CN111321310B - Method and system for preparing magnesium metal - Google Patents
Method and system for preparing magnesium metal Download PDFInfo
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- CN111321310B CN111321310B CN202010084598.2A CN202010084598A CN111321310B CN 111321310 B CN111321310 B CN 111321310B CN 202010084598 A CN202010084598 A CN 202010084598A CN 111321310 B CN111321310 B CN 111321310B
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 238000000034 method Methods 0.000 title claims abstract description 69
- 239000011777 magnesium Substances 0.000 claims abstract description 148
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 141
- 230000009467 reduction Effects 0.000 claims abstract description 71
- 229910052751 metal Inorganic materials 0.000 claims abstract description 70
- 239000002184 metal Substances 0.000 claims abstract description 70
- 238000003723 Smelting Methods 0.000 claims abstract description 67
- 238000005242 forging Methods 0.000 claims abstract description 65
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000003546 flue gas Substances 0.000 claims abstract description 61
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 57
- 239000007788 liquid Substances 0.000 claims abstract description 54
- 239000002893 slag Substances 0.000 claims abstract description 51
- 238000007664 blowing Methods 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- 238000002844 melting Methods 0.000 claims abstract description 25
- 230000008018 melting Effects 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 23
- 230000006698 induction Effects 0.000 claims description 116
- 239000011261 inert gas Substances 0.000 claims description 43
- 239000007789 gas Substances 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 31
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 24
- 239000000155 melt Substances 0.000 claims description 23
- 239000007921 spray Substances 0.000 claims description 21
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical group [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 19
- 239000010459 dolomite Substances 0.000 claims description 19
- 229910000514 dolomite Inorganic materials 0.000 claims description 19
- 230000004907 flux Effects 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 15
- 239000000956 alloy Substances 0.000 claims description 15
- 238000007599 discharging Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 13
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 229910000676 Si alloy Inorganic materials 0.000 claims description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
- 239000010436 fluorite Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 239000000779 smoke Substances 0.000 claims description 5
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 4
- PYLLWONICXJARP-UHFFFAOYSA-N manganese silicon Chemical compound [Si].[Mn] PYLLWONICXJARP-UHFFFAOYSA-N 0.000 claims description 4
- 235000003270 potassium fluoride Nutrition 0.000 claims description 4
- 239000011698 potassium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 238000004891 communication Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 44
- 239000002994 raw material Substances 0.000 abstract description 24
- 238000011084 recovery Methods 0.000 abstract description 14
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000006722 reduction reaction Methods 0.000 description 86
- 239000000243 solution Substances 0.000 description 45
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 42
- 230000008569 process Effects 0.000 description 29
- 238000006243 chemical reaction Methods 0.000 description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 239000010410 layer Substances 0.000 description 23
- 229910052786 argon Inorganic materials 0.000 description 21
- 239000011819 refractory material Substances 0.000 description 15
- 239000000428 dust Substances 0.000 description 13
- 229910052742 iron Inorganic materials 0.000 description 12
- 238000010924 continuous production Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000002485 combustion reaction Methods 0.000 description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 208000028659 discharge Diseases 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000010309 melting process Methods 0.000 description 8
- 229910052710 silicon Inorganic materials 0.000 description 8
- 239000010703 silicon Substances 0.000 description 8
- 238000009423 ventilation Methods 0.000 description 8
- 238000005265 energy consumption Methods 0.000 description 7
- 238000012546 transfer Methods 0.000 description 7
- 238000003912 environmental pollution Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 230000007547 defect Effects 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 230000005672 electromagnetic field Effects 0.000 description 3
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910001021 Ferroalloy Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method and a system for preparing magnesium metal. The preparation method comprises the following steps: (1) Melting a reducing agent or a mixture of the reducing agent and a fluxing agent to obtain a reducing solution; (2) Blowing forging white or a mixture of the forging white and a fluxing agent into the reducing solution for reduction treatment so as to obtain magnesium-containing flue gas, metal melt and smelting slag; (3) And (3) condensing the magnesium-containing flue gas so as to obtain a metal magnesium liquid and magnesium-removing flue gas, wherein the steps (1) to (2) are carried out in a closed environment under normal pressure or positive pressure. The method can realize continuous reduction smelting of the magnesium metal under normal pressure or positive pressure, improve the heat utilization rate, the production efficiency, the raw material utilization rate and the metal recovery rate, and improve the field operation environment.
Description
Technical Field
The invention belongs to the field of metallurgy, and particularly relates to a method and a system for preparing magnesium metal.
Background
At present, more than 95% of domestic magnesium metal is prepared by adopting a vacuum silicon thermal reduction process, namely a Pidgeon process, wherein the process is to firstly calcine dolomite into calcined dolomite, then mix and grind the calcined dolomite with fluorite and 75 ferrosilicon (Si content is more than 75%), press the mixture into a ball block, and then fill the ball block into a high-temperature resistant steel can with one end sealed; the steel tank is heated by burning natural gas or coal gas, and the tank is vacuumized, so that MgO in the calcined dolomite is reduced by Si in ferrosilicon to obtain magnesium vapor, and the magnesium vapor is condensed into solid crude magnesium at the opening end of the reduction tank, and the crude magnesium is refined to remove impurities. Wherein, if the magnesium metal reduction is carried out at normal pressure (101.325 KPa), the desired reaction temperature is 1550 ℃ or higher, and when at 13.3Pa pressure, the desired reaction temperature can be reduced to 1100 ℃. Thus, the vacuum system is able to lower the magnesium reduction temperature, but the system power consumption is large at low vacuum pressures. In addition, the Pijiang method adopts a closed tank type reduction process, so that the technology has low automation level, the whole production process needs manual operation, and comprises the procedures of raw material filling, ingot opening and taking, slag skimming and tank cleaning and the like, and the on-site smoke dust, high temperature, noise, smoke and other pollutants greatly influence the on-site personal health and safety, and the method has the defects of discontinuous smelting, long production period, low heat utilization efficiency, heavy on-site environmental pollution, low automation degree, high heat-resistant steel tank consumption, high cost, low reaction speed and the like.
In order to improve the intermittent production process of the Pidgeon process, a semi-continuous process Margaritite process (Magnetherm) is proposed in France, bauxite and dolomite are used as raw materials, a central electrode heating mode is adopted, the reaction temperature is 1300-1700 ℃, the vacuum degree is 0.266-13.332 kPa, after the raw materials are added into a furnace to be melted, metal magnesium vapor is reduced by vacuumizing, the liquid magnesium is condensed and liquefied, and after 10 hours of continuous feeding, the depth of slag in an electric furnace can reach 2.4m; at this time, the vacuum is cut off, inert gas is injected, the input power of the transformer is reduced, and the necessary furnace temperature is maintained; and then discharging residual iron-depleted (Si mass fraction: 18%) and magnesium-depleted slag (MgO mass fraction: 6%); a second production cycle is then started; after the second production cycle is completed, the magnesium condenser tube is removed and replaced with an empty tank. The method adopts alternating current electrode heating, because the electric furnace system has huge volume and insufficient vacuum degree, and the dolomite raw material is directly filled into the furnace, and the carbonate in the dolomite can generate high-temperature endothermic decomposition reaction, so that the temperature is very high when the electric furnace is used for smelting magnesium, the whole production period of magnesium smelting is 16-24h, 3-8t of metal magnesium can be produced in one day, 7t of raw material consumption of ton magnesium is realized, and the production efficiency is relatively low. In addition, the magnesium oxide is reduced by adopting a carbothermic reduction method under vacuum, but the method has the defects of unstable carbon reduction reaction and easy CO of magnesium vapor 2 Technical defects of difficult separation of oxidation and gas, etc.; or adopting a double-vacuum tank type smelting method, smelting ferrosilicon in one set of vacuum tank under the vacuum degree of 8-5000 Pa, smelting magnesium in the other set, and alternately carrying out the two sets in turn to realize continuous production of metal magnesium, but the method also needs to be carried out under the vacuum condition, and has the defects of complex vacuum system, high operation energy consumption, high price of a vacuum reduction tank, short service period, large use amount and the like.
Thus, the smelting process of magnesium has yet to be further improved.
