secondary water cooler (5) located inside the steam pipe in the steam stream above the chamber (2), the chamber (2) has a siphon heated coil for continuous technical discharge Pure Manganese In A Filling Machine. 9. The device according to claim 8, in which the vacuum pump system is additionally equipped with a secondary water cooling system (6), a condenser (12) and a filter (13). 10. The device according to claim 8, in which the induction evaporator (1) is mounted on a hydraulic platform (9), made with the possibility of vertical movement. 11. The device according to claim 8, in which the movable condensation chamber (2) is made with the possibility of horizontal movement. 12. The device according to claim 8, in which the steam line (14) is connected to the inlet pipe (15) for supplying the purified inert gas to the induction evaporator (1) for re-circulation in the installation circuit, while the inlet pipe (15) has a secondary condenser (12) for purification of inert gas from manganese vapor, which is equipped with a primary filter and a vacuum pump with a water cooling system. 13. The device according to p. 12, in which the inlet pipe (15) has a supply (16) of make-up and a secondary filter (10) for supplying purified inert gas to the installation circuit to provide a stable protective atmosphere from argon during the evaporation process, while (16) make-up is also designed to supply additional inert gas to the installation circuit to make up for losses caused by the process and to control the concentration of gas inside the circulation system.

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