WO2016011696A1 - 一种快速连续炼镁的方法 - Google Patents

一种快速连续炼镁的方法 Download PDF

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WO2016011696A1
WO2016011696A1 PCT/CN2014/085224 CN2014085224W WO2016011696A1 WO 2016011696 A1 WO2016011696 A1 WO 2016011696A1 CN 2014085224 W CN2014085224 W CN 2014085224W WO 2016011696 A1 WO2016011696 A1 WO 2016011696A1
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Prior art keywords
temperature
magnesium
ingredients
pellets
reduction
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PCT/CN2014/085224
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English (en)
French (fr)
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张廷安
豆志河
张子木
刘燕
吕国志
赫冀成
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东北大学
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Priority to US15/118,205 priority Critical patent/US10047413B2/en
Priority to EA201691841A priority patent/EA032015B1/ru
Priority to EP14898095.6A priority patent/EP3173497B1/en
Priority to KR1020167022755A priority patent/KR101763676B1/ko
Publication of WO2016011696A1 publication Critical patent/WO2016011696A1/zh
Priority to IL247574A priority patent/IL247574B/en

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    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/16—Sintering; Agglomerating
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2413—Binding; Briquetting ; Granulating enduration of pellets
    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/242—Binding; Briquetting ; Granulating with binders
    • C22B1/243—Binding; Briquetting ; Granulating with binders inorganic
    • 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
    • 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
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced

Definitions

  • the invention belongs to the technical field of non-ferrous metallurgy, and in particular relates to a method for rapid continuous magnesium smelting.
  • magnesium began to enter the civilian market. Since the 1960s, due to the application of magnesium in the civilian market and space technology, the development of the magnesium industry has been promoted, and the magnesium smelting method and production technology have also made great breakthroughs, and the economic benefits have been continuously improved.
  • electrolysis The thermal reduction method is to obtain magnesium metal by calcining dolomite as a raw material, using ferrosilicon as a reducing agent, and reducing under high temperature and vacuum conditions. The most important of these is the Pijiang process of magnesium smelting. Due to the simple process and the significant reduction in production costs, the world's raw magnesium production has increased significantly.
  • Pidgeon magnesium has the advantages of simple method and low investment cost.
  • the Pijiang method of magnesium smelting needs to be carried out under high temperature and vacuum conditions.
  • the operation is intermittent operation, labor intensity, long reduction cycle (10 ⁇ 12h), low magnesium metal yield (30kg/reduction tank), and Shortcomings such as high energy consumption. Since the reduction tank is used under high temperature and high vacuum for a long period of time, the life of the reduction tank is lowered and the production cost is increased.
  • the raw material dolomite used must first be calcined, and the ultrafine powder produced by calcination cannot be utilized, resulting in serious waste of resources.
  • Patent "Application No.: 200910236975.3” studies the magnesium smelting process of reducing the mixture of calcined white and caustic magnesite using Si-Fe + Al + Ca composite reducing agent, so that the reduction time is shortened to 5-9h.
  • the above research has improved the technical level of thermal magnesium smelting to a certain extent, but the above research is still based on the traditional silicon thermal smelting process, and it is still based on the improvement and improvement of the basic idea of high temperature vacuum, and There is no fundamental breakthrough. Therefore, the conventional silicon hot magnesium smelting has a long reduction cycle, high energy consumption, short life of the reduction tank and high production cost, and still cannot be fundamentally solved.
  • the invention solves the defects of long reduction cycle, high energy consumption, short life of the reduction tank and high production cost in the conventional silicon hot smelting magnesium, and the invention provides a Fast continuous magnesium smelting
  • the method that is, high-temperature reduction in a flowing inert gas, and the generated high-temperature magnesium vapor is immediately carried away by the flowing inert carrier gas, and condensed to obtain magnesium metal.
  • the method of the invention has a fast reaction speed, the reduction time is shortened to less than 90 minutes, the recovery rate of magnesium is increased to over 88%, and the continuous production of magnesium is realized.
  • the method for rapidly and continuously smelting magnesium of the present invention comprises the steps of directly pelletizing, pellet calcination, calcination of a calcined pellet at a high temperature in a flowing argon atmosphere, condensation of high temperature magnesium vapor, and the like.
  • the direct pelletizing means that the dolomite or magnesite which has not been calcined is mixed with the reducing agent and the fluorite in proportion, and the pellets of 5 to 20 mm in diameter are produced by the disc pelletizer; the pellet is calcined It means that the pellet is calcined at 850 ⁇ 1050 °C for 30 ⁇ 120min under argon or nitrogen atmosphere, and the water and volatile substances in the pellet are removed, so that the carbonate is released to C0 2 , and the reducing agent will The MgO formed by diffusion and decomposition during the calcination process is more fully contacted; the high temperature reduction of the calcined pellet refers to the high temperature reduction reaction of the calcined pellet in a flowing argon atmosphere in a "relative vacuum" atmosphere, and the reaction is formed.
  • the high temperature magnesium vapor is immediately carried away by the flowing argon carrier gas.
  • the partial pressure of the high-temperature magnesium vapor at the reaction interface is always much lower than the lamt, that is, at the relative "negative pressure”. status”. Therefore, the atmosphere at the reduction reaction interface for the formation of magnesium vapor is like a vacuum in a closed container, called “relative vacuum” or “relative vacuum”, which provides more sufficient thermodynamics for the reaction to occur.
  • the condensation of magnesium vapor refers to the process of rapidly condensing high-temperature magnesium vapor continuously carried by argon gas in a high-temperature reduction furnace to obtain magnesium metal.