Disclosure of Invention
The invention is mainly based on the following technical defects in the existing magnesium smelting process:
1. most of working procedures on a production site depend on manual operation, so that the labor intensity is high, and potential safety hazards are high; 2. magnesium smelting is intermittent production, the reduction period is long, and the production efficiency is low; 3. the production process is fully open, the dust and the waste gas are more on site, the noise is large, and the environmental pollution is serious; 4. the vacuum reduction tank is high in price, short in service period and large in use amount; 5. the reduction smelting adopts an external heating mode, so that the heat utilization efficiency is low; 6. the magnesium reduction reaction is a solid-solid reaction, the reaction rate is slow, and the raw material utilization rate is low; 7. the reduction smelting is carried out under vacuum condition, the vacuum system is complex, and the operation energy consumption is high; 8. the reduced magnesium vapor is condensed into solid state at the tank mouth, so that the impurities are more, and the magnesium vapor needs to be reheated, melted and purified, thereby having high energy consumption.
The present invention aims to solve at least one of the technical problems in the related art to some extent.
To this end, it is an object of the present invention to propose a method and a system for preparing metallic magnesium. The method can realize continuous reduction smelting of the magnesium metal under normal pressure or positive pressure, improve the heat utilization rate, the production efficiency, the raw material utilization rate and the metal recovery rate, and improve the field operation environment.
According to a first aspect of the present invention, a method for preparing magnesium metal is presented. According to an embodiment of the invention, the method comprises:
(1) Melting a reducing agent or a mixture of the reducing agent and a fluxing agent to obtain a reducing solution;
(2) Blowing forging white or a mixture of the forging white and a fluxing agent into the reducing solution for reduction treatment so as to obtain magnesium-containing flue gas, metal melt and smelting slag;
(3) Condensing the magnesium-containing flue gas to obtain a metal magnesium liquid and magnesium-removing flue gas,
wherein steps (1) to (2) are carried out in a closed environment under normal pressure or positive pressure.
The method for preparing metallic magnesium according to the above embodiment of the present invention has at least the following advantages: 1. compared with the existing vacuum reduction magnesium production process, the method is carried out under normal pressure or positive pressure, vacuum operation is not needed, the load of a vacuum system is small, and the energy power consumption is low; 2. the smelting process is carried out in a closed environment, so that the pollution to the environment is low, the noise is low, and the field operation environment is obviously improved; 3. the melting treatment and the reduction treatment can be carried out in one reaction furnace without melt transfer, so that the process flow is shortened, the heat loss is greatly reduced, and the heat utilization efficiency is remarkably improved; 4. continuous feeding and discharging can be realized, continuous production of magnesium metal is realized, and the raw material utilization rate, the production efficiency and the metal recovery rate are high; 5. the production system can be simplified and the production cost can be significantly reduced.
In addition, the method for preparing metallic magnesium according to the above embodiment of the present invention may have the following additional technical features:
in some embodiments of the invention, the method of preparing metallic magnesium further comprises: (4) And (3) dedusting and drying the magnesium-removed flue gas, and then reusing the magnesium-removed flue gas in the step (2) as a blowing carrier.
In some embodiments of the invention, steps (1) - (2) are performed under an inert atmosphere of 0.1-0.3 MPa.
In some embodiments of the invention, in step (1), the temperature of the melt process is from 1300 to 1500 c,
in some embodiments of the present invention, the reducing agent is at least one selected from the group consisting of ferrosilicon, calcium silicon, manganese silicon, aluminum metal, and calcium metal, and the fluxing agent is at least one selected from the group consisting of fluorite, potassium fluoride, and sodium fluoride.
In some embodiments of the invention, the particle size of the reducing agent is 5 to 50mm and the particle size of the fluxing agent is 0.1 to 30mm.
In some embodiments of the invention, in step (2), the temperature of the reduction treatment is 1300-1500 c,
in some embodiments of the invention, step (2) further comprises: and adding a reducing agent and/or a fluxing agent into the reducing liquid.
In some embodiments of the present invention, in step (2), the blowing mode includes at least one of bottom blowing, side blowing and top blowing.
In some embodiments of the present invention, in step (2), the inert gas is used as a blowing carrier to blow the forging white or the mixture of the forging white and the fluxing agent into the reducing solution, and the mass ratio of the blown gas to the solid is 1: (10-100).
In some embodiments of the invention, in step (2), the forging is performed by calcining dolomite at 800-850 ℃ for 1.5-3 hours.
In some embodiments of the invention, in step (2), the white-forged particle size is not more than 1mm, preferably not less than 90wt% of the fraction having a particle size of not more than 75 μm; the particle diameter of the flux is not more than 1mm, and preferably not less than 90wt% of the fraction having a particle diameter of not more than 75 μm.
In some embodiments of the invention, steps (1) - (2) are performed in an induction furnace disposed within a closed chamber having a pressure greater than the pressure within the induction furnace.
In some embodiments of the invention, the pressure in the induction furnace is 0.1-0.2 MPa, the pressure in the closed chamber is 0.15-0.3 MPa,
in some embodiments of the invention, the inner lining of the induction furnace is graphite refractory material, the secondary outer layer is magnesium refractory material, the outermost layer is a metal shell,
In some embodiments of the invention, the content of the reducing solution and/or the metal melt is not less than 10-20% of the volume of the hearth of the induction furnace,
in some embodiments of the invention, in the step (1), the initial content of the reducing solution is 20-35% of the volume of the hearth of the induction furnace,
in some embodiments of the invention, in step (2), the content of the metal melt is not more than 50% of the depth of the hearth of the induction furnace,
in some embodiments of the present invention, the induction furnace and the closed chamber are subjected to a vacuum-pumping treatment and an inert gas-filling treatment in advance before the step (1) is performed.
According to a second aspect of the present invention, a system for carrying out the above method for preparing metallic magnesium is presented. According to an embodiment of the invention, the system comprises:
the device comprises a closed chamber, a first gas inlet and a second gas inlet, wherein the closed chamber is provided with a first inert gas inlet;
the induction furnace is arranged in the closed chamber, the induction furnace comprises a furnace shell, a heating device, a furnace shell lining and a spray gun, the induction furnace is provided with a particle inlet, a powder inlet, a second inert gas inlet, a flue gas outlet, a smelting slag outlet and a melt outlet which penetrate through the closed chamber, the heating device is arranged in the furnace shell, the spray gun penetrates through the closed chamber and is inserted into the powder inlet, a smoke discharging area and a smelting area which are distributed up and down are limited in a hearth of the induction furnace, and a slag layer area and a melt area which are distributed up and down are limited in the smelting area;
The condensing device comprises a condenser and a magnesium liquid storage tank which are arranged in an up-down communication mode, wherein the condenser is provided with a flue gas inlet and a magnesium removal flue gas outlet, the magnesium liquid storage tank is provided with a magnesium liquid outlet and an impurity outlet, and the flue gas inlet is connected with the flue gas outlet.
The system for preparing metallic magnesium according to the above embodiment of the present invention has at least the following advantages: 1. the system has the advantages of simple structure, low cost, no need of a vacuum tank and only one smelting furnace, less energy consumption in the reaction process, no need of melt transfer, and remarkable reduction of heat loss; 2. the system has high automation degree and good tightness, and the induction furnace is arranged in the closed chamber, so that the environmental pollution and noise in the smelting process can be obviously reduced, the production environment is improved, and the heat loss can be further reduced; 3. continuous feeding and discharging can be realized, continuous production of magnesium metal can be realized under normal pressure or positive pressure, and the production efficiency, the raw material utilization rate and the metal recovery rate are improved; 4. the smelting process can be carried out in inert atmosphere, and the combustion of magnesium vapor can be effectively avoided, so that the recovery rate of magnesium is further improved.
In some embodiments of the invention, the system for preparing metallic magnesium further comprises: the first vacuumizing device is connected with the closed chamber and/or the induction furnace.
In some embodiments of the invention, the system for preparing metallic magnesium further comprises: the dust removing device is connected with the magnesium-removing flue gas outlet; the air inlet of the drying device is connected with the dust removing device, and the air outlet of the drying device is connected with the gas discharging device and/or the spray gun.
