Method of heating reaction mix in production of metal salts and device to this end

FIELD: metallurgy.

SUBSTANCE: proposed method comprises heating the reaction mix in assembly consisting of two units composed of heaters and bubblers. Every of said unit is heated in turns to boil the solution and to direct live steam to bubbler of another unit. Proposed device represents the assembly consisting of two units composed of heaters and bubblers and integrated in a system by steam-gas pipelines. Note here that one pipeline is connected with bubblers while another one is connected with atmosphere. Shutoff valves and auxiliaries are fitted between units and pipelines. Proposed device may comprise shutoff valves automatic changer-over devices and their control unit.

EFFECT: maximum application of live steam heat, optimised thermal and hydrodynamic conditions, lower costs.

4 cl, 2 dwg, 3 ex

 

The invention relates to a method of heating the working masses in the process of obtaining metal compounds, and device for its implementation.

Obtaining metal compounds (salts, acids, basic salts) as a rule, is carried out by chemical dissolution (etching) of metals in solutions of acids or salts. Chemical etching of metals in acids is carried out, for example:

- obtaining of copper sulfate from copper and sulfuric acid;

- obtaining of silver nitrate of silver and nitric acid;

- obtaining of hexachloroplatinic acid by dissolving platinum in Aqua Regia;

Basic salts in some cases is produced by the interaction of metals with solutions of salts. So, getting oxychloride carried out by reacting aluminum metal with a solution of aluminium chloride.

All these processes are characterized by long duration (from several hours to several days), accompanied by the release of gases and, as a rule, require heating up to the maximum possible in betablocking the conditions of a temperature of the boiling point of the solution. Economic and technological efficiency of the processes of obtaining compounds of metals is largely determined by the method of heating the working masses.

As direct sources of heat for nahrawan the solutions in the processes and apparatuses of chemical technology use flue gases, or electrical energy. The most common heating electric resistance /Kasatkin A.G. Basic processes and apparatus of chemical technology M: Alliance, 2009,, s/. The disadvantage of the use of electricity for heating is the relative high cost of electricity.

To transfer heat to the heated medium is widely used intermediate fluids are water vapour, hot water, high temperature heat transfer fluids (mineral oils, organic liquids, molten salts and other). Most commonly used heating agent is water vapor. Common hollow steam heated, transferring heat through the wall of the heat exchanger /A. Kasatkin, the Basic processes and apparatus of chemical technology M: Alliance, 2009, s/. The disadvantage is unproductive consumption of steam associated with the departure of part of the steam condensate (so-called span pairs).

The known method of heating solutions with live steam, which is injected directly into the heated liquid /Kasatkin A.G. Basic processes and apparatus of chemical technology M: Alliance, 2009, s/. Enter direct steam through the bubblers - pipes located at the bottom of the device. This method of heating allows better use of the heat of the steam, as steam condensate is mixed with the heated fluid and temperature virainia the tsya. The disadvantage is the dilution of the heated medium steam condensate.

The closest analogue is the method of heating the reaction mixture in the process of obtaining metals by dissolution of metals at the boiling temperature with the formation of steam. (F. Habashi, fundamentals of applied metallurgy, Vol.2, M., metallurgy, 1975, p.23-43). It is impossible to regulate the heating process, high energy consumption and loss solution.

The objective of the invention is to develop a method of heating the working masses, to ensure maximum use of the heat of steam without dilution of the heated medium, and device for its implementation.

The problem is solved by the proposed method of heating the reaction mixture in the process of obtaining metal compounds by dissolving metals to the boiling temperature with the formation of steam, the difference is that heat when dissolving is carried out in a system of two devices equipped with heaters and bubblers, each of the two devices alternately heated by the heaters to heat the reaction mixture, bring the solution to kiberia and the resulting steam is directed into the bubbler other apparatus with stopping any heating of the reaction mixture heater.

The discharge of exhaust steam is carried out on the apparatus heated by direct steam.

Periodically switch: in odd-numbered cycles of the first device is heated by the heater, and the second live steam coming from the first apparatus; in even-numbered cycles, on the contrary, the second device is heated by the heater, and the first acute ferry.

Switching is carried out at set intervals, or upon reaching a given level of solution in one of the units or upon reaching a predetermined temperature of the solution. It is preferable to perform switching in automatic mode using a time relay or automatic level control or temperature solutions.