  • the method for rapidly and continuously smelting magnesium of the present invention specifically comprises the following steps:
  • Dolomite 75Si-Fe alloy: fluorite, according to the mass ratio of 110: (10-13): (3.0 ⁇ 4.0) Ingredients, mix evenly, then add 1.0 ⁇ 2.0% water glass as the total mass of the ingredients 2.0 to 5.0% water of the total mass of the binder and ingredients;
  • dolomite A1: fluorite, according to the mass ratio of 115 : ( 10-13 ): (2.0-3.0) ingredients, mix evenly, then add 1.0 ⁇ 2.0% of the total mass of the water glass as a binder and 2.0 to 5.0% of the total mass of the ingredients;
  • Pelletizing Mix the ingredients evenly, make balls, and obtain pellets with a particle size of 5 ⁇ 20mm. Dry the pellets naturally for 10 ⁇ 24h; Step 2: Calcination of pellets
  • the air-dried pellets are placed in a high-temperature furnace, a rotary kiln or a fluidized bed to be heated to 150 ⁇ 250 °C, dehydrated for 30 to 60 minutes, and then heated to 850 ⁇ 1050 °C under argon or nitrogen atmosphere. Calcined for 30 ⁇ 120min;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into a closed high-temperature reduction furnace without cooling under argon gas treatment, and then subjected to a high-temperature reduction reaction in a flowing argon atmosphere at a reduction temperature of 1300 to 1600 ° C.
  • the time is 20 ⁇ 90min
  • the flow rate of argon gas is 2.0 ⁇ 5.0m 3 /h
  • the high temperature magnesium steam is continuously obtained, and mixed with argon gas to form a high temperature mixed gas, and the reducing slag is continuously discharged to the high temperature reduction furnace;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the high-temperature reduction furnace through the flowing argon gas stream, and is sent to the condensing system through the sealed line to be condensed to obtain magnesium metal.
  • the method for rapidly and continuously smelting magnesium of the present invention may specifically include the following steps:
  • the magnesite Al : CaO: fluorite according to the mass ratio of 48 : ( 10-13 ): ( 15-18): ( 2.0-3.0 ) ingredients, mix evenly, then add 2.0 ⁇ 3.0% of the total mass of the ingredients Water glass as 2.0 to 6.0% of the total mass of the binder and ingredients;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a high-temperature furnace, a rotary kiln or a fluidized bed to be heated to 150 ⁇ 250 °C, dehydrated for 30 to 60 minutes, and then heated to 850 ⁇ 1050 °C under argon or nitrogen atmosphere. Calcined for 30 ⁇ 120min;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into a closed high-temperature reduction furnace without cooling under argon gas treatment, and then subjected to a high-temperature reduction reaction in a flowing argon atmosphere at a reduction temperature of 1300 to 1600 ° C.
  • the time is 20 ⁇ 90min
  • the flow rate of argon gas is 2.0 ⁇ 5.0m 3 /h
  • the high temperature magnesium steam is continuously obtained, and mixed with argon gas to form a high temperature mixed gas
  • the reducing slag is continuously discharged to the high temperature reduction furnace;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the high-temperature reduction furnace through the flowing argon gas stream, and is sent to the condensing system through the sealed line to be condensed to obtain magnesium metal.
  • the compound A1 or 75Si-Fe alloy in the step 1 is replaced by a composite reducing agent, and the composite reducing agent is one of the following three types:
  • the amount of the composite reducing agent used is: 1 mass unit of A1 can be replaced by 2.2 times mass unit of Ca; 1 mass unit of 75Si-Fe alloy can be replaced by 2.2 times mass unit of Ca; 1 mass unit of A1 and 1 mass unit of 75Si -Fe alloy is equivalent.
  • step 1 a disc pelletizer is used for the ball formation;
  • step 3 the high temperature reduction furnace is an intermediate frequency induction furnace or a high temperature resistance furnace;
  • the condensation mode in the step 4 is direct condensation or atomization condensation, and the direct condensation mode is circulating water-cooling condensation.
  • the 75Si-Fe alloy is: Si-Fe alloy having a Si content of 75%.
  • MgC0 3 -CaC0 3 MgO-CaO+2C0 2 ( 1 )
  • MgC0 3 MgO +C0 2 (2)
  • the high-temperature reduction reaction is carried out in a flowing inert argon atmosphere, the high-temperature magnesium vapor generated at the pellet reaction interface is immediately carried away by the flowing argon gas, so that at the reaction interface, for the warm magnesium vapor, it is always at A partial pressure is much lower than the negative pressure state of the lamat, the so-called "relative vacuum” or "relative vacuum”. Since the generated high-temperature magnesium vapor is carried by inert argon at any time, it will promote the reaction of high-temperature reduction to form magnesium vapor (3) ⁇ (6) Thoroughly proceed to the right, greatly improving the degree of reduction and reduction of MgO. The reduction time was shortened to 20 ⁇ 90min, and the recovery rate of magnesium metal was increased to over 88%. At the same time, the reducing slag is directly discharged, and the continuous production of magnesium metal is realized.
  • the present invention eliminates the vacuum system and the vacuum reduction tank, and the equipment is simpler; since the reduction operation is performed under the condition of "relative vacuum” (“relative vacuum”), Simple operation, low equipment requirements, reduced equipment investment and operating costs.
  • the conventional silicon thermal magnesium smelting process is to first calcine dolomite or magnesite, cool, and then press the ball. During the dolomite calcination process, about 5% of the fine powder is not used and is wasted.
  • the method of the present invention directly utilizes uncalcined dolomite or magnesite ore and then calcins the pellets without the problem of waste of fines. Therefore, the raw material utilization rate of the method of the present invention is remarkably improved, and the pollution is remarkably lowered.