In some embodiments of the invention, a heat exchange device is arranged between the dust removing device and the magnesium-removing flue gas outlet.
In some embodiments of the present invention, a supercharger and an inert gas storage tank are sequentially connected between the air outlet of the drying device and the spray gun, and a second vacuumizing device is arranged between the air outlet of the drying device and the gas emptying device.
In some embodiments of the present invention, the particulate inlet is connected to a reductant bin, the spray gun is connected to a forging stock bin, the particulate inlet and/or the spray gun is connected to a flux bin, and the reductant bin, the flux bin, and the forging stock bin are each independently of an upper and lower dual bin structure.
In some embodiments of the invention, the reductant bin, the flux bin, and the forging stock bin are independently connected to a first evacuating device and the inert gas storage tank, respectively.
In some embodiments of the invention, the furnace shell further comprises a metal shell and a secondary outer layer, the secondary outer layer being a layer of magnesia refractory material and the furnace shell lining being a layer of graphite refractory material.
In some embodiments of the invention, the powder inlet is arranged at the bottom and/or the side part and/or the top of the induction furnace, the spray gun is inserted into the powder inlet from the bottom and/or the top of the induction furnace perpendicular to the horizontal direction, and/or is inserted into the powder inlet from the side part of the induction furnace along the direction with an included angle of not more than 10 degrees with the horizontal direction.
In some embodiments of the invention, the melt zone is no greater than 50% of the induction furnace hearth depth.
In some embodiments of the invention, the wall of the closed chamber is provided with a heat-insulating layer.
In some embodiments of the invention, the side and/or bottom of the magnesium liquid storage tank is provided with an insulation layer.
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
Fig. 1 is a flow chart of a method of preparing metallic magnesium according to one embodiment of the present invention.
Fig. 2 is a schematic structural view of a system for preparing metallic magnesium according to an embodiment of the present invention.
Fig. 3 is a schematic structural view of a system for preparing metallic magnesium according to still another embodiment of the present invention.
Fig. 4 is a schematic structural view of a system for preparing metallic magnesium according to still another embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
According to a first aspect of the present invention, a method for preparing magnesium metal is presented. Referring to fig. 1, according to an embodiment of the present invention, the method includes: (1) Melting a reducing agent or a mixture of the reducing agent and a fluxing agent to obtain a reducing solution; (2) Blowing forging white or a mixture of the forging white and a fluxing agent into the reducing solution for reduction treatment so as to obtain magnesium-containing flue gas, metal melt and smelting slag; (3) Condensing the magnesium-containing flue gas to obtain a metal magnesium solution and magnesium-removed flue gas, wherein the steps (1) - (2) are performed in a closed environment under normal pressure or positive pressure. The method can realize continuous reduction smelting of magnesium metal under normal pressure or positive pressure, remarkably improve the production efficiency of magnesium smelting, improve the field operation environment, and improve the heat utilization rate, the raw material utilization rate, the magnesium vapor yield and the crude magnesium purity.
The method for preparing metallic magnesium according to the above embodiment of the present invention will be described in detail with reference to fig. 1.
S100: melting the reducing agent or the mixture of the reducing agent and the fluxing agent in a closed environment under normal pressure or positive pressure to obtain a reducing solution
According to the embodiment of the invention, the reducing agent or the mixture of the reducing agent and the fluxing agent is subjected to melting treatment in a closed environment under normal pressure or positive pressure, so that vacuum operation is not needed, the load of a vacuum system is small, the energy power consumption is low, the environmental pollution is low, the noise is low, and the field operation environment is remarkably improved.
According to an embodiment of the present invention, the kinds of the reducing agent and the flux in the present invention are not particularly limited, and those skilled in the art can select according to actual needs. For example, the reducing agent may be at least one selected from the group consisting of ferrosilicon, a calcium-silicon alloy, a manganese-silicon alloy, metallic aluminum, and metallic calcium, and the flux may be at least one selected from the group consisting of fluorite, potassium fluoride, and sodium fluoride, wherein the Si content of the ferrosilicon alloy is not less than 75%. Further, the reducing agent and the flux may be subjected to crushing and sieving treatment in advance before the step (1), wherein the particle size of the reducing agent may be 20 to 50mm, and the particle size of the flux may be 0.1 to 30mm, for example, 5 to 30mm, whereby the melting efficiency and the raw material utilization ratio may be further improved.
According to still another embodiment of the present invention, the melting process may be performed under an inert atmosphere of 0.1 to 0.3MPa, for example, 0.1 to 0.12MPa, and the inventors found that if the reaction pressure is too high, not only the power consumption of the energy source is high, but also the sealing requirement on the reaction system is high, and the flow rate of the required inert gas is also high, the flow in the reaction system is easily disturbed, and thus the melt splash is caused, and the purity of the magnesium metal vapor is affected.
According to another embodiment of the present invention, the temperature of the melting process may be 1300-1500 ℃, and the inventor finds that if the temperature of the melting process is too low, the raw materials are not easy to melt, the reduction reaction is slow, the melt is easier to cool, and if the temperature of the melting process is too high, the energy consumption of the system is high.
According to another specific embodiment of the invention, the melting treatment can be performed in an induction furnace arranged in a closed chamber, the pressure in the closed chamber can be larger than the pressure in the induction furnace, so that the environment pollution is small, the noise is low, the on-site operation environment is remarkably improved, the heat loss can be further reduced, a smelting pool can be directly formed in the induction furnace, and in addition, the pressure in the closed chamber is larger than the pressure in the induction furnace, and the overflow of reaction materials, melt and slag in the induction furnace can be effectively avoided. Further, the pressure in the induction furnace can be 0.1-0.2 MPa, for example, 0.1-0.12 MPa, the pressure in the closed chamber can be 0.15-0.3 MPa, for example, 0.11-0.13 MPa, and the inert gas flows filled in the induction furnace and the closed chamber can be controlled to be regulated respectively, so that the overflow of reaction materials, melt and slag in the induction furnace can be avoided, the energy power consumption of the system can be further reduced, and the magnesium metal oxidation caused by the air leakage entering the system can be prevented.
According to another specific embodiment of the invention, the inner lining of the induction electric furnace can be graphite refractory material, the secondary outer layer can be magnesium refractory material, the magnesium refractory material is used for wrapping the graphite refractory material inner lining, the outermost layer can be a metal shell, the graphite refractory material can induce under the action of an induction electromagnetic field, and the graphite refractory material can be used for heating and heat transfer, so that the heat conduction efficiency is further improved, the heat loss is reduced, the corrosion degree of the refractory material is reduced, and the service life of the induction electric furnace is further prolonged.
According to still another embodiment of the present invention, the induction furnace and the closed chamber may be subjected to a vacuum-pumping treatment and an inert gas-charging treatment in advance before the melting treatment is performed, specifically, the induction furnace and the closed chamber may be subjected to a vacuum-pumping treatment to 1000Pa in advance before the melting treatment is performed, and then the inert gas is charged to 0.1MPa, thereby repeating the above-mentioned steps twice to sufficiently discharge the residual air in the closed chamber, the inside of the induction furnace, and the system piping; and then respectively flowing inert gas with specific flow velocity into the induction furnace and the closed chamber to ensure that the pressure in the induction furnace is 0.1-0.2 MPa and the pressure in the closed chamber is 0.15-0.3 MPa, thereby promoting the smooth proceeding of the reduction reaction.
According to another specific embodiment of the invention, the initial content of the reducing solution can be 20-35% of the volume of the hearth of the induction furnace, and the inventor discovers that if the initial content of the reducing solution is small, the reducing agent needs to be continuously added in the subsequent reduction treatment process, so that the system fluctuation is large, the temperature in a smelting pool can be obviously reduced, the normal operation of the reduction treatment is influenced, and if the initial content of the reducing solution is large, the occupied height of slag in the hearth is high, the slag discharge treatment needs to be performed in time, the slag discharge frequency is high, the magnesium purity is reduced due to easy splashing of melt in the furnace, and the magnesium yield of a single batch is reduced. The invention can further facilitate the continuous production of the magnesium production process and improve the production efficiency and the magnesium liquid yield by controlling the initial content of the reducing liquid to be 20-35% of the volume of the hearth of the induction furnace.
