A condensing and refining integrated device and method for continuous magnesium smelting

Abstract

A kind of condensation and refining integrated device and method for continuous magnesium smelting belong to pyrometallurgy field.The present application precisely controls condensation temperature by setting controllable temperature condensing plate, ensures that magnesium vapor can be condensed into liquid magnesium efficiently and drop smoothly to be collected, realizes the automation control from crude magnesium collection to refining process by the synergistic work of light signal sensing device, current signal sensor and refining chamber piston push rod etc., improves production efficiency and the stability of product quality.Meanwhile, in the refining process, the present application stirs crude magnesium liquid and refining agent by high-temperature-resistant eccentric stirring paddle, so that they are fully mixed, and the refining effect is improved.When refining is carried out by the device provided by the present application, refining slag can be discharged in time, so as to avoid interference to the refining process, and the quality of refined magnesium after removing impurities is high, which meets the needs of industrial production.

Description

TECHNICAL FIELD

[0001] The present application belongs to the field of pyrometallurgy, and particularly relates to a condensation and refining integrated device and method for continuous magnesium smelting. BACKGROUND

[0002] In recent years, with the development of non-ferrous metal field, the demand for magnesium and its alloy gradually increases. Especially, magnesium-aluminum alloy is widely used in the field of civil vehicles and aerospace due to its lightweight, excellent physical properties and good mechanical processing performance. At present, the annual production of raw magnesium in the world is about 1 million tons, and the annual production of raw magnesium in China accounts for more than 80%, which is a real big country of raw magnesium smelting, and also the country with the highest magnesium resource reserves. With the proposal of green smelting requirements, the disadvantages of high energy consumption and large carbon emissions of the existing raw magnesium smelting process seriously restrict the further development of raw magnesium production.

[0003] The production process of raw magnesium in China is mainly concentrated in Fugu, Yulin, Nanjing Yunhai Group, Shanghai Baosteel Group, etc., and the production process adopts the small investment and fast construction of the Pidgeon process of silicon hot magnesium smelting process. The heat transfer mode of this process is single heat transfer, and it is very common to set a long time in the reduction stage, and the balling process of high-temperature calcined white cooling to room temperature also causes great energy waste. The relative vacuum continuous magnesium smelting process proposed by Zhang Tingan team of Northeast University provides a new way for green continuous smelting of raw magnesium [1]~[3] . The process improves the heat transfer mode to the form of heat transfer and heat convection coupling, greatly shortens the time required for reduction reaction, from 10-14 hours to 1-1.5 hours. And the balling process adopts direct balling of magnesium-containing raw ore, which avoids the energy loss of high-temperature calcined white, and the innovative process reduces the energy consumption of per ton of magnesium by more than 30% and the carbon emission by more than 43%. However, in the process of industrialization promotion, although this way has good energy saving and emission reduction effect, the flowing carrier gas destroys the process of free diffusion and crystallization of magnesium vapor particles to the condensation plate, and only powder crystalline magnesium can be collected. This problem is a problem that needs to be solved in the process of industrialization of the process.

[0004] In recent years, Chinese researchers have conducted a large number of studies on condenser equipment. Patent CN117488071A discloses a closed rotary furnace for continuous magnesium smelting and its use method, mainly including: a closed rotary furnace, a heating kiln body and a condensing device. The mixed gas of magnesium vapor and inert gas generated during the heating process is condensed to produce liquid magnesium. Although it can greatly shorten the magnesium smelting period and realize efficient utilization of heat. But the collected magnesium will still crystallize in powder form, and the nucleation and growth conditions of magnesium vapor are poor. Patent CN117488072A discloses a method and device for continuous magnesium smelting and co-production of refining agent in a relative vacuum, which points out a scheme for continuous magnesium smelting and co-production of refining agent in a relative vacuum. The invention mainly includes: a sealed furnace body, a track conveying device, a calcination zone heating gun, a reduction zone heating gun, a condenser and a negative pressure conditioning furnace. This method and device realize continuous magnesium smelting of low-grade magnesite and dolomite, and co-produce refining agent while producing metal magnesium, solving the problem of the current reduction tailings that cannot be utilized from the source of the process, but the problem of powder crystallization of magnesium vapor has not been solved.

[0005] In summary, the existing relative vacuum continuous magnesium smelting condensation process does not have the conditions for large size grain nucleation and growth, and the subsequent refining process needs to reheat the crude magnesium, causing secondary waste of energy.

[0006] Document [1] Han J, Fu D, Guo J, et al. Nucleation and Condensation of Magnesium Vapor in Argon Carrier[J]. Metals, 2020, 10(11): 1441.

[0007] Document [2] Li R B, Zhang S J, Guo L J, et al. Numerical study of magnesium (Mg) production by the Pidgeon process: Impact of heat transfer on Mg reduction process[J]. International Journal of Heat and Mass Transfer, 2013, 59: 328-337.

[0008] Document [3] Fan B guo, Jia L, Han F, et al. Study on magnesium slag desulfurizer modified by additives in quenching hydration[J]. Journal of Material Cycles and Waste Management, 2019, 21(5): 1211-1223. SUMMARY

[0009] The purpose of the present application is to solve the problems of magnesium vapor powder condensation, high energy consumption and large carbon emissions in subsequent crude magnesium refining, and to provide a condensation and refining integrated device and method for continuous magnesium smelting in relative vacuum. The present application realizes the liquid condensation of magnesium vapor through a specific process and device, and achieves the integrated continuous operation of condensation and refining, reduces energy consumption and carbon emissions, and reduces environmental pollution.