  • the technology of the present invention is different from the conventional silicon thermal magnesium smelting technique in that the dolomite or magnesite is directly spheronized, and then Calcined pellets at 850 ⁇ 1050 °C in a protective atmosphere to achieve low temperature rapid calcination of dolomite or magnesite.
  • the calcined pellets are continuously conveyed to a high-temperature reduction furnace without cooling, and are subjected to high-temperature reduction.
  • the residual heat of the calcined tail gas and the residual heat of the high-temperature reducing tail gas are directly used for preheating the pellets and the inert carrier gas. Therefore, the energy consumption of the method of the invention is significantly reduced.
  • the method of the present invention is carried out in a flowing inert argon atmosphere, and the generated high-temperature magnesium vapor is continuously carried by the flowing argon gas, that is, the "relative vacuum” means is adopted, and the vacuum system is eliminated.
  • the vacuum reduction tank realizes the continuous production of magnesium metal and greatly shortens the reduction cycle.
  • the magnesium reduction cycle is shortened from 8 ⁇ 12h in the traditional silicon thermal method to 20 ⁇ 90min.
  • the recovery rate and resource utilization rate of magnesium metal are greatly improved, and the comprehensive recovery rate of magnesium metal is increased to over 88%, and the inert protective carrier gas can be recycled.
  • the technology of the present invention is a green and green process of environmental protection and energy saving, and the cost per production of 1 ton of metal magnesium can be reduced by more than 4,000 yuan.
  • this technology can process a large amount of secondary resources of MgO-rich boron mud to achieve its green clean utilization.
  • the composition of dolomite used is: MgO mass fraction is 21.7%, CaO is 30.5%, the rest is C0 2 , and the total amount of trace impurities is not higher than 2.0%.
  • the composition of the magnesite used is: MgO mass fraction is 47.05%, the rest is C0 2 , and the trace impurity is not higher than 1.5%.
  • the argon gas used was 99.95% high purity argon.
  • the medium frequency induction furnace used has an induction furnace coil diameter of 200 mm.
  • the reduction time referred to in the step 3 of the following examples refers to the residence time of the calcined pellets in the high temperature reduction zone.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite 75Si-Fe alloy: Fluorite according to the mass ratio of 110: 10: 3.0, adding 1.0% of the total mass of the above three materials as the binder and 5.0% of the total mass of the three materials. Water
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, obtain a pellet with a particle size of 5 ⁇ 20mm, and dry the pellet naturally for 24h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a high-temperature furnace and heated to 200 ° C, dehydrated for 45 minutes, then heated to 1050 ° C under an argon atmosphere, and calcined for 30 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the intermediate frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas.
  • high-temperature magnesium vapor is continuously obtained, and mixed with argon gas to form a high-temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1350 ° C , the reduction time is 90min, and the argon flow rate is 4.5m 3 /h ;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 89%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite 75Si-Fe alloy: Fluorite according to the mass ratio of 110: 12: 3.5, add 1.5% of the total mass of the above three materials as the binder and 5.0% of the total mass of the three materials.
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, obtain a pellet with a particle size of 5 ⁇ 20mm, and dry the pellet naturally for 24h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 45 min, then heated to 1000 ° C in a high purity nitrogen atmosphere, and calcined for 60 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the high-temperature resistance furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high-temperature mixed gas, and the reducing slag is continuously discharged to the high-temperature resistance furnace; wherein the reduction temperature is 1450 ° C, the reduction time is 50 min, and the argon gas flow rate is 3.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the high-temperature electric resistance furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 90%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite 75Si-Fe alloy: Fluorite according to the mass ratio of 110: 12: 4.0, adding 2.0% of the total mass of the above three materials as the binder and 4.0% of the total mass of the three materials.
  • Pelletizing Mix the ingredients evenly, use a disc ball machine to make the ball, and obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 12h; Step 2: Pellet calcination
  • the air-dried pellets are placed in a fluidized bed and heated to 250 ° C, dehydrated for 30 minutes, then heated to 950 ° C in a high purity nitrogen atmosphere, and calcined for 70 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1600 ° C, the reduction time is 20 min, and the argon flow rate is 5.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then sent to the jet atomizer through the sealed pipeline, and atomized and condensed to obtain metallic magnesium particles, and the recovery rate of the metallic magnesium is 92%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite A1: Fluorite according to the mass ratio of 115: 10: 2.0, adding 1.0% of the total mass of the above three materials of water glass as the binder and 4.5% of the total mass of the three materials;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 6h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 150 ° C, dehydrated for 60 min, then heated to 850 ° C under an argon atmosphere, and calcined for 120 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high-temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1300 ° C, the reduction time is 90 min, and the argon gas and the flow rate are 2.0 m 3 /h ;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 91.5%.