According to a further specific embodiment of the invention, the reducing agent and the fluxing agent can be respectively and independently fed into the induction furnace through the upper bin and the lower bin, wherein the upper bin and the lower bin can be connected with the vacuumizing device and the inert gas storage tank, so that air can be isolated, the pressure in the bins can be stabilized, the addition of the reducing agent and the fluxing agent is facilitated, and the subsequent burning loss of magnesium vapor can be further avoided.
S200: blowing forging white or a mixture of the forging white and a fluxing agent into the reducing solution to perform reduction treatment to obtain magnesium-containing flue gas, metal melt and smelting slag
According to the embodiment of the invention, the reduction treatment is performed by blowing the forging white or the mixture of the forging white and the fluxing agent into the reducing liquid so as to obtain the magnesium-containing flue gas, the metal melt and the smelting slag, wherein the reduction treatment is also performed in a closed environment under normal pressure or positive pressure, and the forging white or the mixture of the forging white and the fluxing agent can be directly added into the reducing liquid without transferring the reducing liquid. Therefore, the method not only can shorten the process flow, greatly reduce heat loss and obviously improve heat utilization efficiency, but also can realize continuous feeding and discharging, for example, a proper amount of reducing agent and fluxing agent can be periodically fed in the reduction treatment process, and metal melt and smelting slag can be timely discharged, thereby realizing continuous production of metal magnesium and obviously improving the raw material utilization rate, the production efficiency and the metal recovery rate.
According to one embodiment of the invention, the forging stock is obtained by calcining dolomite at 800-850 ℃ for 1.5-3 hours, wherein the grain size of the forging stock may be not more than 1mm, the grain size of the fluxing agent may be not more than 1mm, and further, the preferable grain sizes of the two blowing powders are not more than 75 μm and the part is not less than 90wt%. Therefore, the contact area between the forging white and the reducing liquid can be further improved, and the reduction rate and the reduction effect are further improved.
According to still another embodiment of the present invention, the pressure conditions and atmosphere of the reduction treatment control may be consistent with those of the melting treatment, that is, the reduction treatment may be performed under an inert atmosphere of 0.1 to 0.3MPa, for example, 0.1 to 0.15MPa, whereby not only the stability of the system can be ensured, the turbulence of the gas flow in the reaction system can be avoided, the smooth progress of the reduction treatment can be made, but also the contact combustion of magnesium vapor with oxygen can be avoided, thereby further improving the recovery rate and quality of magnesium.
According to another specific embodiment of the invention, the temperature of the reduction treatment can be 1300-1500 ℃, and the forging white is directly sprayed into the reducing solution under the airtight condition, so that not only are the heat loss inherent to the transfer of the reducing solution and the equipment remarkably reduced, but also the smelting slag can play a certain role in preserving heat for the melt, so that more heat can be used for the reduction reaction of the forging white; in addition, the content of the reducing solution is relatively high, and the metallic iron and the like in the reducing solution can be used as a high-temperature catalyst to further improve the reduction reaction rate, so that the reduction treatment can be smoothly performed under normal pressure or positive pressure and at the temperature of 1300-1500 ℃.
According to another embodiment of the invention, the reducing agent and/or fluxing agent can be further added into the reducing solution in the reducing treatment process, the content of the effective components in the reducing solution is continuously reduced along with the reduction reaction, and the production rate of magnesium metal is also reduced, at the moment, the reducing agent can be added into the furnace, and the content of the effective components of the reducing agent in the molten pool is increased, so that the continuous production of magnesium metal can be further facilitated.
According to another embodiment of the invention, during the reduction treatment, the power of the induction electric furnace can be increased or decreased in time according to the temperature change in the furnace, and the temperature in the furnace is kept between 1400 and 1500 ℃, so that the stable reduction treatment can be further facilitated.
According to another specific embodiment of the invention, at least one of bottom blowing, side blowing and top blowing can be adopted to blow the forging white or the mixture of the forging white and the fluxing agent into the reducing solution, so that the forging white and the reducing solution can be further favorably fully mixed, mgO in the forging white fully reacts with the reducing solution to generate metal Mg, and the metal Mg enters the upper space of the induction furnace along with argon gas flow after being heated and gasified, is discharged from a pipeline and enters a condensing device, and is finally cooled into liquid magnesium. In addition, if a side blowing and/or bottom blowing mode is adopted, inert gas flow can be always sprayed into the spray gun from the beginning of the melting reaction to the ending of the reduction reaction, so that the reducing solution and/or the metal melt can be prevented from flowing backwards to block the muzzle.
According to another embodiment of the present invention, the inert gas may be used as a blowing carrier to blow the forging white or the mixture of the forging white and the fluxing agent into the reducing solution, and the mass ratio of the blown gas to the solid may be 1: (10-100), the inventors found that if the ratio of the mass of the injected gas to the solid is too large, sufficient contact between the white forging and the reducing liquid is not facilitated, and the reduction rate and the reduction effect are affected, whereas if the ratio of the mass of the injected gas to the solid is too small, the white forging supplied to the reducing liquid per unit time is small, the reduction efficiency is similarly affected, and the flow rate of the inert gas flow is relatively high during the injection, and the disturbance to the melt is large. According to the invention, inert gas is used as a blowing carrier, so that not only can a smelting system be ensured to be in a non-oxidizing environment and the combustion loss of magnesium vapor generated by reduction be avoided, but also the metal melt can have a moderate stirring effect, thereby further improving the reduction efficiency and the reduction effect of forging white and improving the production efficiency and the recovery rate of magnesium.
According to another specific embodiment of the invention, the content of the reducing solution and/or the metal melt can be not lower than 10-20% of the volume of a hearth of the induction furnace, after smelting slag or the metal melt in the furnace is accumulated to a certain depth respectively, a smelting slag outlet or a melt outlet can be opened at random to discharge the smelting slag and the metal melt in the furnace, but the reducing solution and/or the metal melt with 10-20% of the volume of the hearth can be kept in the furnace, so that on one hand, the melting speed of solid raw materials filled in the furnace can be increased, the heating efficiency and the heating speed of the induction furnace can be improved, and on the other hand, metals such as iron in the reducing solution and/or the metal melt can be used as high-temperature catalysts to further promote the MgO reduction reaction speed, and further improve the magnesium production speed.
According to another specific embodiment of the invention, the content of the metal melt can be not higher than 50% of the depth of the hearth of the induction furnace, so as to avoid overflow of smelting slag and the like in the furnace and smooth feeding of the reducing agent and/or fluxing agent, and when the content of the metal melt is higher than 50% of the depth of the hearth of the induction furnace, the smelting slag and the metal melt can be discharged timely, wherein the metal melt can be sold as an alloy or can be smelted into the reducing agent in the submerged arc furnace again to be used in the magnesium preparation process.
According to another specific embodiment of the invention, the forging stock can be used for feeding materials into the induction furnace by adopting a feed bin with an upper bin structure and a lower bin structure, and the feed bin can be connected with a vacuumizing device and an inert gas storage tank, so that air can be isolated, the pressure in the feed bin can be stabilized, the addition of the forging stock is facilitated, and the combustion loss of magnesium vapor caused by introducing air into a system can be further avoided.
S300: condensing the magnesium-containing flue gas to obtain a metal magnesium liquid and magnesium-removing flue gas
According to the embodiment of the invention, the magnesium-containing flue gas is subjected to condensation treatment, so that the metal magnesium liquid and the magnesium-removing flue gas can be obtained. The temperature of the magnesium-removing flue gas can reach 700-750 ℃, so that heat exchange, dust removal and drying treatment can be further carried out on the magnesium-removing flue gas, the flue gas components after the heat exchange, dust removal and drying treatment are inert gases, the flue gas components can be directly discharged to the air or used as a blowing carrier for forging white, when the flue gas is used as the blowing carrier, the flue gas can be vacuumized for a plurality of times in advance, residual air in the whole system is exhausted, and then the flue gas after the drying treatment is pressurized by a supercharger and then is filled into an inert gas storage tank to be used as the blowing carrier for forging white.