[0010] To achieve the above purpose, the technical solution adopted by the present application is:

[0011] A condensation and refining integrated device for continuous magnesium smelting, comprising a refining system and a condensation system, the refining system being adjacent to the condensation system and being connected through a non-return valve II arranged above the system wall and a non-return valve I arranged at the bottom of the system wall.

[0012] The condensation system comprises a condensation zone, a crude magnesium liquid collection zone, a magnesium slag discharge zone and an argon gas discharge zone. The refining system comprises a magnesium liquid refining zone and a system pressure control zone, and the system pressure control zone is arranged above the magnesium liquid refining zone.

[0013] The crude magnesium liquid collection zone is located at the bottom of the condensation system, and the condensation zone is located directly above the crude magnesium liquid collection zone. The magnesium slag collection zone and the crude magnesium liquid collection zone are separated by a magnesium slag overflow weir. The argon gas discharge zone is arranged above the magnesium slag discharge zone. The mixed gas inlet is arranged at a relative position of the argon gas discharge zone.

[0014] The magnesium liquid refining zone is provided with a refining chamber and a high-temperature-resistant eccentric stirring paddle at the bottom. The high-temperature-resistant eccentric stirring paddle is inserted into the refining chamber from the side wall of the refining chamber. The bottom of the refining chamber is provided with a non-return valve I and a refined magnesium liquid outlet at a relative position. The system pressure control zone is provided with a refining chamber piston push rod. The refining agent adding port is arranged at the center of the bottom of the refining chamber piston push rod. The light signal sensor is arranged above the refining agent adding port. The bottom of the system pressure control zone is higher than the non-return valve II.

[0015] The non-return valve I is provided with a current signal sensor above the side close to the crude magnesium liquid collection zone.

[0016] The condensing area is provided with a temperature-controllable condensing plate which is fixed in the condenser shell by welding; the temperature-controllable condensing plate comprises a condensing plate body, a flow baffle body and a silicon-molybdenum rod; three flow baffle bodies are arranged in staggered manner perpendicular to the condensing plate body, and the magnesium vapor passes through the flow baffle bodies in a flow state; 5-10 silicon-molybdenum rod insertion openings are arranged in a single row and uniformly at the position opposite to each flow baffle body, and the silicon-molybdenum rod passes through the silicon-molybdenum rod insertion opening and is fixed in the flow baffle body;

[0017] The bottom of the magnesium slag discharge area is provided with a magnesium slag discharge outlet; the argon gas discharge area is provided with an argon gas outlet piston push rod through the argon gas outlet piston push rod insertion opening;

[0018] The height of the magnesium slag overflow weir is 5%-15% of the total height of the condenser; the check valve I and the check valve II are one-way check valves with the same structure.

[0019] A condensing and refining integrated method for relative vacuum continuous magnesium smelting is realized by using the above device, and comprises the following steps:

[0020] Step 1: mix the magnesium-containing raw ore, the reducing agent and the fluxing agent according to the set mass ratio to obtain pellets;

[0021] Step 2: send the pellets to the reduction tank to perform calcination and reduction integrated operation to generate magnesium vapor, introduce the carrier gas into the reduction tank, and the magnesium vapor enters the condenser through the high-temperature-resistant alloy material pipeline;

[0022] Step 3: the magnesium vapor condenses into liquid magnesium on the surface of the temperature-controllable condensing plate, and drops to the lower coarse magnesium liquid collection area to be collected, so as to obtain coarse magnesium liquid and covering slag;

[0023] Step 4: when the height of the magnesium liquid and the covering slag in the coarse magnesium liquid collection area reaches 5%-15% of the total height of the condensing system, the magnesium liquid refining chamber piston push rod moves upward, the magnesium liquid is sucked into the magnesium liquid refining area, and the refining agent is automatically added; after standing, the high-temperature-resistant eccentric stirring paddle mixes and stirs the coarse magnesium liquid and the refining agent to obtain fine magnesium liquid and refining slag;

[0024] Step 5: when the height of the fine magnesium liquid and the refining slag in the magnesium liquid refining area reaches 85%-90% of the total height of the magnesium liquid refining area, the magnesium liquid refining chamber piston push rod moves downward, and the refining slag is discharged from the upper check valve II to the coarse magnesium liquid collection area. When the total mass of the fine magnesium liquid and the refining slag in the magnesium liquid refining area reaches 7%-17% of the mass of the raw material, the magnesium liquid refining chamber piston push rod stops circulating work, the fine magnesium liquid is discharged from the fine magnesium liquid discharge outlet, and the refining slag enters the coarse magnesium liquid collection area. In the coarse magnesium liquid collection area, as the magnesium vapor continuously condenses into liquid magnesium and drops into the coarse magnesium liquid, the covering slag at the top of the coarse magnesium liquid overflows the magnesium slag overflow weir and is discharged from the magnesium slag discharge outlet; when the current signal sensor displays that the mass of the coarse magnesium liquid and the covering slag reaches 7%-17% of the mass of the raw material, the magnesium liquid refining chamber piston push rod starts the circulating work, and the above refining process is repeated.