Also proposed a device for heating the reaction mixture in the process of obtaining metal salts, including apparatus with a heater, the difference of which is that it contains two apparatus, equipped with heaters and bubblers, and the devices connected to the system piping for steam and exhaust steam, and piping for sharp pair connected with bubblers, piping for exhaust steam from the atmosphere, and between the apparatus and piping, install isolation valves for controlling the release of steam.

Preferably, the device may contain elements of automatic switching valves, and a control unit for the automatic switched the I valves.

Can be used any known method of heating apparatus - an electric current, a hollow steam and other

Figure 1 presents the scheme of the device.

The device contains two devices 1 and 2, provided with a heater 3 and 4 and bubblers 5 and 6. The pipeline sharp pair 7 with installed valves 10 and 11 is connected to the bubblers, the exhaust vapor 8 with installed valves 9 and 12 with the atmosphere.

The device operates as follows.

When closed and valves 9 and 11 and open the valves 10 and 12 include a heater 3 heater 4 is turned off). Heat the solution in the apparatus 1 to the boiling point. Formed in the unit 1 steam through the pipe 7 enters the bubbler 6 heating apparatus 2. Proven gas-vapor mixture is removed from the apparatus 2 to line 8.

Then make the switch. Turn off the heater 3, a heater 4, open the valves 9 and 11, close the valves 10 and 12, heat the solution in the apparatus 2 to the boiling point. Formed in the unit 2 steam through the pipe 7 enters the bubbler 5 on the heating apparatus 1. Proven gas-vapor mixture is removed from the apparatus 1 via line 8.

This process periodically (cyclically) repeat. In odd-numbered cycles of steam from the apparatus 1 enters the apparatus 2, in even-numbered cycles of steam and the apparatus 2 enters the apparatus 1. The steam evaporates and condenses mainly within the system of the two devices, moving from device to device and back. The total number of circulating water in the device remains almost unchanged. If necessary, resulting in a small number of migrating vapor can condense and return the water into the machine.

Figure 2 shows the option of using steam heaters (heating of hollow steam through the jacket of the device), providing for automatic adjustment by transmitting signals from the level sensors of the reaction mixture on the control unit valves (lines transmitting signals from the control unit to the actuator is not specified).

The list of positions of figure 2

1, 2 - devices

3, 4 - bubblers,

5 is a control block

LI-1, LI-1 - level sensors,

XV-1...XV-10 - valves.

The regulation algorithm: at the lower level of the reaction mixture in the apparatus 1 to the limit value, the signal from the sensor LI-1 is supplied to the control unit, where the actuator signal: valve XV-1, XV-5 XV-9 XV-4 XV-8 - close, XV-3, XV-7 XV-2, XV-6 XV-10 - open.

Similarly, by decreasing the level of the reaction mixture in the apparatus 2 to the limit value, the control unit receives the signal from the sensor, LI-2, after which the actuator signal: valve XV-1, XV-5 XV-9 XV-4 XV-8 - open, XV-3, XV-7 XV-2, XV-6 XV-10 - closing the ü.

The essence of the invention is illustrated by the following examples.

Example 1

The process of obtaining silver nitrate from silver metal and nitric acid in the proposed system for heating the working masses.

Etching of silver in nitric acid proceeds according to the reaction:

3Ag+4HNO3=3AgNO3+NO↑+2H2O

Etching of silver is carried out in a system of two units with a capacity of 160 liters Apparatus provided with steam jackets, germetiziruyushchimi caps, bubblers and pipes for gas-vapor mixture, of One of the pipes (piping steam) is connected with bubblers, and the second exhaust pair) - with the atmosphere. Between the apparatus and piping, install isolation valves.

In the load devices over standard metal ingot silver GOST 28595 mass (30±2) kg, pour in 25 liters of distilled water and 25 l (35 kg) nitric acid (HC, density 1.4).

First, both apparatus a hollow steam heated, with exhaust steam is discharged. After reaching the boiling point stop the supply of steam to the jacket of the second apparatus, direct steam, generated in the first device, the second bubbler apparatus and lead the process of etching silver on the proposed method.