According to one specific embodiment of the invention, the impurities precipitated in the magnesium liquid can be returned to the reduction treatment process for continuous reaction, other solid impurities in the magnesium-containing flue gas can be complemented and collected by the metal magnesium liquid, the impurities in the tank can be cleaned out at random due to the density and property difference, and the impurities with high magnesium content can be returned to the reduction treatment process for re-smelting.
According to another specific embodiment of the invention, the ferrosilicon alloy with Si content not lower than 75% can be crushed into blocks with particle size of 5-50 mm, the fluxing agent is crushed and sieved into particles with particle size of 0.1-30 mm, such as 5-30 mm, and the like, and the particles are placed in a furnace top bin, the reducing agent bin and the fluxing agent are sealed by adopting an upper bin structure and a lower bin structure, and a vacuumizing inlet and an argon filling inlet can be arranged in the bin to isolate air and stabilize the pressure in the bin. Adding ferrosilicon alloy into an induction furnace, heating and melting the ferrosilicon alloy into liquid state, and controlling the temperature of the ferrosilicon liquid at 1400-1500 ℃. The inner lining of the induction furnace is made of graphite refractory material, the secondary outer layer is a magnesium refractory material layer, the secondary outer layer is wrapped with the graphite refractory material, the outermost layer is a metal shell, and the whole heating furnace body is arranged in a closed chamber. The closed chamber and the induction furnace are both provided with an air suction inlet and an argon inlet, argon flows are filled into the furnace body when the furnace body runs, and the gas pressure in the closed chamber is larger than that in the induction furnace. The graphite refractory material generates induction heat under the action of an induction electromagnetic field, heats and melts ferrosilicon alloy in the furnace, and forms an alloy molten pool in the furnace, wherein the amount of the molten pool accounts for about 20-35% of the capacity of a hearth of the induction furnace.
Further, before smelting production, residual air in the furnace and in the pipeline is reduced to the greatest extent by means of vacuumizing and injecting argon into the system for multiple times, so that the subsequent oxidation combustion of the reduced magnesium metal vapor is prevented. After the pressure of inert gas in the system is stable and ferrosilicon is melted, argon is used as carrier gas, calcined dolomite powder is sprayed into a ferrosilicon molten pool in the furnace, and the mass ratio of sprayed gas to solid can be 1: (10-100). MgO in the calcined dolomite powder and Si in the ferrosilicon liquid undergo a reduction reaction to generate metal Mg, the metal Mg enters an upper space of an induction furnace along with argon gas flow after being heated and gasified, then is discharged from a pipeline and enters a condensing device, finally is cooled to liquid magnesium and is stored in a tank, heat-insulating materials are wrapped around the magnesium liquid storage tank, and the liquid magnesium in the tank is discharged out of an ingot at regular intervals. With the consumption of Si element in ferrosilicon in the reduction reaction, the Si content in the reducing agent is continuously reduced, the ferrosilicon alloy liquid is gradually changed into lean ferrosilicon water, and the production rate of magnesium metal is also reduced. At this time, ferrosilicon alloy can be added into the furnace to increase Si content in the molten pool. When the poor silicon molten iron in the furnace is accumulated to more than 50% of the depth of the molten pool, the melt outlet of the furnace body can be opened, the poor silicon molten iron is discharged to a ladle, the poor silicon molten iron can be sold as low silicon ferroalloy, and the poor silicon molten iron can be smelted into high silicon ferroalloy in the submerged arc furnace again and returned to magnesium smelting. In addition, the ferrosilicon liquid with 10-20% of the hearth volume is always kept in the induction furnace as a bottom molten pool, so that the melting speed of solid raw materials in the furnace is increased, the MgO reduction reaction rate is promoted, and the production rate of magnesium metal is further increased. SiO produced by magnesium reduction 2 Reacts with CaO in calcined dolomite to generate calcium silicate slag, and is melted into liquid slag under the action of a fluxing agent added into the furnace. After the liquid slag accumulates in the furnace to a certain depth, a smelting slag outlet is opened, the liquid slag is discharged into a slag basin under the siphon action, and the reducing slag is sold for producing building materials. After the magnesium vapor is liquefied and collected, the residual flue gas is cooled, dedusted and dried, and then is pressurized again and sent into an argon storage tank, and the residual flue gas is returned to a smelting system for recycling. When the gas pressure in the argon storage tank is reduced, pure argon gas can be supplemented to the argon storage tank, and the pressure stability of the argon storage tank is maintained.
In summary, the method for preparing metallic magnesium according to the above embodiment of the present invention has at least the following advantages: 1. compared with the existing vacuum reduction magnesium production process, the method is carried out under normal pressure or positive pressure, vacuum operation is not needed, the load of a vacuum system is small, and the energy power consumption is low; 2. the smelting process is carried out in a closed environment, so that the pollution to the environment is low, the noise is low, and the field operation environment is obviously improved; 3. the melting treatment and the reduction treatment can be carried out in one reaction furnace without melt transfer, so that the process flow is shortened, the heat loss is greatly reduced, and the heat utilization efficiency is remarkably improved; 4. continuous feeding and discharging can be realized, continuous production of magnesium metal is realized, and the raw material utilization rate, the production efficiency and the metal recovery rate are high; 5. the production system can be simplified and the production cost can be significantly reduced.
According to a second aspect of the present invention, a system for carrying out the above method for preparing metallic magnesium is presented. According to an embodiment of the present invention, as shown in fig. 1, the system includes: a closed chamber 100, an induction furnace 200 and a condensing unit 300. The system for preparing metallic magnesium is described in detail below with reference to fig. 2 to 4.
Closed chamber 100
According to the embodiment of the invention, the first inert gas inlet 110 is arranged on the closed chamber, wherein the closed chamber is suitable for sealing the induction furnace and the operation area thereof, thereby not only reducing noise and environmental pollution in the magnesium production process, remarkably improving the field operation environment, but also further reducing the heat loss of the whole operation system; in addition, by arranging the inert gas inlet on the closed chamber, residual air in the closed chamber can be discharged by injecting inert gas flow and the closed chamber can be controlled to be in a normal pressure or positive pressure environment.
According to an embodiment of the present invention, the wall of the closed chamber 100 may be provided with a heat insulating layer (not shown), wherein the heat insulating layer may be provided on the inner surface, the outer surface of the wall of the closed chamber, or a cavity may be formed in the wall to form a heat insulating interlayer, thereby further reducing heat loss during magnesium smelting and improving heat utilization rate.
Induction furnace 200
According to an embodiment of the present invention, the induction furnace 200 is disposed in the closed chamber 100, the induction furnace comprises a furnace shell 210, a heating device 220, a furnace shell lining 230 and a spray gun 240, the induction furnace 200 is provided with a particle material inlet 251, a powder material inlet 252, a second inert gas inlet 253, a flue gas outlet 254, a smelting slag outlet 255 and a melt outlet 256 which penetrate through the closed chamber, the heating device 230 is disposed in the furnace shell 210, the spray gun 240 penetrates through the closed chamber 100 and is inserted into the powder material inlet 252, a smoke discharging area 260 and a smelting area 270 which are distributed up and down are defined in a hearth of the induction furnace 200, and the smelting area 270 is defined with a slag layer area 271 and a melt area 272 which are distributed up and down. The method comprises the steps of adding a reducing agent into an induction furnace through a particle material inlet, blowing forging white into the induction furnace through a spray gun, injecting inert gas into a closed chamber through an inert gas inlet to discharge residual air in the induction furnace and control the pressure in the induction furnace, wherein the induction furnace is suitable for forming a smelting area in a hearth, carrying out smelting treatment on the reducing agent or a mixture of the reducing agent and a fluxing agent under normal pressure or positive pressure to obtain a reducing solution, and blowing the forging white or the mixture of the forging white and the fluxing agent into the reducing solution to carry out reduction treatment to obtain magnesium-containing flue gas, metal melt and smelting slag, wherein the smelting and the reduction of the forging white of the reducing agent can be realized only by the induction furnace without other smelting equipment, thereby not only shortening the process flow, but also greatly reducing heat loss, further realizing continuous feeding and discharging of magnesium metal, and remarkably improving the utilization rate of raw materials, the production efficiency and high metal recovery rate.