[0025] In step 1, the magnesium-containing raw ore at least comprises dolomite and magnesite; the reducing agent comprises but is not limited to one or a mixture of several of ferrosilicon, aluminum scrap, biomass carbon; and the fluxing agent comprises but is not limited to fluorite or CaF2;

[0026] In step 1, the magnesium-containing raw ore at least comprises dolomite and magnesite; the reducing agent comprises but is not limited to one or a mixture of several of ferrosilicon, aluminum scrap, biomass carbon; and the fluxing agent comprises but is not limited to fluorite or CaF2;

[0027] In step 2, the calcination temperature is 900-1050 DEG C, the calcination time is 1-3 h, the reduction temperature is 1250-1350 DEG C, and the reduction time is 1-3 h;

[0028] The carrier gas is an inert gas, and the carrier gas flow rate is 0.1 m 3 / h-2.5 m 3 / h;

[0029] In step 3, the controllable temperature condensing plate surface temperature is 750-850 DEG C;

[0030] In step 4, when the magnesium liquid in the crude magnesium liquid collection area reaches 5-15% of the total height of the condenser, the piston rod of the refining chamber moves upward, the crude magnesium liquid in the condenser is sucked into the magnesium liquid refining area through the check valve I, when the crude magnesium liquid is sucked into the refining chamber, the valve core of the check valve I is in an open state, the current signal sensor is interrupted, the refining agent is added into the magnesium liquid refining area through the refining agent adding port, and meanwhile, the light signal sensor adjusts the high-temperature-resistant eccentric stirring paddle to start working and perform refining.

[0031] The current signal sensor is located on the side wall of the valve body of the check valve I, detects the working state of the check valve I through an electric signal, and is externally connected to a test electric signal on-off;

[0032] The refining agent is added in an inductive manner, the light signal sensor is located above the refining agent inlet, and the refining agent is added when the piston rod of the refining chamber moves upward and exceeds the position of the refining agent inlet;

[0033] The standing time is 1-10 s.

[0034] Compared with the prior art, the present application has the following beneficial effects:

[0035] 1. The application provides a device and method for condensation and refining integration of relative vacuum continuous magnesium smelting, which mixes magnesium-containing raw ore (such as dolomite, magnesite, etc.), reducing agent (such as silicon iron, aluminum scrap, biomass charcoal, etc.), fluxing agent (such as fluorite, CaF2 reagent, etc.) according to a specific ratio, and after calcination and reduction integration operation, magnesium vapor is condensed into liquid magnesium on a controllable temperature condensing plate and collected, and subsequent refining is performed. The application solves the problem of powdered condensation of magnesium vapor in the existing relative vacuum continuous magnesium smelting process, realizes condensation and refining integration continuous operation, and the reduction slag generated in the production process can be treated and utilized separately, reducing resource waste.

[0036] 2. The application precisely controls the condensation temperature at 750-850 DEG C through the controllable temperature condensing plate, so as to ensure that the magnesium vapor can be efficiently condensed into liquid magnesium and smoothly drip and collect. The automatic control from the crude magnesium collection to the refining process is realized through the cooperative work of the light signal sensing device, the current signal sensor and the refining chamber piston push rod. The application can automatically adjust the operation according to the state of the magnesium liquid and the refining slag, and improve the production efficiency and the stability of the product quality.

[0037] 3. The condensation and refining integration device of the application has reasonable design, and in the refining process, the crude magnesium liquid and the refining agent are stirred by the high-temperature-resistant eccentric stirring paddle, so that the two are fully mixed, and the refining effect is improved. The refining slag can be discharged in time, so as to avoid interference on the refining process, the refined magnesium after impurity removal has high quality, and meets the industrial production demand. Meanwhile, the device can realize continuous production, the production efficiency of magnesium is improved by 8-17%, and the production cost is reduced. BRIEF DESCRIPTION OF DRAWINGS

[0038] Figure 1 It is a schematic view of the condensation and refining integration device for continuous magnesium smelting of the application;

[0039] Figure 2 It is a structure schematic view of the controllable temperature condensing plate;

[0040] Figure 3 It is a top view of the controllable temperature condensing plate;

[0041] Figure 4 It is a left view of the controllable temperature condensing plate;

[0042] Figure 5 It is a B-B sectional view of the controllable temperature condensing plate;

[0043] Figure 6 It is a schematic view of the valve body of the one-way check valve;

[0044] Figure 7 It is a side view of the valve body of the one-way check valve;

[0045] Figure 8 It is a schematic view of the valve core of the one-way check valve;

[0046] Figure 9 Valve core side view of one-way check valve;

[0047] Wherein, 1-mixed gas inlet, 2-rough magnesium liquid collection area, 3-magnesium slag discharge area, 4-magnesium liquid refining area, 5-argon discharge area, 6-magnesium slag discharge outlet, 7-controllable temperature condensing plate, 8-check valve I, 9-argon outlet piston push rod, 10-refining chamber piston push rod, 11-high-temperature-resistant eccentric stirring paddle, 12-magnesium slag overflow weir, 13-condensing plate main body, 14-argon outlet piston push rod insertion port of the baffle main body, 15-silicon molybdenum rod insertion port, 17-check valve II, 18-fine magnesium liquid outlet, 19-current signal sensor, 20-refining agent adding port, 21-optical signal sensor. DETAILED DESCRIPTION

[0048] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application is further described in detail below in combination with the drawings and examples. It should be understood that the specific examples described herein are only used to explain the present application and do not limit the present application.