  • the method for rapidly and continuously smelting magnesium includes the following steps: Step 1: Ingredients for making balls
  • Dolomite A1: Fluorite according to the mass ratio of 115: 12: 2.5, add 1.5% of the total mass of the above three materials of water glass as the binder and 3.0% of the total mass of the three materials;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 2h;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 220 ° C, dehydrated for 50 minutes, then heated to 950 ° C under argon atmosphere, and calcined for 50 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1500 ° C, the reduction time is 45 min, and the argon gas flow rate is 4.2 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 93.0%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite A1: Fluorite according to the mass ratio of 115: 13: 3.0, adding 2.0% of the total mass of the above three materials of water glass as the binder and 2.0% of the total mass of the three materials;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 15mm, and naturally dry the pellet for 20h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 180 ° C, dehydrated for 55 min, then heated to 900 ° C under an argon atmosphere, and calcined for 60 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1550 ° C, the reduction time is 20 min, and the argon flow rate is 5.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 93.5%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Magnesite 75Si-Fe alloy: CaO: Fluorite is added in a mass ratio of 45:10: 16: 2.0, adding 2.0% of the total mass of the above four materials as the binder and four materials. 6.0% of the total mass of water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 18h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 35 minutes, then heated to 1050 ° C under an argon atmosphere, and calcined for 40 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1300 ° C, the reduction time is 90 min, and the argon gas and the flow rate are 3.0 m 3 /h ;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then sent to the jet atomizer through the sealed pipeline, and atomized and condensed to obtain magnesium metal particles, and the recovery rate of the magnesium metal is 90%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Will magnesite 75Si-Fe alloy: CaO: Fluorite according to the mass ratio of 45: 12: 18: 2.5, adding 2.5% of the total mass of the above four materials of water glass as binder and four materials 5.0% of the total mass of water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 10 ⁇ 25mm, and naturally dry the pellet for 10h;
  • Step 2 Pellet calcination
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1400 ° C, the reduction time is 50 min, and the argon flow rate is 4.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 91%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Will magnesite 75Si-Fe alloy: CaO: Fluorite according to the mass ratio of 45: 13: 20: 3.0, adding 3.0% of the total mass of the above four materials as the binder and four materials 3.0% of the total mass of water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 25mm. The pellet is naturally air-dried for 15h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln to a temperature of 210 ° C, dehydrated for 50 minutes, then heated to 950 ° C under an argon atmosphere, and calcined for 70 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1600 ° C, the reduction time is 20 min, and the argon flow rate is 5.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 95%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Will magnesite Ah CaO: Fluorite according to the mass ratio of 48: 10: 15: 2.0 ingredients, adding 2.0% of the total mass of the above four materials of water glass as the binder and the total mass of the four materials of 6.0 % of water; Pelletizing: Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 25mm, and dry the pellet naturally for 8h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 50 min, then heated to 950 ° C under an argon atmosphere, and calcined for 120 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1300 ° C, the reduction time is 80 min, and the argon gas flow rate is 3.5 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 91%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Magnesite Al: CaO: Fluorite is added in a mass ratio of 48: 12: 17: 2.5, adding 2.5% of the total mass of the above four materials as the binder and the total mass of the four materials. 2.0% water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 25mm, and naturally dry the pellet for lh;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 190 ° C, dehydrated for 60 min, then heated to 900 ° C under an argon atmosphere, and calcined at a temperature of lOOmin;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1450 ° C, the reduction time is 40 min, and the argon gas flow rate is 4.5 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed tank path, and subjected to circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 94%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Will magnesite Ah CaO: Fluorite in accordance with the mass ratio of 48: 13: 18: 3.0, add 3.0% of the total mass of the above four materials of water glass as the binder and the total mass of the four materials of 5.0 % of water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 25mm, and naturally dry the pellet for lh;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 45 minutes, then heated to 850 ° C under argon atmosphere, and calcined for 120 minutes.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1600 ° C, the reduction time is 20 min, and the argon flow rate is 5.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the vertical medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 96%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite Al : 75Si-Fe alloy: Fluorite according to the mass ratio of 110: 3.0: 6.5: 3.0, adding 1.0% of the total mass of the above four materials to the water glass as the binder and the total of the four materials 4.0% water by mass;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, obtain a pellet with a particle size of 5 ⁇ 20mm, and dry the pellet naturally for 24h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a high-temperature furnace and heated to 200 ° C, dehydrated for 50 minutes, then heated to 1000 ° C under an argon atmosphere, and calcined for 30 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and Argon is mixed together, The high temperature mixed gas is formed, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1350 ° C, the reduction time is 90 min, and the argon flow rate is 4.5 m 3 /h ;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 90%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 210 ° C, dehydrated for 35 minutes, then heated to 1050 ° C under argon atmosphere, and calcined for 40 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the high-temperature resistance furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high-temperature mixed gas, and the reducing slag is continuously discharged to the high-temperature resistance furnace; wherein the reduction temperature is 1320 ° C, the reduction time is 85 min, and the argon gas flow rate is 3.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the high-temperature electric resistance furnace through the flowing argon gas flow, and then sent to the jet atomizer through the sealed pipeline, and directly atomized and condensed to obtain metallic magnesium particles, and the recovery rate of the metallic magnesium is 92%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite Al: Ca: 75Si-Fe alloy: Fluorite is added in a mass ratio of 110: 2.7: 8.8: 5: 4.0, adding 2.0% of the total mass of the above four materials as a binder and 4.0% of the total mass of the four materials; pelletizing: mixing the ingredients evenly, using a disc pelletizer to make the ball, obtaining a pellet with a particle size of 5 ⁇ 20mm, and drying the pellet naturally for 15h ;
  • Step 2 Pellet calcination The air-dried pellets are placed in a fluidized bed and heated to 240 ° C, dehydrated for 40 minutes, then heated to 980 ° C in a high-purity nitrogen atmosphere, and calcined for 60 minutes;
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace; wherein the reduction temperature is 1500 ° C, the reduction time is 20 min, and the argon flow rate is 5.0 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then sent to the jet atomizer through the sealed pipeline, and directly atomized and condensed to obtain magnesium metal particles, and the recovery rate of the magnesium metal is 91%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 45 minutes, then heated to 950 ° C under argon atmosphere, and calcined for 120 minutes.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace, wherein the reduction temperature is 1400 ° C, the reduction time is 75 min, and the argon gas flow rate is 3.5 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 91%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Step 1 Ingredients for making balls Ingredients: Dolomite: Al: Ca: 75Si-Fe alloy: Fluorite according to the mass ratio of 115: 6.6: 6.6: 2.5: 3.0, adding 2.0% of the total mass of the above five materials to the water glass as a binder and Water of 2.0% of the total mass of the five materials; Build the ball: Mix the ingredients evenly, use a disc pelletizer to make the ball, obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 18h ;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 200 ° C, dehydrated for 50 min, then heated to 900 ° C under an argon atmosphere, and calcined for 60 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace, wherein the reduction temperature is 1500 ° C, the reduction time is 25 min, and the argon gas flow rate is 4.5 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the medium-frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium condensing tank through the sealed pipeline to perform circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 94%.