According to one embodiment of the present invention, the system for preparing metallic magnesium may further comprise: first evacuating device 400 as shown in fig. 2 or 3, first evacuating device 400 may be connected to closed chamber 100 and/or induction furnace 200. Therefore, the induction furnace and the closed chamber can be subjected to vacuumizing treatment and inert gas filling treatment in advance before the melting treatment and the reduction treatment, specifically, the induction furnace and the closed chamber can be subjected to vacuumizing to 1000Pa and then inert gas filling to 0.1MPa in advance before the melting treatment, so that the residual air in the closed chamber, the induction furnace and the system pipeline can be fully discharged after repeating the steps twice; and then respectively controlling the pressure in the induction furnace and the closed chamber by respectively flowing inert gas with specific flow velocity into the induction furnace and the closed chamber so as to promote the smooth proceeding of the reduction reaction.
According to still another embodiment of the present invention, the melting process may be performed under an inert atmosphere of 0.1 to 0.3MPa, for example, 0.1 to 0.15MPa, and the inventors found that if the reaction pressure is too high, not only the energy power consumption is high, but also the tightness requirement on the reaction system is high, and the required flow rate of the inert gas flow is also high, the flow disturbance in the reaction system is easy to cause, and the melt splash is easy to cause, and the purity of the magnesium vapor is affected.
According to still another embodiment of the present invention, the pressure in the closed chamber 100 may be greater than the pressure in the induction furnace 200, whereby the overflow of the reaction materials, melt and slag in the induction furnace may be effectively prevented. Further, the pressure in the induction furnace can be 0.1-0.2 MPa, for example 0.1-0.15 MPa, the pressure in the closed chamber can be 0.15-0.3 MPa, for example 0.15-0.3 MPa, and the inert gas flows filled in the induction furnace and the closed chamber can be controlled to be regulated respectively, so that the overflow of reaction materials, melt and slag in the induction furnace can be avoided, the energy power consumption of the system can be further reduced, and the magnesium metal oxidation caused by the air leakage entering the system can be prevented.
According to yet another embodiment of the present invention, the furnace shell 210 may further include a metal shell and a secondary outer layer, the secondary outer layer may be a magnesium refractory layer, the furnace shell liner 230 may be a graphite refractory layer, and the graphite refractory generates induction heat under the action of the induction electromagnetic field, thereby not only improving the service life of the induction electric furnace, but also heating and transferring heat by using the graphite refractory, thereby further improving the heat conduction efficiency, reducing heat loss, reducing the erosion degree of the refractory, and further improving the service life of the induction electric furnace.
According to another embodiment of the present invention, as shown in fig. 3 or fig. 4, the powder inlet 252 may be disposed at the bottom and/or the side and/or the top of the induction furnace 200, so that at least one of bottom blowing, side blowing and top blowing may be adopted to blow the forging white or the mixture of the forging white and the fluxing agent into the reducing solution, thereby further facilitating the full mixing of the forging white and the reducing solution, improving the reduction efficiency, enabling MgO in the forging white to fully react with the reducing solution and generate metal Mg, and after the metal Mg is heated and gasified, the metal Mg enters into the upper space of the induction furnace along with argon gas flow, is discharged from the pipeline and enters into the condensing device, and finally is cooled into liquid magnesium. In addition, if the powder inlet 252 is provided at the bottom and/or the side of the induction furnace 200, an inert gas flow can be always injected into the spray gun from the beginning of the melting reaction to the end of the reduction reaction, so as to prevent the backflow of the reducing solution and/or the metal melt from blocking the muzzle.
According to still another embodiment of the present invention, when the powder inlet 252 is provided at the bottom and/or the top of the induction furnace 200, the spray gun 240 may be inserted perpendicularly to the horizontal direction into the powder inlet, and when the powder inlet 252 is provided at the side of the induction furnace 200, the angle between the spray gun 240 and the horizontal direction may be not more than 10 degrees.
According to yet another embodiment of the present invention, the melt zone 272 may be no more than 50% of the depth of the furnace hearth of the induction furnace, so as to avoid overflow of slag and the like in the furnace and smooth addition of reducing agent and/or fluxing agent, and when the content of the metal melt is higher than 50% of the depth of the furnace hearth of the induction furnace, the slag and the metal melt may be discharged in time, wherein the metal melt may be sold as an alloy or may be smelted again in the submerged arc furnace to form the reducing agent for use in the magnesium preparation process. Further, after the smelting slag or the metal melt in the furnace is accumulated to a certain depth respectively, the smelting slag outlet or the melt outlet can be opened at random to discharge the smelting slag and the metal melt in the furnace, but the reducing liquid and/or the metal melt with the hearth volume of 10-20% can be kept in the furnace, so that on one hand, the melting speed of solid raw materials in the furnace can be increased, the heating efficiency and the heating speed of the induction furnace can be improved, and on the other hand, metals such as iron in the reducing liquid and/or the metal melt can be used as a high-temperature catalyst to further promote the MgO reduction reaction rate and further improve the magnesium production rate.
According to still another embodiment of the present invention, as shown in fig. 3 or 4, the particulate inlet 251 may be connected to the reducing agent bin 610, the spray gun 240 is connected to the forging stock bin 620, the particulate inlet 251 and/or the spray gun 240 are connected to the flux bin 630, and the reducing agent bin 610, the flux bin 630 and the forging stock bin 620 may be respectively and independently of one another in a double-bin structure, thereby being more advantageous in isolating air and avoiding air from being introduced into the induction furnace during charging. Further, the reducing agent bin 610, the flux bin 630 and the forging stock bin 620 may be separately connected to the first vacuumizing device 400 and the inert gas storage tank, respectively, so that residual air in the bin may be further exhausted through vacuumizing and injecting inert gas, thereby isolating air and stabilizing pressure in the bin, so that not only is addition of the reducing agent and the flux facilitated, but also subsequent combustion loss of magnesium vapor may be further avoided.
According to still another embodiment of the present invention, the reducing agent hopper 610, the flux hopper 630, and the forging stock hopper 620 may be separately provided with a feed valve and a doser (not shown), respectively, whereby precise control of the addition amount of raw materials may be more advantageous.
According to still another embodiment of the present invention, the kinds of the reducing agent and the fluxing agent in the present invention are not particularly limited, and may be selected by those skilled in the art according to actual needs. For example, the reducing agent may be at least one selected from the group consisting of ferrosilicon, a calcium-silicon alloy, a manganese-silicon alloy, metallic aluminum, and metallic calcium, and the flux may be at least one selected from the group consisting of fluorite, potassium fluoride, and sodium fluoride, wherein the Si content of the ferrosilicon alloy is not less than 75%. Further, the reducing agent and the flux may be subjected to crushing and sieving treatment in advance before the step (1), wherein the particle size of the reducing agent may be 20 to 50mm, the particle size of the flux may be 0.1 to 30mm, for example, 5 to 30mm, etc., whereby the melting efficiency and the raw material utilization ratio can be further improved. In the present invention, the white forging is obtained by calcining dolomite at 800 to 850℃for 1.5 to 3 hours, wherein the particle size of the white forging may be not more than 1mm, the particle size of the flux may be not more than 1mm, and further, the preferable particle size of the two blowing powders is not more than 75 μm and not less than 90% by weight. Therefore, the contact area between the forging white and the reducing liquid can be further improved, and the reduction rate and the reduction effect are further improved.
According to another embodiment of the present invention, the temperature of the melting process may be 1300-1500 ℃, and the inventor finds that if the temperature of the melting process is too low, the raw materials are not easy to melt, the reduction reaction is slow, the melt is easier to cool, and if the temperature of the melting process is too high, the energy consumption of the system is high.
According to another specific embodiment of the invention, the initial content of the reducing solution can be 20-35% of the volume of the hearth of the induction furnace, and the inventor discovers that if the initial content of the reducing solution is small, the reducing agent needs to be continuously added in the subsequent reduction treatment process, so that the system fluctuation is large, the temperature in a smelting pool can be obviously reduced, the normal operation of the reduction treatment is influenced, and if the initial content of the reducing solution is large, the occupied height of slag in the hearth is high, the slag discharge treatment needs to be performed in time, the slag discharge frequency is high, the magnesium purity is reduced due to easy splashing of melt in the furnace, and the magnesium yield of a single batch is reduced. The invention can further facilitate the continuous production of the magnesium production process and improve the production efficiency and the magnesium liquid yield by controlling the initial content of the reducing liquid to be 20-35% of the volume of the hearth of the induction furnace.