Periodically (1 every 30 min) switch: the odd cycles of the first device is heated hollow steam, and the second live steam coming from the first apparatus; in even-numbered cycles, on the contrary, the second device is a hollow steam heated, and the first acute ferry. Switching is carried out in automatic mode by means of valves.

The discharge gas mixture is carried out of the apparatus, heated with live steam. Gas-vapor mixture for neutralization of the emitted oxides of nitrogen is passed through the adsorption column with a solution of urea.

After complete dissolution of silver resulting solution was diluted with distilled water and filtered on a vacuum filter. The filtrate is evaporated to form a crystalline film and cool. The precipitated crystals of silver nitrate sucked off on a vacuum filter, the mother liquor together with the washing water evaporated and crystallized as described above. Both factions crystals are mixed and dried at 110°C in the drying oven. The finished product is Packed for shipment to consumers.

The main technological parameters of the etching process:

duration - 4 hours

- the consumption of nitric acid - 35 kg

- loss of silver with ventilation emissions - 0.3 g

- the emission of nitrogen oxides into the atmosphere - 0.25 kg

Example 2 (comparative)

The process of obtaining silver nitrate from silver metal and nitric acid is when you go to traditional hardware design.

Etching of silver is carried out in two bowls with a capacity of 160 liters, provided with steam jackets, caps and exhaust ventilation.

To each Cup download one standard metal ingot silver GOST 28595 mass (30±2) kg, pour 50 l of distilled water, include steam heating. Then poured nitric acid-the first portion 15 l, the subsequent 5 l (every 1.5 hours). Just download 40 l (56 kg) nitric acid. The process is continued until complete dissolution of silver.

The process is conducted at operating local exhaust ventilation for removing the released nitrogen oxides. Air emissions are passed through an adsorption column with a solution of urea.

After dissolving the silver solution is filtered, the filtrate is returned to the bowl and are crystallization and drying of the product, as in example 1.

The main technological parameters of the process:

- the duration of the etching - 9 h

- the consumption of nitric acid is 56 kg

- loss of silver with ventilation emissions of 1.5,

- the emission of nitrogen oxides into the atmosphere - 3 kg

Example 3

The process of obtaining high-base oxychloride from aluminum metal and a solution of aluminium chloride in the proposed system for heating the working masses.

Obtaining high-base oxychloride, aluminium metal is lifescope and a solution of aluminium chloride is carried out in a total reaction: 10Al+2AlCl 3+30H2O=6Al2(OH)5Cl+15 NM2

The process is conducted in the system of the two devices with a volume of 6 m3. The apparatus is equipped with a steam jacket, bubblers and pipes for gas-vapor mixture, of One of the pipes (piping steam) is connected with bubblers, and the second exhaust pair) - with the atmosphere. Between the apparatus and piping, install isolation valves.

In each process cycle in both devices download metal aluminium, aluminium chloride and water in predetermined proportions. Aluminum load in the form of standard bars (ingots) of primary aluminum by weight (15±1,5) kg according to GOST 11070-74.

Each device is loaded:

- aluminum metal - 180 kg (in the first cycle is 1800 kg);

a solution of aluminum chloride aluminum chloride - 82,7 kg; water - 1500 DM3).

The amount of aluminum metal loaded in each unit at the start of the technological process (in the first cycle, 10 times more than required by the equation of the chemical reaction and is 1800 kg In each subsequent cycle consumes about 10% aluminum (180 kg), 90% of the metal remains in the apparatus as carryover. At the beginning of each cycle in the machine load bars aluminum metal in an amount corresponding to the weight of the metal used in the previous cycle. So about what atom, is maintained at a constant amount of metal in the device.

First, both apparatus a hollow steam heated, with exhaust steam is discharged. After reaching the boiling point stop the supply of steam to the jacket of the second apparatus, direct steam, generated in the first device, the second bubbler apparatus and lead the process of etching aluminum on the proposed method.

Periodically (1 x 60 min) switch: in odd-numbered cycles of the first device a hollow steam heated, and the second live steam coming from the first apparatus; in even-numbered cycles, on the contrary, the second device is a hollow steam heated, and the first acute ferry. Switching is carried out in automatic mode by means of valves.