  • the method for rapidly and continuously smelting magnesium includes the following steps:
  • Dolomite Ca: 75Si-Fe alloy: Fluorite according to the mass ratio of 115: 15.4: 6: 2.0, add 1.0% of the total mass of the above four materials as the binder and the total of the four materials. 4.5% by mass of water;
  • Pelletizing Mix the ingredients evenly, use a disc pelletizer to make the ball, and obtain a pellet with a particle size of 5 ⁇ 20mm, and naturally dry the pellet for 10h;
  • Step 2 Pellet calcination
  • the air-dried pellets are placed in a rotary kiln and heated to 180 ° C, dehydrated for 55 min, then heated to 850 ° C under an argon atmosphere, and calcined for 120 min.
  • Step 3 Continuous high temperature reduction of calcined pellets
  • the calcined high-temperature pellets are continuously fed into the medium-frequency induction furnace through the sealed pipeline without cooling under the protection of argon gas, and then subjected to continuous high-temperature reduction reaction in a flowing argon atmosphere to continuously obtain high-temperature magnesium vapor, and
  • the argon gas is mixed together to form a high temperature mixed gas, and the reducing slag is continuously discharged into the intermediate frequency induction furnace, wherein the reduction temperature is 1350 ° C, the reduction time is 80 min, and the argon gas flow rate is 3.5 m 3 /h;
  • Step 4 Condensation of high temperature magnesium vapor
  • the high-temperature magnesium vapor is carried out of the intermediate frequency induction furnace through the flowing argon gas flow, and then directly carried into the magnesium cold through the sealed pipeline, and subjected to circulating water-cooling condensation to obtain a metal magnesium ingot, and the recovery rate of the magnesium metal is 93%.

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Abstract

一种炼镁方法，包括将白云石或菱镁矿，与还原剂和萤石混合后造球，得到球团；在氮气或氩气气氛下煅烧球团，得到高温球团；在氩气保护下，将高温球团不经冷却，直接送入密闭的高温还原炉中进行高温还原反应，得到高温镁蒸气；通过氩气流将高温镁蒸气带出高温还原炉，冷凝后得到金属镁。该炼镁方法缩短了还原时间，提高了镁回收率。

Description

一种快速连续炼镁的方法
技术领域
本发明属于有色金属冶金技术领域， 特别涉及一种快速连续炼镁的方法。
背景技术
20世纪 50年代， 镁开始进入民用市场。 20世纪 60年代以来， 由于镁在民用市场和空间 技术上的应用， 推动了镁工业的发展， 炼镁方法和生产技术也有了很大突破， 经济效益不断 提高。 世界上炼镁方法主要有电解法和热还原法两大类。 热还原法是以煅烧白云石为原料， 以硅铁为还原剂， 在高温和真空条件下进行还原制得金属镁。 其中最重要的是皮江法炼镁， 由于工艺简单， 生产成本大幅降低， 使全世界的原镁产量大幅增加。 皮江法炼镁具有方法简 单， 投资成本低等优点。但是皮江法炼镁需要在高温和真空条件下进行， 操作为间歇性操作、 劳动强度大， 存在着还原周期长（需要 10~12h)， 金属镁产率低 （30kg/还原罐）， 以及能耗高 等缺点。 由于还原罐长时间在高温和高真空条件下使用， 致使还原罐寿命降低， 生产成本增 高。 同时所用原料白云石首先要经过煅烧， 煅烧产生的超细粉料无法利用， 造成严重的资源 浪费。
针对传统硅热法炼镁存在还原周期长， 生产成本高等缺点， 国内从核心设备、 关键工艺 突破角度， 先后开发出新型炼镁装置、 以及铝热法炼镁和钙热法炼镁新思路。 例如， 专利"申 请号： 200710035929.8"和"专利号： ZL96247592.0"等设计了感应加热炼镁装置。 其中专利"申 请号： 200710035929.8"还设计出采用多套加料装置和多套镁蒸汽冷凝装置组合， 实现炼镁的 机械化操作。夏德宏等人研究了采用液态钙热还原法炼镁的思路， 通过操作工艺条件的优化， 提高了操作的自动化水平。 专利"申请号： 200510045888.1 "和"申请号： 200910236975.3"开发 了新型金属热还原法炼镁新思路，专利"申请号 : 200510045888.1 "研究了铝热还原法炼镁思路， 使得还原温度降低了 50°C， 还原时间缩短到 7~8h。 专利"申请号： 200910236975.3"研究了采 用 Si-Fe+Al+Ca复合还原剂还原煅白和苛性菱镁矿混合物的炼镁工艺， 使得还原时间缩短到 5-9h。 以上研究在一定程度上提高了热法炼镁的技术水平， 但是以上研究都还在建立在传统 的硅热法炼镁工艺基础上， 都还是基于高温真空这一基本思路的改进和提高， 并没有本质上 的突破。 因此， 传统的硅热炼镁所存在的还原周期长， 能耗高、 还原罐寿命短以及生产成本 高等缺点， 仍旧得不到根本解决。
发明内容
针对现有热法炼镁生产及研究所存在的缺点和不足， 解决传统的硅热炼镁所存在的还原 周期长， 能耗高、 还原罐寿命短以及生产成本高等缺点， 本发明提供一种快速连续炼镁的方 法， 即在流动的惰性气体中进行高温还原， 同时生成的高温镁蒸汽被流动的惰性载气立即携 带走， 冷凝得到金属镁。 本发明方法反应速度快， 还原时间缩短到 90min以内， 镁的回收率 提高到 88%以上， 同时实现了镁的连续生产。