[0049] The present application provides a condensing and refining integrated device for continuous magnesium smelting, which comprises two functional areas in total, i.e. a magnesium vapor condensing system and a refining system. The magnesium vapor condensing system obtains rough magnesium liquid, and the refining system is provided with a high-temperature-resistant eccentric stirring paddle. The whole of the two systems is a welded part, and the communication between the two systems is realized by two check valves arranged on the system wall. The lower check valve I is responsible for inhaling the rough magnesium liquid into the refining chamber, and the upper check valve II is responsible for discharging the refining slag to the magnesium vapor collection area.

[0050] The device provided by the present application further comprises a controllable temperature condensing plate at the top of the rough magnesium liquid collection area. The controllable temperature condensing plate is composed of a condensing plate main body, a silicon molybdenum rod and a baffle main body. The plate body of the condensing plate is a hole structure corresponding to the uniformly distributed silicon molybdenum rod insertion ports of the baffle main body. The silicon molybdenum rod is inserted into the silicon molybdenum rod insertion ports of the plate body and is fixed in the baffle main body by insertion. The position of the silicon molybdenum rod exposed to the plate body is clamped and electrified by an aluminum sheet at the tail of the silicon molybdenum rod, and then heated to 750-850 DEG C, so as to ensure that the magnesium vapor is condensed into liquid phase.

[0051] The application provides a condensation and refining integrated device for relative vacuum continuous magnesium smelting, which comprises a crude magnesium liquid collecting area, a refining area, a controllable temperature condensing plate, a refining chamber piston push rod, a one-way check valve, a high-temperature-resistant eccentric stirring paddle, a current signal sensor and a light signal sensing device. The controllable temperature condensing plate body can accurately control the condensing temperature, thereby providing good conditions for the condensation of magnesium vapor. The refining chamber piston push rod realizes efficient operation of absorbing the molten liquid magnesium into the refining chamber and discharging the refining slag to the collecting chamber through reciprocating motion combined with the one-way valve. The high-temperature-resistant eccentric stirring paddle is made of high-temperature-resistant material, and the unique eccentric design can fully mix the crude magnesium liquid and the refining agent, thereby increasing the refining efficiency by 8% to 17%. The current signal sensor and the light signal sensing device monitor the height and mass change of the magnesium liquid and the refining slag in the crude magnesium liquid collecting area and the magnesium liquid refining area, thereby providing reliable data support for automatic control.

[0052] The application also provides a condensation and refining integrated method for relative vacuum continuous magnesium smelting, which is realized by using the above device and comprises the following steps.

[0053] Step 1, mix the magnesium-containing raw ore (including but not limited to dolomite and magnesite), the reducing agent (including but not limited to silicon iron and aluminum scrap) and the fluxing agent (including but not limited to fluorite and CaF2 reagent) in a proportion to obtain pellets; when the reducing agent is silicon iron, the proportion is set as dolomite:magnesite:reducing agent:fluxing agent=(6.0-6.6):(6.4-6.6):(1.4-1.8):(0.2-0.6).

[0054] Step 2, send the prepared pellets to the reduction tank for calcination and reduction integrated operation, and let the magnesium vapor generated by reduction pass through the high-temperature-resistant alloy pipe with a five-layer structure (from inside to outside, the inner layer of high-temperature-resistant alloy pipe, the refractory cement layer, the refractory brick broken filler coating layer, the asbestos insulation layer and the outer layer of high-temperature-resistant alloy pipe) into the condenser.

[0055] Step 3, the magnesium vapor enters the inside of the condenser through the check valve, condenses into liquid magnesium on the surface of the controllable temperature condensing plate with the surface temperature kept at 750-850 DEG C, and then drops to the lower crude magnesium liquid collecting area for collection, thereby obtaining the crude magnesium liquid and the covering slag.

[0056] Step 4, when the crude magnesium liquid and the covering slag reach 5%-15% of the total height of the condensation system, the refining chamber piston push rod moves upward to absorb the molten liquid magnesium into the refining chamber and automatically add the refining agent. After the refining agent is added and kept still for 1-10 s, the crude magnesium liquid is mixed and stirred with the refining agent by using the high-temperature-resistant eccentric stirring paddle for 10-20 min, thereby obtaining the refined magnesium liquid and the refining slag.

[0057] Step 5, when the height of the refined magnesium liquid and the refining slag in the refining chamber reaches 85% to 90% of the total height of the magnesium liquid refining zone set by the light signal sensor, the refining chamber piston push rod moves downward, and the refining slag is discharged from the upper non-return valve II to the crude magnesium liquid collection zone. When the total mass of the refined magnesium liquid and the refining slag in the refining chamber reaches 7% to 17% of the mass of the raw material, the refining chamber piston push rod stops circulating work. The refined magnesium liquid is discharged from the refined magnesium liquid discharge port, and the refining slag enters the crude magnesium liquid collection zone. In the crude magnesium liquid collection zone, as the magnesium vapor continues to condense into liquid magnesium and drop into the crude magnesium liquid, the covering slag at the top of the crude magnesium liquid will overflow the magnesium slag overflow weir with a height of 5% to 15% of the total height of the condenser, and be discharged from the magnesium slag discharge port. When the current signal sensor at the bottom of the collection chamber shows that the mass of the crude magnesium liquid and the covering slag reaches 7% to 17% of the mass of the raw material, the refining chamber piston push rod starts circulating work, and the above refining process is repeated.