According to still another embodiment of the present invention, the pressure conditions and atmosphere controlled by the reduction treatment can be consistent with those of the melting treatment, so that not only can the stability of the system be ensured, and the turbulence of the gas flow in the reaction system be avoided, so that the reduction treatment can be smoothly performed, but also the contact combustion of magnesium vapor and oxygen can be avoided, thereby further improving the recovery rate and quality of magnesium.
According to another specific embodiment of the invention, the temperature of the reduction treatment can be 1300-1500 ℃, and the forging white is directly sprayed into the reducing solution under the airtight condition, so that not only are the heat loss inherent to the transfer of the reducing solution and the equipment remarkably reduced, but also the smelting slag can play a certain role in preserving heat for the melt, so that more heat can be used for the reduction reaction of the forging white; in addition, the content of the reducing solution is relatively high, and the metallic iron and the like in the reducing solution can be used as a high-temperature catalyst to further improve the reduction reaction rate, so that the reduction treatment can be smoothly performed under normal pressure or positive pressure and at the temperature of 1300-1500 ℃.
According to another embodiment of the invention, during the reduction treatment, the power of the induction electric furnace can be increased or decreased in time according to the temperature change in the furnace, and the temperature in the furnace is maintained at 1400-1550 ℃, so that the stable reduction treatment can be further facilitated.
According to another embodiment of the invention, the reducing agent and/or fluxing agent can be further added into the reducing solution in the reducing treatment process, the content of the effective components in the reducing solution is continuously reduced along with the reduction reaction, and the production rate of magnesium metal is also reduced, at the moment, the reducing agent can be added into the furnace, and the content of the effective components of the reducing agent in the molten pool is increased, so that the continuous production of magnesium metal can be further facilitated.
According to another embodiment of the present invention, the inert gas may be used as a blowing carrier to blow the forging white or the mixture of the forging white and the fluxing agent into the reducing solution, and the mass ratio of the blown gas to the solid may be 1: (10-100), the inventors found that if the ratio of the mass of the injected gas to the solid is too large, sufficient contact between the white forging and the reducing liquid is not facilitated, and the reduction rate and the reduction effect are affected, whereas if the ratio of the mass of the injected gas to the solid is too small, the white forging supplied to the reducing liquid per unit time is small, the reduction efficiency is similarly affected, and the flow rate of the inert gas flow is relatively high during the injection, and the disturbance to the melt is large. According to the invention, inert gas is used as a blowing carrier, so that not only can a smelting system be ensured to be in a non-oxidizing environment and the combustion loss of magnesium vapor generated by reduction be avoided, but also the metal melt can have a moderate stirring effect, thereby further improving the reduction efficiency and the reduction effect of forging white and improving the production efficiency and the recovery rate of magnesium.
Condensing unit 300
According to an embodiment of the present invention, the condensing apparatus 300 includes a condenser 310 and a magnesium liquid storage tank 320 which are arranged in up-down communication, the condenser having a flue gas inlet 311 and a magnesium removal flue gas outlet 312, the magnesium liquid storage tank having a magnesium liquid outlet 321 and an impurity outlet 322, the flue gas inlet 311 being connected to the flue gas outlet 254. The condensing device is suitable for condensing the magnesium-containing flue gas to obtain metal magnesium liquid and magnesium-removing flue gas.
According to an embodiment of the present invention, as shown in fig. 4, the side and/or bottom of the magnesium solution storage tank 320 may be provided with a heat insulation layer 330, thereby not only reducing heat loss of the molten metal magnesium solution, but also facilitating ingot casting.
According to still another embodiment of the present invention, as shown in fig. 3 and 4, the system for preparing metallic magnesium may further include: the dust removing device 710 and the drying device 720, wherein the dust removing device 710 is connected with the magnesium-removed flue gas outlet 312; the air inlet of the drying device 720 is connected with the dust removing device 710, and the air outlet of the drying device 720 is connected with the gas discharging device 800 and/or the spray gun 240; further, a heat exchanging device 730 may be further disposed between the dust removing device 710 and the magnesium removal flue gas outlet 312. Therefore, the magnesium-removed flue gas can be directly discharged to the air after heat exchange, dust removal and drying, or can be used as a blowing carrier for forging.
According to still another embodiment of the present invention, as shown in fig. 3 or 4, a supercharger 910 and an inert gas storage tank 920 connected in sequence may be provided between the air outlet of the drying device 720 and the spray gun 240, and a second vacuumizing device 500 is provided between the air outlet of the drying device 720 and the gas discharging device 800. Specifically, the air outlet pipeline of the drying device 720 may include three branches, where a first branch 721 is sequentially connected to the supercharger 910 and the inert gas storage tank 920, a first air vent valve 724 is disposed on the first branch, a second branch 722 and a third branch 723 are connected to the air outlet device 800, a second air vent valve 725 is disposed upstream of the second branch 722 and the third branch 723, a third air vent valve 726 is disposed on the second branch 722, and a second vacuum pumping device 500 is disposed on the third branch 723. Thus, when the heat-exchanged, dust-removed and dried magnesium-removed flue gas is directly discharged to the air, the first ventilation valve 724 and the second vacuumizing device 500 can be closed, and the second ventilation valve 725 and the third ventilation valve 726 can be opened at the same time; when the magnesium-removed flue gas after heat exchange, dust removal and drying is used as a blowing carrier, the first ventilation valve 724 and the third ventilation valve 726 can be closed in advance, the second ventilation valve 725 and the second vacuumizing device 500 are opened simultaneously, the whole system gas transmission pipeline and the whole system are vacuumized, air is prevented from remaining in the system, the second ventilation valve 725 and the second vacuumizing device 500 are closed after the vacuumizing is completed, the first ventilation valve 724 and the supercharger 910 are opened simultaneously, the dried flue gas is pressurized, and then an inert gas storage tank is filled in, so that the magnesium-removed flue gas is used for blowing the carrier.
According to yet another embodiment of the present invention, the first and second evacuation devices 400 and 500 may each independently include one or more vacuum pumps, wherein, as shown in fig. 2 and 3, the first evacuation device 400 may include at least two vacuum pumps 410, thereby evacuating and ventilating each of the bins, the closed cells, and the induction furnace, respectively.
According to one specific embodiment of the invention, the impurities precipitated in the magnesium liquid can be returned to the reduction treatment process for continuous reaction, other solid impurities in the magnesium-containing flue gas can be complemented and collected by the metal magnesium liquid, the impurities in the tank can be cleaned out at random due to the density and property difference, and the impurities with high magnesium content can be returned to the reduction treatment process for re-smelting.
In summary, the system for preparing metallic magnesium according to the above embodiment of the present invention has at least the following advantages: 1. the system has the advantages of simple structure, low cost, no need of a vacuum tank and only one smelting furnace, less energy consumption in the reaction process, no need of melt transfer, and remarkable reduction of heat loss; 2. the system has high automation degree and good tightness, and the induction furnace is arranged in the closed chamber, so that the environmental pollution and noise in the smelting process can be obviously reduced, the production environment is improved, and the heat loss can be further reduced; 3. continuous feeding and discharging can be realized, continuous production of magnesium metal can be realized under normal pressure or positive pressure, and the production efficiency, the raw material utilization rate and the metal recovery rate are improved; 4. the smelting process can be carried out in inert atmosphere, and the combustion of magnesium vapor can be effectively avoided, so that the recovery rate of magnesium is further improved.
The scheme of the present invention will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the present invention and should not be construed as limiting the scope of the invention. The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Preparation stage
Raw material preparation: and heating dolomite to 800-850 ℃ in a rotary kiln, keeping the temperature for 2 hours, directly discharging to obtain calcined dolomite (calcined dolomite for short), ball milling to obtain particles with the particle size smaller than 200 meshes, and loading the particles into a calcined dolomite storage bin. Crushing 75 ferrosilicon and fluorite into blocks with the particle size not less than 20mm, and respectively loading the blocks into a furnace top reducing agent bin and a fluxing agent bin.