本发明的快速连续炼镁的方法， 包括直接造球团、 球团煅烧、 煅烧球团在流动氩气气氛 中高温还原、 高温镁蒸汽的冷凝等步骤。 其中， 直接造球团是指将未经煅烧处理的白云石或 菱镁矿， 与还原剂和萤石按比例混合好， 采用圆盘造球机造成直径 5~20mm的球团； 球团煅 烧是指将球团在氩气或氮气气氛下中 850~1050°C温度下煅烧 30~120min， 排除球团中的水分 和挥发性物质， 使其中的碳酸盐分解放出 C02， 同时还原剂会在煅烧过程中经扩散与分解生 成的 MgO接触更充分； 煅烧球团高温还原是指在 "相对真空"气氛中将煅烧后的球团在流动 的氩气气氛中进行高温还原反应， 反应生成的高温镁蒸汽立即被流动的氩气载气携带走。 对 于每一个反应界面来讲， 由于生成的高温镁蒸汽立即被携带离开了反应界面， 所以对于反应 界面上的高温镁蒸汽来讲， 其分压一直远低于 latm， 即处于相对的 "负压状态"。 因此， 对 于生成镁蒸汽的还原反应界面上的氛围， 就好像一个密闭的容器抽了真空一样， 称之为 "相 对真空 "或"相对负压"， 这为反应的发生提供了更充分的热力学及动力学条件； 镁蒸汽的冷 凝是指将由高温还原炉中氩气气体连续携带出来的高温镁蒸汽快速冷凝得到金属镁的过程。
本发明的快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： 75Si-Fe合金： 萤石， 按照质量比为 110: ( 10-13 )： ( 3.0~4.0) 配料， 混合均匀， 然后添加配料总质量的 1.0~2.0%的水玻璃作为粘结剂和配料总质量的 2.0~5.0%的 水；
或将白云石： A1: 萤石， 按照质量比为 115 : ( 10-13 )： (2.0-3.0) 配料， 混合均匀， 然 后添加配料总质量的 1.0~2.0%的水玻璃作为粘结剂和配料总质量的 2.0~5.0%的水；
造球： 将配料混合均匀， 造球， 得到粒径为 5~20mm的球团， 将球团自然风干 10~24h; 步骤 2: 球团煅烧
将风干好的球团， 放在高温炉、 回转窑或流化床中升温到 150~250°C， 保温 30~60min脱 水， 然后在氩气或氮气气氛下升温到 850~1050°C， 保温煅烧 30~120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下连续送入到密闭的高温还原炉中， 然后在 流动的氩气气氛中进行高温还原反应， 还原温度为 1300~1600°C， 还原时间 20~90min， 氩气 流量为 2.0~5.0m3/h， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把 还原渣连续排出高温还原炉； 步骤 4: 高温镁蒸汽的冷凝
高温镁蒸汽通过流动的氩气流携带出高温还原炉， 通过密封管路输送到冷凝系统， 进行 冷凝， 得到金属镁。
本发明的快速连续炼镁的方法， 也可以具体包括如下步骤：
步骤 1 : 配料造球
配料：将菱镁矿： 75Si-Fe合金： CaO:萤石，按照质量比为 45： ( 10-13 )：( 16-20)： ( 2.0-3.0 ) 配料， 混合均匀， 然后添加配料总质量的 2.0~3.0%的水玻璃作为粘结剂和配料总质量的 2.0~6.0%的水；
或将菱镁矿： Al : CaO: 萤石按照质量比为 48 : ( 10-13 )： ( 15-18)： ( 2.0-3.0 ) 配料， 混合均匀， 然后添加配料总质量的 2.0~3.0%的水玻璃作为粘结剂和配料总质量的 2.0~6.0%的 水；
步骤 2: 球团煅烧
将风干好的球团， 放在高温炉、 回转窑或流化床中升温到 150~250°C， 保温 30~60min脱 水， 然后在氩气或氮气气氛下升温到 850~1050°C， 保温煅烧 30~120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下连续送入到密闭的高温还原炉中， 然后在 流动的氩气气氛中进行高温还原反应， 还原温度为 1300~1600°C， 还原时间 20~90min， 氩气 流量为 2.0~5.0m3/h， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把 还原渣连续排出高温还原炉；
步骤 4: 高温镁蒸汽的冷凝
高温镁蒸汽通过流动的氩气流携带出高温还原炉， 通过密封管路输送到冷凝系统， 进行 冷凝， 得到金属镁。
上述的快速连续炼镁的方法， 步骤 1中的配料 A1或 75Si-Fe合金， 用复合还原剂代替， 复合还原剂为以下三种中的一种：
( 1 ) Al+75Si-Fe合金； （2) Ca+75Si-Fe合金； （3 ) Al+Ca+75Si-Fe合金；
复合还原剂的用量标准为： 1质量单位的 A1可用 2.2倍质量单位的 Ca代替； 1质量单位 的 75Si-Fe合金可用 2.2倍质量单位的 Ca代替； 1质量单位的 A1和 1质量单位的 75Si-Fe合 金相当。
所述的步骤 1中造球时采用圆盘造球机； 步骤 3中高温还原炉为中频感应炉或高温电阻 炉；
所述的步骤 4中的冷凝方式为直接冷凝或雾化冷凝， 直接冷凝方式为循环水冷冷凝。 所述的 75Si-Fe合金为： Si质量含量为 75%的 Si-Fe合金。
上述步骤 2球团煅烧过程中， 发生的化学反应如下：
以白云石为原料时：
MgC03-CaC03=MgO-CaO+2C02 ( 1 )
以菱镁矿为原料时：
MgC03=MgO +C02 (2)
煅烧使得球团中的 MgC03、 CaC03彻底分解， 高温煅烧过程中球团进一步烧结， 其中金 属还原剂经过扩散与 MgO接触更充分，为下一步的高温还原生成高温镁蒸汽创造了更充分的 动力学条件。
上述步骤 3煅烧球团高温还原， 反应方程式如下：
以白云石为原料时：
2MgO-CaO +Si=2Mg(g)†+2CaO-Si02 ( 3 )
3MgO-CaO +2Al=3Mg(g)†+3CaO-2Al203 (4)
以菱镁矿为原料时：
2MgO+2CaO +Si=2Mg(g)†+2CaO-Si02 ( 5 )
21MgO+12CaO +14Al=21Mg(g)†+12CaO-7Al203 (6)
由于高温还原反应是在流动的惰性氩气气氛中进行， 因此在球团反应界面上生成的高温 镁蒸汽立即被流动的氩气携带走， 因此在反应界面上对温镁蒸汽来讲， 始终处于一个分压远 低于 latm的负压状态， 即所谓的 "相对真空"或 "相对负压"。 由于生成的高温镁蒸汽随时 被惰性氩气携带， 将促进高温还原生成镁蒸汽的反应（3 ) 〜 (6) 向右彻底进行， 极大地提高 了 MgO的还原程度和还原速度。 还原时间缩短到 20~90min， 金属镁的回收率提高到 88%以 上。 同时还原渣直接排出， 实现了金属镁的连续生产。
本发明的快速连续炼镁的方法与已有技术相比的具有如下优点：
( 1 )与传统的硅热法炼镁技术相比， 本发明取消了真空系统以及真空还原罐， 设备更简 单； 由于还原操作是在 "相对真空"（"相对负压"）条件下进行， 操作简单， 设备要求低， 降 低了设备投资及操作成本。
(2)传统的硅热法炼镁是先将白云石或菱镁矿煅烧、 冷却， 然后压球。 白云石煅烧过程 中会产生 5%左右的粉细料无法使用而浪费。本发明方法是直接利用未煅烧白云石或菱镁矿造 球， 然后煅烧球团， 不存在粉细料浪费的问题。 因此， 本发明方法的原料利用率显著提高， 污染显著降低。