[0058] The magnesium raw ore used in the present application at least includes dolomite and magnesite, and can also include one or more of brucite, carnallite, olivine, etc.

[0059] The refining agent of the present application is composed of a base flux and an additive, and the additive is CaF2 or sulfur; when the additive is CaF2, the composition of the refining agent is 90%-94% of the base flux and 6%-10% of CaF2; when the additive is sulfur, the composition of the refining agent is 75%-80% of the base flux and 20%-25% of sulfur; the composition of the base flux is 35%-41% of MgCl2, 34%-40% of KCl, 5%-11% of NaCl, 6%-12% of BaCl2, and ≤2% of MgO.

[0060] Further, in step 1, the magnesium-containing raw ore has a wide source, and different proportions of dolomite and magnesite can be selected according to actual conditions, and appropriate proportions of reducing agent and flux can be matched to meet the process requirements.

[0061] Further, in step 2, the design of the reducing tank and the high-temperature alloy material pipeline can ensure stable operation in a high-temperature and relatively vacuum environment, effectively reducing heat loss and magnesium vapor leakage.

[0062] Further, in step 3, the controllable temperature condensing plate realizes accurate temperature control through the built-in silicon-molybdenum rod, and the bottom curved condensing plate shell structure design is beneficial to the smooth dripping and collection of liquid magnesium.

[0063] The addition amount and stirring time of the refining agent can be adjusted according to the specific composition and quality requirements of the crude magnesium liquid to achieve the best refining effect.

[0064] Further, in step 5, through the cooperation of the height sensing device and the current signal sensor, the automatic control of the refining process is realized, and the production efficiency and the stability of the product quality are improved.

[0065] The application will be further described below in conjunction with the drawings and specific embodiments.

[0066] Embodiment 1:

[0067] The embodiment provides a condensation and refining integrated device for continuous magnesium smelting, which comprises a refining system and a condensation system, as shown in the figure. Figure 1 The refining system is connected in communication with the condensation system through a check valve II 17 arranged above a system wall and a check valve I 8 arranged at the bottom of the system wall. The condensation system comprises a condensation zone, a crude magnesium liquid collecting zone 2, a magnesium slag discharging zone 3 and an argon gas discharging zone 5. The refining system comprises a magnesium liquid refining zone 4 and a system pressure control zone, and the system pressure control zone is arranged above the magnesium liquid refining zone.

[0068] The crude magnesium liquid collecting zone 2 is located at the bottom of the condensation system, and the condensation zone is located directly above the crude magnesium liquid collecting zone 2. The magnesium slag collecting zone is separated from the crude magnesium liquid collecting zone 2 by arranging a magnesium slag overflow weir 12. The argon gas discharging zone 5 is arranged above the magnesium slag discharging zone 3, and the mixed gas inlet 1 is arranged at a relative position of the argon gas discharging zone 5.

[0069] The magnesium liquid refining zone is provided with a refining chamber and a high-temperature-resistant eccentric stirring paddle 11 at the bottom, and the high-temperature-resistant eccentric stirring paddle 11 is inserted into the refining chamber from the side wall of the refining chamber. The check valve I 8 and the refined magnesium liquid outlet 18 are arranged at relative positions at the bottom of the refining chamber. The system pressure control zone is provided with a refining chamber piston push rod 10, and the refining agent adding port 20 is arranged at the center of the bottom of the refining chamber piston push rod 10. The light signal sensor 21 is arranged above the refining agent adding port 20. The bottom of the system pressure control zone is higher than the check valve II 17. The check valve I 8 and the check valve II 17 are check valves with the same structure, as shown in the figure. Figures 6-9

[0070] The current signal sensor 19 is arranged above the side close to the crude magnesium liquid collecting zone of the check valve I 8.

[0071] The condensation zone is provided with a temperature-controllable condensation plate 7 which is fixed in the condenser shell in a welding manner. The temperature-controllable condensation plate 7 comprises a condensation plate main body 13, a flow baffle main body 15 and a silicon molybdenum rod, as shown in the figure. Figure 2 Figures 3-5 ​​As shown, three baffle bodies 15 are staggered perpendicularly to the condensing plate body 13, and the magnesium vapor is in a fluidized state through the baffle body 15; the condensing plate body 13 is uniformly provided with 5-10 silicon-molybdenum rod insertion ports 16 in a single column at a position opposite to each baffle body 15, and the position of each column of silicon-molybdenum rod insertion ports 16 is opposite to the position of the baffle body 15; the silicon-molybdenum rod passes through the silicon-molybdenum rod insertion port 16 and is fixed in the baffle body 15.

[0072] The bottom of the magnesium slag discharge area 3 is provided with a magnesium slag discharge port 6; the argon discharge area 5 is provided with an argon outlet piston push rod 9 through the argon outlet piston push rod insertion port 14.

[0073] As shown in the figure, Figure 1 As shown in the figure, The condenser body is composed of a crude magnesium liquid collection area 2, a magnesium slag discharge area 3, and a magnesium liquid refining area 4. The magnesium liquid refining area 4 is made of a material with high temperature resistance and low thermal conductivity, which can effectively reduce heat loss. Between the crude magnesium liquid collection area 2 and the magnesium slag discharge area 3, a component magnesium slag overflow weir 12 is installed for separating the crude magnesium liquid and the slag phase, which can effectively block the crude magnesium liquid from entering the magnesium slag discharge area 3.