The discharge gas mixture is carried out of the apparatus, heated with live steam. Waste gas-vapor mixture is directed into the tank for condensate through the heat exchanger, cooled by circulating water. The steam condenses in the tank, the hydrogen is discharged into the atmosphere by means of local exhaust ventilation. The condensate accumulating, return pump in the apparatus.

Upon receipt of the product, the relevant technical conditions, disable steam heating apparatus, after which the solution pump pump of the apparatus in the intermediate tank, cooled, filtrowa and pumped to the warehouse for subsequent shipment to consumers.

In the apparatus of the newly loaded aluminum metal and an aqueous solution of aluminium chloride, begin the next cycle of obtaining high-base oxychloride.

In each cycle produces about 1743 kg of highly basic solution of oxychloride of the following composition: oxide of aluminum (Al2O3) - 22,8-24,0%, chlorine (Cl) - a 7.9-8.4%, the density 1,325...1,345 g/cm3. The main technological parameters of the process:

Duration - 40 hours;

Steam consumption per 1 ton of product - 1,0 Gcal;

The flow of circulating water per 1 ton of product - 2.5 m3;

Loss of aluminum with air emissions - 0.2 kg per 1 ton of the product.

Example 4 (comparative)

The process of obtaining high-base oxychloride from aluminum metal and a solution of aluminium chloride with traditional hardware design.

The process is conducted in two units with a volume of 6 m3. Apparatus provided with steam jackets and pipelines for the discharge of exhaust steam to the atmosphere.

In each process cycle in both devices download metal aluminium, aluminium chloride and water. The number of downloaded reagents is the same as in example 3.

Both devices are hollow steam heated, with proven gas-vapor mixture is directed into the tank for condensate through the heat exchanger, cooled by circulating water. Steam cond is siruela in the vessel, the hydrogen is discharged into the atmosphere by means of local exhaust ventilation. The condensate accumulating, return pump in the apparatus, thus carry out periodic recharge condensate tap water.

The process requires a systematic monitoring and regulation, since the disturbance of the water balance of the product may crystallize on the surface of ingots of aluminum, which will lead to the termination of the etching.

Upon receipt of the product, the relevant technical conditions, disable steam heating apparatus, after which the solution pump pump of the apparatus in the intermediate tank, cooled, filtered and pumped to the warehouse. In the apparatus of the newly loaded aluminum metal and an aqueous solution of aluminium chloride, begin the next cycle of obtaining high-base oxychloride.

The result is about 1743 kg of product, which is similar to the composition of the product obtained in example 3 according to the proposed method.

The main technological parameters of the process:

Duration - 50 h;

Steam consumption per 1 ton of product - 2,0 Gcal;

The flow of circulating water per 1 ton of the product - 5 m3;

Additional consumption of tap water per 1 ton of product - 1 m3.;

Loss of aluminum with air emissions - 0.5 kg per 1 ton of the product.

The list of positions on IG

1, 2 - devices

3, 4 - heaters

5, 6 - bubblers,

7 - pipeline sharp pair

8 - exhaust vapor

9, 10, 11, 12 - valves

The proposed method of implementation of such processes has a number of significant advantages. With the alternation of modes of heating process becomes oscillatory in nature, due to this it becomes adjustable.

1) Automatically maintain constant the maximum temperature close to the boiling point. In the apparatus, which is currently heated by the heater, it slightly exceeds the boiling point of the solution at atmospheric pressure due to the fact that the pressure in the apparatus above atmospheric at the height of the water column corresponding to the height of the bubbler; the temperature in the second apparatus is approximately equal to the condensation temperature of steam.

2) Reduced energy consumption, since the heat of evaporation of a solution in one device automatically utilized through the use of the heat of condensation of steam in another device.

3) Dramatically reduces loss solution, since steam is not lost, only transferred from device to device and back, the total amount of solution in the two devices remains approximately constant. In contrast to the usual options of heating with live steam (in which the solution is highly diluted with condensate) and unlike the normal boiling temperature (at which the solution is subjected to evaporation) process can be maintained indefinitely, it is particularly important when carrying out long-term heterogeneous chemical processes.

4) is Reduced to a minimum loss of the target product with ventilation emissions, which is very important when we are dealing with expensive raw materials - metals, including precious (platinum, gold, silver).