(3 )本发明技术与传统的硅热法炼镁技术不同， 首先将白云石或菱镁矿直接造球， 然后 在保护性气氛中 850~1050°C煅烧球团， 实现了白云石或菱镁矿的低温快速煅烧。 并将煅烧球 团不经冷却连续输送到高温还原炉中进行高温还原， 煅烧尾气余热以及高温还原尾气余热直 接用来预热球团及惰性载气。 因此， 本发明方法的能耗显著降低。
(4)本发明方法由于高温还原过程是在流动的惰性氩气气氛环境中进行， 生成的高温镁 蒸汽被流动的氩气连续携带走， 即采用了 "相对真空"手段， 取消了真空系统和真空还原罐， 实现了金属镁的连续生产， 极大地缩短了还原周期。 使得镁还原周期由传统硅热法的 8~12h， 缩短到 20~90min。 大大提高了金属镁的回收率和资源利用率， 金属镁的综合回收率提高到 88%以上， 同时惰性保护载气可循环利用。 因此， 本发明技术是环保、 节能的绿色新工艺， 每生产生产 1吨金属镁成本可降低 4000元以上。 同时， 本技术可以处理大量的富含 MgO的 硼泥二次资源， 实现其绿色清洁利用。
具体实施方式
以下实施例中：
所采用的白云石组成为： MgO质量分数为 21.7%， CaO为 30.5%， 其余为 C02， 微量杂 质总量不高于 2.0%。
所采用的菱镁矿组成为： MgO质量分数为 47.05%， 其余为 C02， 微量杂质不高于 1.5%。 所采用的氩气为 99.95%的高纯氩气。
所采用的圆盘造球机的直径 O=1000mm， 边高 h=300mm， 倾角 α=45°， 转速 28rpm。 所采用的中频感应炉， 感应炉线圈直径为 200mm。
以下实施例步骤 3中所指的还原时间是指煅烧球团在高温还原区的停留时间。
实施例 1
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： 75Si-Fe合金： 萤石按照质量比为 110: 10： 3.0配料， 添加上述三种物 料总质量的 1.0%的水玻璃作为粘结剂和三种物料总质量的 5.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 24h;
步骤 2: 球团煅烧
将风干好的球团， 放在高温炉中升温到 200°C， 保温 45min脱水， 然后在氩气气氛下升 温到 1050°C， 保温煅烧 30min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1350°C， 还原时间 90min, 氩气流量为 4.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 89%。
实施例 2
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： 75Si-Fe合金： 萤石按照质量比为 110: 12： 3.5配料， 添加上述三种物 料总质量的 1.5%的水玻璃作为粘结剂和三种物料总质量的 5.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 24h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 45min脱水， 然后在高纯氮气气氛 下升温到 1000°C， 保温煅烧 60min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入高温电阻炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出高温电阻炉； 其中还原温度为 1450°C， 还原时间 50min, 氩气流量为 3.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出高温电阻炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 90%。
实施例 3
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： 75Si-Fe合金： 萤石按照质量比为 110: 12： 4.0配料， 添加上述三种物 料总质量的 2.0%的水玻璃作为粘结剂和三种物料总质量的 4.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 12h; 步骤 2: 球团煅烧
将风干好的球团， 放在流化床中升温到 250°C， 保温 30min脱水， 然后在高纯氮气气氛 下升温到 950°C， 保温煅烧 70min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1600°C， 还原时间 20min, 氩气流量为 5.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路输送到射流雾化 器， 雾化冷凝得到金属镁颗粒， 金属镁的回收率 92%。
实施例 4
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： A1: 萤石按照质量比为 115 : 10： 2.0配料， 添加上述三种物料总质量 的 1.0%的水玻璃作为粘结剂和三种物料总质量的 4.5%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 6h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 150°C， 保温 60min脱水， 然后在氩气气氛下升 温到 850°C， 保温煅烧 120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1300°C， 还原时间 90min, 氩气、流量为 2.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 91.5%。
实施例 5
快速连续炼镁的方法， 具体包括如下步骤： 步骤 1 : 配料造球
配料： 将白云石： A1: 萤石按照质量比为 115 : 12： 2.5配料， 添加上述三种物料总质量 的 1.5%的水玻璃作为粘结剂和三种物料总质量的 3.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 2h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 220°C， 保温 50min脱水， 然后在氩气气氛下升 温到 950°C， 保温煅烧 50min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1500°C， 还原时间 45min, 氩气流量为 4.2m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 93.0%。
实施例 6