[0074] The top of the condensing system in this embodiment is provided with a mixed gas inlet 1, and its position is accurately designed to ensure that the magnesium vapor can uniformly enter the inside of the condenser. The temperature-controllable condensing plate is fixed in the inside of the condensing system at a suitable position through a support, and its surface temperature can be accurately controlled at 750-850°C.

[0075] The crude magnesium liquid collection area 2 is located below the temperature-controllable condensing plate 7, and the bottom of the crude magnesium liquid collection area 2 is provided with a current signal sensor 19 for real-time monitoring of the quality of the magnesium liquid and the covering slag in the crude magnesium liquid collection area 2. The left side of the crude magnesium liquid collection area 2 is connected with a refining chamber piston push rod 10, and when the magnesium liquid and the covering slag reach 5% of the total height of the condenser, the refining chamber piston push rod 10 moves upward to suck the molten liquid magnesium into the magnesium liquid refining area 4.

[0076] The magnesium liquid refining area 4 is arranged on one side of the collection chamber, and the magnesium liquid refining area 4 is installed with a high-temperature-resistant eccentric stirring paddle 11. When the molten liquid magnesium enters the magnesium liquid refining area 4, a refining agent is automatically added, and after 1s of adding the refining agent, the high-temperature-resistant eccentric stirring paddle 11 starts to work, and the stirring time is 10 min. An optical signal sensor 21 is arranged above the refining agent addition port 20, and when the magnesium liquid and the covering slag reach 5% of the total height of the condenser, the refining chamber piston push rod 10 moves downward to discharge the refining slag from the upper check valve II to the crude magnesium liquid collection area 2.

[0077] The embodiment also provides a condensation-refining integrated method for continuous magnesium smelting in relative vacuum, which is realized by using the device and includes the following steps.

[0078] Step 1: mixing and balling dolomite and magnesite, which are magnesium-containing raw ores, aluminum chips as a reducing agent and fluorite as a flux according to a mass ratio of 6:6.6:1.8:0.6 to obtain pellets;

[0079] Step 2: sending the pellets to a reduction tank, calcining at 1000℃ for 1h, then increasing the temperature to 1300℃ for reduction for 1h to perform integrated operation to generate magnesium vapor, and introducing argon into the reduction tank at a flow rate of 0.2m 3 / h, and the mixed gas of the magnesium vapor and the argon is introduced into the condensation system through a high-temperature alloy pipeline;

[0080] Step 3: controlling the temperature of the temperature-controllable condensation plate 7 to be 750℃-850℃, and condensing the magnesium vapor into liquid magnesium on the surface of the temperature-controllable condensation plate 7 and dropping to the lower coarse magnesium liquid collection area 2 to be collected to obtain coarse magnesium liquid and covering slag;

[0081] Step 4: when the height of the magnesium liquid and the covering slag in the coarse magnesium liquid collection area 2 reaches 5% of the total height of the condensation system, the magnesium liquid is sucked into the magnesium liquid refining area 4 by the upward movement of the piston push rod 10 of the refining chamber, and the refining agent is automatically added; after 1s, the coarse magnesium liquid is mixed and stirred with the refining agent by the high-temperature eccentric stirring paddle for 10min to obtain fine magnesium liquid and refining slag;

[0082] Step 5: when the height of the fine magnesium liquid and the refining slag in the magnesium liquid refining area 4 reaches 85%-90% of the total height of the magnesium liquid refining area, the piston push rod 10 of the refining chamber moves downward, and the refining slag is discharged from the upper non-return valve II 17 to the coarse magnesium liquid collection area 2. When the total mass of the fine magnesium liquid and the refining slag in the magnesium liquid refining area 4 reaches 7% of the mass of the raw material, the piston push rod 10 of the refining chamber stops the circulation work, the fine magnesium liquid is discharged from the fine magnesium liquid outlet 18, and the refining slag enters the coarse magnesium liquid collection area 2. In the coarse magnesium liquid collection area 2, as the magnesium vapor continuously condenses into liquid magnesium and drops into the coarse magnesium liquid, the covering slag at the top of the coarse magnesium liquid overflows the magnesium slag overflow weir 12 and is discharged from the magnesium slag discharge outlet 6. When the current signal sensor 19 shows that the mass of the coarse magnesium liquid and the covering slag reaches 7%-17% of the mass of the raw material, the piston push rod 10 of the refining chamber starts the circulation work, and the above refining process is repeated. The production efficiency of magnesium is improved by 8%, and the production cost is reduced.

[0083] Embodiment 2:

[0084] The device structure of the embodiment is basically the same as that of Embodiment 1, and the difference lies in that:

[0085] A flow guide device is added at the mixed gas inlet 1 of the condenser, which can guide the magnesium vapor to enter the condensation system at a specific angle and speed, making the condensation of magnesium vapor on the controllable temperature condensation plate 7 more uniform.