5) In some cases, the reagents being used more weight. So, when dissolved precious metals (gold, platinum) in Aqua Regia process proceeds through the stage of formation of gaseous chlorine, which is the cascade of two devices fully "digested", i.e. dissolves more gold or platinum. Accordingly, fewer toxic gas enters the ventilation.

Improved hydrodynamic regime of the process: in one of the devices of the mixing occurs due to bubbles generated steam (and dissolved gas)in the other jet of steam applied (as well as gas received from the first device and emitted from the second device). Alternating modes ensures optimal hydrodynamics.

1. The method of heating the reaction mixture in the process of obtaining metal salts by dissolving metals to the boiling temperature with the formation of steam, characterized in that the heating when the dissolution is carried out in a system of two devices equipped with heaters and barbeau the apostrophes, each of the two devices alternately heated by the heaters to heat the reaction mixture, bring the solution to boil and the resulting steam is directed into the bubbler other apparatus with stopping any heating of the reaction mixture heater.

2. Device for heating the reaction mixture in the process of obtaining metal salts, characterized in that it is made in the form of a system of two devices equipped with heaters and bubblers, and the devices connected to the system piping for steam and exhaust steam, and piping for sharp pair connected with bubblers, and the exhaust steam from the atmosphere, and between the apparatus and piping, install isolation valves for controlling the release of steam.

3. The device according to claim 2, characterized in that it contains elements of automatic switching valves.

4. The device according to claim 2, characterized in that it comprises a control unit for automatic switching of valves.



 

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7 cl, 1 dwg

FIELD: metallurgy.

SUBSTANCE: group of inventions relates to extraction of molybdenum from acid liquors, containing mixture of nitric and sulfur acid and molybdenum in wide range of concentration and also other admixtures and can be used at regeneration of molybdenum from waste colution for etching of molybdenum cores in manufacturing of electric bulbs and electronic devices and solutions of hydrometallurgy manufacturing. Extraction of molybdenum is implemented from solutions with diferent content in it of molybdenum. Acid solution is treated by electromagnetic field with frequency selected in the area of mid-range radio waves, formed water is driven off, laid-down sediment is filtered. Extracted acid is returned into etching process. Installation includes reactor block, filtration unit, tanks for solutions, pipelines, stop and variable valves. Reactor block includes reactor, electromagnetic field generator, inductor and matching device. Inductor is located inside or outside thru reactor. Installation additionally contains rectifying still for distillation of water, direct connected to reactor.

EFFECT: increasing of extraction ratio subject to circulation of colutions, process is ecologically safe, industrial sewages are not formed.

7 cl, 1 dwg, 2 tbl, 2 ex

FIELD: metallurgy.

SUBSTANCE: invention elates to device for cyanic leaching of gold from gold-bearing materials. Device contains tank for leaching with located gold-bearing material, collapsible tank, branch pipe for discharge and withdrawal of efficient solution and branch pipe for feeding of cyanide. It is outfitted by filled by alkali reaction vessel-closed scrubber, allowing siphon pipe, gas disperser HCN D pipe for feeding of alkaline solution and branch pipe for feeding of cyanide. Device is outfitted by pipe for gas distillation HCN and its feeding into reaction vessel - closed scrubber and pipe for feeding of air oxygen into tank. Additionally tank for leaching is implemented with internal perforated wall. Into space between external and internal walls of tank it is mounted siphon pipe connected to collapsible tank. In collapsible tank it is located system for solution blending branch pipe for discharge and withdrawal of efficient solution and gage tank for feeding of inorganic acid.

EFFECT: increasing of leaching speed of gold and improvement of environmental protection.

5 cl, 1 dwg

FIELD: metallurgy.

SUBSTANCE: method includes heating of kyanite to 1250-1350°C. At the same time kyanite prior to heating is mixed with solid carbon at the weight ratio from 1:0.37 to 1:1.85. Heating is carried out in atmosphere of halogen-containing gases. Produced halogenides are cooled and separated, afterwards a mixture is prepared from them with required content in the product of aluminium, silicon and other chemical elements available in kyanite. Then the mixture of halogenides is heated either in atmosphere of oxygen with production of complex oxides or in recovery atmosphere with production of alloys.

EFFECT: complex wasteless processing of kyanite concentrate.

5 cl, 4 ex

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