System exhaust: and (3) vacuumizing the induction furnace, the closed chamber, the subsequent flue, condensation and other systems to 1000Pa, closing the vacuum system, opening the argon gas charging system, introducing argon gas into the induction furnace and the closed chamber, closing the argon gas system after the gas pressure in the induction furnace reaches 0.1MPa, and opening the vacuum system. And repeating the process for 2 times, and fully discharging residual air in the induction furnace, the closed chamber and the subsequent system. Finally, continuously introducing argon flow into the furnace, maintaining the pressure of the gas in the furnace at 0.1-0.12 MPa and the pressure of the closed chamber at 0.11-0.13 MPa.
(II) melt-processing
In the exhaust process of the system, ferrosilicon alloy and fluxing agent are added into an induction furnace, the induction furnace is electrified and heated, the ferrosilicon alloy in the furnace gradually rises in temperature, and gradually melts into a liquid state after reaching 1500 ℃, a reducing agent molten pool is formed in the furnace, and the depth of the molten pool is about 25% of the depth of a hearth. In the process of producing a molten pool, argon gas flow is always sprayed into the spray gun, so that the backflow of molten pool liquid is prevented from blocking the muzzle.
(III) reduction treatment and condensation treatment
After the molten pool in the induction furnace is formed and the exhaust is completed, a valve of the calcining Bai Liaocang is opened, and the powdery calcined dolomite is blown into the molten pool in the furnace under the driving of argon flow blowing. The magnesium vapor is continuously reduced, and is driven by the argon flow to enter a condensing device with the temperature maintained at 700-750 ℃ to be continuously condensed into molten magnesium. The residual flue gas is injected into an argon storage tank after being cooled, dedusted, dehydrated and pressurized, and is led to an induction furnace system for recycling.
Wherein, according to the reaction rate of magnesium vapor and the condensation amount of magnesium liquid in the furnace and the slag melting condition, ferrosilicon alloy and fluxing agent are timely added into the furnace. The power of the induction furnace is increased and decreased in time according to the temperature change in the furnace, and the temperature in the furnace is kept between 1400 and 1500 ℃. After the slag or the lean silicon iron in the furnace are accumulated for a certain depth respectively, a smelting slag outlet or a melt outlet is opened at random, the slag in the furnace is discharged into a slag ladle outside the furnace, the lean silicon iron in the furnace is discharged into a molten iron ladle outside the furnace, and a molten iron pool accounting for about 10-15% of the furnace capacity is still kept in the furnace. The waste residue discharged from the furnace is sold for building material production, and the lean silicon molten iron is used as low silicon iron alloy for manufacturing alloy steel.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (5)
1. A method of preparing metallic magnesium comprising:
(1) Melting a reducing agent or a mixture of the reducing agent and a fluxing agent to obtain a reducing solution; the temperature of the melting treatment is 1300-1500 ℃; the reducing agent is at least one selected from ferrosilicon alloy, calcium silicon alloy, manganese silicon alloy, metallic aluminum and metallic calcium;
(2) Blowing forging white or a mixture of the forging white and a fluxing agent into the reducing solution for reduction treatment so as to obtain magnesium-containing flue gas, metal melt and smelting slag; the temperature of the reduction treatment is 1300-1500 ℃;
(3) Condensing the magnesium-containing flue gas to obtain a metal magnesium liquid and magnesium-removing flue gas,
wherein, the steps (1) - (2) are carried out in a closed environment under normal pressure or positive pressure;
the steps (1) - (2) are carried out under an inert atmosphere of 0.1-0.3 MPa;
the steps (1) - (2) are carried out in an induction furnace arranged in a closed chamber, and the pressure in the closed chamber is larger than the pressure in the induction furnace;
in the step (1), the initial content of the reducing solution is 20-35% of the volume of the hearth of the induction furnace;
the pressure in the induction furnace is 0.1-0.2 MPa, the pressure in the closed chamber is 0.15-0.3 MPa,
the content of the reducing solution and/or the metal melt is not less than 10-20% of the volume of the hearth of the induction furnace,
In the step (2), the content of the metal melt is not higher than 50% of the depth of the hearth of the induction furnace,
in the step (2), the grain size of the forging white is not more than 1mm; the particle size of the fluxing agent is not more than 1mm;
a system for carrying out the method for preparing metallic magnesium, comprising:
the device comprises a closed chamber, a first gas inlet and a second gas inlet, wherein the closed chamber is provided with a first inert gas inlet;
the induction furnace is arranged in the closed chamber, the induction furnace comprises a furnace shell, a heating device, a furnace shell lining and a spray gun, the induction furnace is provided with a particle inlet, a powder inlet, a second inert gas inlet, a flue gas outlet, a smelting slag outlet and a melt outlet which penetrate through the closed chamber, the heating device is arranged in the furnace shell, the spray gun penetrates through the closed chamber and is inserted into the powder inlet, a smoke discharging area and a smelting area which are distributed up and down are limited in a hearth of the induction furnace, and a slag layer area and a melt area which are distributed up and down are limited in the smelting area;
the condensing device comprises a condenser and a magnesium liquid storage tank which are arranged in an up-down communication mode, wherein the condenser is provided with a flue gas inlet and a magnesium removal flue gas outlet, the magnesium liquid storage tank is provided with a magnesium liquid outlet and an impurity outlet, and the flue gas inlet is connected with the flue gas outlet.
2. The method as recited in claim 1, further comprising:
(4) And (3) dedusting and drying the magnesium-removed flue gas, and then reusing the magnesium-removed flue gas in the step (2) as a blowing carrier.
3. The method according to claim 1 or 2, wherein in the step (1), the flux is at least one selected from fluorite, potassium fluoride and sodium fluoride,
optionally, the particle size of the reducing agent is 5-50 mm, and the particle size of the fluxing agent is 0.1-30 mm.
4. A method according to claim 3, wherein step (2) further comprises: adding a reducing agent and/or a fluxing agent into the reducing liquid,
optionally, in the step (2), the blowing mode comprises at least one of bottom blowing, side blowing and top blowing,
optionally, in the step (2), blowing forging white or a mixture of forging white and a fluxing agent into the reducing solution by taking inert gas as a blowing carrier, wherein the mass ratio of the blown gas to the solid is 1: (10-100),
optionally, in the step (2), the forging white is obtained by calcining dolomite at 800-850 ℃ for 1.5-3 hours,
optionally, in step (2), the portion having a particle diameter of not more than 75 μm is not less than 90wt%; the flux has a particle diameter of not more than 75 μm and a particle diameter of not less than 90wt%.
5. The method according to claim 1 or 4, wherein the inner lining of the induction furnace is graphite refractory, the secondary outer layer is magnesia refractory, the outermost layer is a metal shell,
optionally, the induction furnace and the closed chamber are subjected to vacuum pumping treatment and inert gas filling treatment in advance before the step (1) is performed.
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| CN112501434B (en) * | 2020-10-19 | 2023-04-14 | 北京中冶设备研究设计总院有限公司 | Liquid magnesium smelting reducing agent and application thereof |
| CN114293014B (en) * | 2021-12-16 | 2022-09-27 | 西安交通大学 | Silicon carbide-free thermal reduction magnesium metallurgy device and method |
| CN114480879A (en) * | 2022-03-07 | 2022-05-13 | 沈阳益富冶炼技术装备有限公司 | Method and system for continuously producing magnesium metal |
| CN115747523A (en) * | 2022-11-18 | 2023-03-07 | 昆明理工大学 | Method for smelting magnesium by vacuum carbothermic reduction |
| CN117346528B (en) * | 2023-12-05 | 2024-03-15 | 湘潭和鑫盛新材料有限公司 | Vacuum pumping and top blowing inert gas induction furnace for refining metal |
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| CN101117667A (en) * | 2007-09-19 | 2008-02-06 | 北京科技大学 | Magnesium metal reduction process using liquid calcium as reducing agent and device thereof |
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| CN101117667A (en) * | 2007-09-19 | 2008-02-06 | 北京科技大学 | Magnesium metal reduction process using liquid calcium as reducing agent and device thereof |
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