[0086] A flow regulating valve is installed on the non-return valve I 18 and the non-return valve II 17 between the collection chamber and the refining chamber, which can accurately control the flow of magnesium liquid into the refining chamber according to the actual production situation. When the light signal sensor 21 at the bottom of the crude magnesium liquid collection area 2 and the upper part of the magnesium slag overflow weir 12 detects that the magnesium liquid and the covering slag reach 8% of the total height of the condensation system, the refining chamber piston push rod 10 starts to suck the molten liquid magnesium into the magnesium liquid refining area 4. At this time, the refining agent adding time is adjusted to 3s, and the high-temperature resistant eccentric stirring paddle 11 stirring time is 12min, to adapt to different production needs.

[0087] When the height of the refined magnesium liquid and the refining slag in the magnesium liquid refining area 4 reaches 6% of the total height of the refining chamber, the refining chamber piston push rod 10 starts to discharge the refining slag to the collection chamber. Through these adjustments, the condensation refining process is further optimized, and the production efficiency is improved by 8%-17%.

[0088] Example 3:

[0089] In this embodiment, the device is improved as follows:

[0090] The material of the controllable temperature condensation plate 7 is upgraded to a new type of alloy material that is resistant to high temperature, high thermal conductivity and has good corrosion resistance. This material not only can more efficiently realize the condensation of magnesium vapor, but also prolongs the service life of the condensation plate.

[0091] The current signal sensor 19 at the bottom of the crude magnesium liquid collection area 2 uses a high-precision and high-sensitivity model, which can more accurately monitor the quality changes of the crude magnesium liquid and the covering slag. When the current signal sensor 19 at the bottom of the crude magnesium liquid collection area 2 shows that the quality of the crude magnesium liquid and the covering slag reaches 7% of the raw material quality, the refining chamber piston push rod 10 starts the circulating work.

[0092] In the magnesium liquid refining area 4, the structure of the high-temperature resistant eccentric stirring paddle 11 is optimized, the number and angle of the paddle blades are increased, and the stirring effect is better. The refining agent adding time is 5s, and the stirring time is 14min, to ensure that the crude magnesium liquid and the refining agent are fully mixed, further improve the refining effect, and get higher purity refined magnesium.

[0093] Example 4:

[0094] This embodiment mainly optimizes the automatic control part of the device:

[0095] In the entire device, a more advanced automation integration system is installed, which uses intelligent algorithms to automatically adjust the working parameters of each component according to the sensor data in the collection chamber and the refining chamber. For example, according to the flow and temperature of magnesium vapor, the temperature of the temperature-controlled condensing plate 7 is automatically adjusted; according to the height and mass of the magnesium liquid and the covering slag in the collection chamber, the movement of the piston push rod in the refining chamber and the addition amount of the refining agent are accurately controlled.

[0096] During the condensation process, when the flow of magnesium vapor is large, the automation integration system automatically increases the cooling efficiency of the condensing plate to ensure that the magnesium vapor can be condensed in time. During the refining process, when the impurity content in the crude magnesium liquid is detected to be higher than 7%, the system automatically increases the addition amount of the refining agent and the stirring time. Through these intelligent controls, the stability of production and product quality are further improved.

[0097] When the height sensor device detects that the magnesium liquid and the covering slag reach 12% of the total height of the condenser at the bottom of the collection chamber and the upper part of the overflow weir, the piston push rod in the refining chamber sucks the molten liquid magnesium into the refining chamber, the refining agent is added for 7s, and the stirring time is 16min. When the height of the refined magnesium liquid and the refining slag in the refining chamber reaches 8% of the total height of the refining chamber, the piston push rod in the refining chamber discharges the refining slag. When the total mass of the refined magnesium liquid and the refining slag in the refining chamber reaches 10% of the mass of the raw material, the piston push rod in the refining chamber stops circulating work.

[0098] Example 5:

[0099] This example adjusts the overall structure of the device:

[0100] The positions of the collection chamber and the refining chamber are optimized, so that the distance between them is closer, reducing the heat loss and time consumption of the magnesium liquid during transportation. At the same time, the non-return valve I 8 and the non-return valve II 17 connecting the collection chamber and the refining chamber are thickened, and a heat preservation layer is added, further reducing heat loss.

[0101] At the top of the condenser, a gas recovery device is added to collect uncondensed magnesium vapor and other gases. These gases can be reused in the production process after treatment, improving resource utilization.

[0102] In magnesium liquid refining area 4, an auxiliary heating device is added, which can be automatically started when the temperature needs to be increased to promote the refining reaction during the refining process. When the current signal sensor 19 at the bottom of the crude magnesium liquid collection area 2 shows that the quality of the crude magnesium liquid and the covering slag reaches 17% of the raw material quality, the refining chamber piston push rod 10 starts the circulating work. At this time, the refining agent is added for 10s, and the stirring time is 20min. When the height of the refined magnesium liquid and the refining slag in the magnesium liquid refining area 4 reaches 10% of the total height of the refining system, the refining chamber piston push rod 10 discharges the refining slag. When the total mass of the refined magnesium liquid and the refining slag in the magnesium liquid refining area 4 reaches 15% of the raw material quality, the refining chamber piston push rod 10 stops the circulating work. Through these improvements, the production efficiency is further improved by 8%-17%, and the production cost is reduced by 7%-9%.

Claims

1. A condensation-refining integrated apparatus for continuous magnesium production, characterized by, The refining system is connected with the condensing system through a check valve II arranged above a system wall and a check valve I arranged at the bottom of the system wall; The condensing system comprises a condensing area, a crude magnesium liquid collecting area, a magnesium slag discharging area and an argon gas discharging area; the crude magnesium liquid collecting area is located at the bottom of the condensing system, the condensing area is located directly above the crude magnesium liquid collecting area, and the magnesium slag collecting area is separated from the crude magnesium liquid collecting area by arranging a magnesium slag overflow weir; the argon gas discharging area is arranged above the magnesium slag discharging area; a mixed gas inlet is arranged at a relative position of the argon gas discharging area; The refining system comprises a magnesium liquid refining area and a system pressure control area, and the system pressure control area is arranged above the magnesium liquid refining area; The magnesium liquid refining area is provided with a refining chamber and a high-temperature-resistant eccentric stirring paddle at the bottom of the refining chamber, the high-temperature-resistant eccentric stirring paddle is inserted into the refining chamber from the side wall of the refining chamber, and a check valve I and a refined magnesium liquid outlet are arranged at relative positions of the bottom of the refining chamber; the system pressure control area is provided with a refining chamber piston push rod, a refining agent adding port is arranged at the center of the bottom of the refining chamber piston push rod, and an optical signal sensor is arranged above the refining agent adding port; the bottom of the system pressure control area is higher than the check valve II; An electric current signal sensor is arranged above the side of the check valve I close to the crude magnesium liquid collecting area; The check valve I and the check valve II are check valves of the same structure; The condensing area is provided with a temperature-controllable condensing plate which is fixed to a condenser shell by welding; The temperature-controllable condensing plate comprises a condensing plate main body, a flow baffle main body and a silicon molybdenum rod; three flow baffle main bodies are arranged in a staggered manner perpendicular to the condensing plate main body, five to ten silicon molybdenum rod insertion ports are arranged in a single row and uniformly at a relative position of each flow baffle main body and the condensing plate main body, the silicon molybdenum rod passes through the silicon molybdenum rod insertion port and is fixed in the flow baffle main body; The height of the magnesium slag overflow weir is 5% to 15% of the total height of the condenser.

2. A condensation-refining integrated apparatus for continuous magnesium production according to claim 1, wherein The magnesium slag discharging area is provided with a magnesium slag discharging port at the bottom, and the argon gas discharging area is provided with an argon gas outlet piston push rod through an argon gas outlet piston push rod insertion port.

3. A method for the integrated condensation refining of magnesium in relative vacuum, in continuous, using the apparatus according to claim 1 or 2, characterized in that, The method comprises the following steps: Step 1: mixing a magnesium-containing raw ore, a reducing agent and a fluxing agent according to a set mass ratio to obtain pellets; Step 2: sending the pellets to a reduction tank to perform calcination and reduction integration to generate magnesium vapor, introducing a carrier gas into the reduction tank, and introducing the magnesium vapor into a condenser through a high-temperature-resistant alloy pipeline; Step 3: condensing the magnesium vapor into liquid magnesium on the surface of the temperature-controllable condensing plate, and dropping the liquid magnesium into a crude magnesium liquid collecting area below to collect the liquid magnesium and cover slag; Step 4: when the height of the magnesium liquid and the cover slag in the crude magnesium liquid collecting area reaches 5% to 15% of the total height of the condensing system, the refining chamber piston push rod moves upward to suck the magnesium liquid into the magnesium liquid refining area and automatically add a refining agent; after standing, the high-temperature-resistant eccentric stirring paddle mixes and stirs the crude magnesium liquid and the refining agent to obtain refined magnesium liquid and refining slag. Step 5: When the height of the refined magnesium liquid and the refining slag in the magnesium liquid refining zone reaches 85% to 90% of the total height of the magnesium liquid refining zone, the piston push rod of the refining chamber moves downward, and the refining slag is discharged from the upper check valve II to the crude magnesium liquid collection zone; when the total mass of the refined magnesium liquid and the refining slag in the magnesium liquid refining zone reaches 7% to 17% of the mass of the raw material, the piston push rod of the refining chamber stops circulating work, the refined magnesium liquid is discharged from the refined magnesium liquid discharge port, and the refining slag enters the crude magnesium liquid collection zone; in the crude magnesium liquid collection zone, as the magnesium vapor continues to condense into liquid magnesium and drop into the crude magnesium liquid, the cover slag at the top of the crude magnesium liquid overflows the magnesium slag overflow weir and is discharged from the magnesium slag discharge port; when the current signal sensor displays that the mass of the crude magnesium liquid and the cover slag reaches 7% to 17% of the mass of the raw material, the piston push rod of the refining chamber starts circulating work, and the above refining process is repeated.

4. A method for continuous magnesium refining and condensing integration under relative vacuum according to claim 3, characterized in that, In step 4, when the height of the magnesium liquid and the cover slag in the crude magnesium liquid collection zone reaches 5% to 15% of the total height of the condenser, the piston push rod of the refining chamber moves upward, and the crude magnesium liquid in the condenser is sucked into the magnesium liquid refining zone through the check valve I; when the crude magnesium liquid is sucked into the refining chamber, the valve core of the check valve I is in an open state, the current signal sensor is interrupted, and the refining agent is added to the magnesium liquid refining zone through the refining agent adding port; at the same time, the high-temperature-resistant eccentric stirring paddle starts to work under the adjustment of the light signal sensor, and the refining is carried out.

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