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： A1: 萤石按照质量比为 115 : 13： 3.0配料， 添加上述三种物料总质量 的 2.0%的水玻璃作为粘结剂和三种物料总质量的 2.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~15mm的球团， 将球团自 然风干 20h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 180°C， 保温 55min脱水， 然后在氩气气氛下升 温到 900°C， 保温煅烧 60min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1550°C， 还原时间 20min, 氩气流量为 5.0m3/h; 步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 93.5%。
实施例 7
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： 75Si-Fe合金： CaO: 萤石按照质量比为 45 : 10： 16： 2.0配料， 添加 上述四种物料总质量的 2.0%的水玻璃作为粘结剂和四种物料总质量的 6.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 18h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 35min脱水， 然后在氩气气氛下升 温到 1050°C， 保温煅烧 40min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1300°C， 还原时间 90min, 氩气、流量为 3.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路输送到射流雾化 器， 雾化冷凝得到金属镁颗粒， 金属镁的回收率 90%。
实施例 8
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： 75Si-Fe合金： CaO: 萤石按照质量比为 45 : 12： 18： 2.5配料， 添加 上述四种物料总质量的 2.5%的水玻璃作为粘结剂和四种物料总质量的 5.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 10~25mm的球团， 将球团自 然风干 10h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 250°C， 保温 40min脱水， 然后在氩气气氛下升 温到 1000°C， 保温煅烧 90min; 步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1400°C， 还原时间 50min, 氩气流量为 4.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 91%。
实施例 9
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： 75Si-Fe合金： CaO: 萤石按照质量比为 45 : 13： 20： 3.0配料， 添加 上述四种物料总质量的 3.0%的水玻璃作为粘结剂和四种物料总质量的 3.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~25mm的球团， 将球团自 然风干 15h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 210°C， 保温 50min脱水， 然后在氩气气氛下升 温到 950°C， 保温煅烧 70min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1600°C， 还原时间 20min, 氩气流量为 5.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 95%。
实施例 10
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： Ah CaO: 萤石按照质量比为 48: 10： 15： 2.0配料， 添加上述四种物 料总质量的 2.0%的水玻璃作为粘结剂和四种物料总质量的 6.0%的水； 造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~25mm的球团， 将球团自 然风干 8h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 50min脱水， 然后在氩气气氛下升 温到 950°C， 保温煅烧 120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1300°C， 还原时间 80min, 氩气流量为 3.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 91%。
实施例 11
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： Al: CaO: 萤石按照质量比为 48: 12： 17： 2.5配料， 添加上述四种物 料总质量的 2.5%的水玻璃作为粘结剂和四种物料总质量的 2.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~25mm的球团， 将球团自 然风干 lh;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 190°C， 保温 60min脱水， 然后在氩气气氛下升 温到 900°C， 保温煅烧 lOOmin;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1450°C， 还原时间 40min, 氩气流量为 4.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封罐路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 94%。 快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： Ah CaO: 萤石按照质量比为 48: 13： 18： 3.0配料， 添加上述四种物 料总质量的 3.0%的水玻璃作为粘结剂和四种物料总质量的 5.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~25mm的球团， 将球团自 然风干 lh;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 45min脱水， 然后在氩气气氛下升 温到 850°C， 保温煅烧 120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1600°C， 还原时间 20min, 氩气流量为 5.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出竖式中频感应炉， 然后通过密封管路直接携带入 镁冷凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 96%。
实施例 13
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： Al: 75Si-Fe合金： 萤石按照质量比为 110: 3.0： 6.5： 3.0配料， 添加 上述四种物料总质量的 1.0%的水玻璃作为粘结剂和四种物料总质量的 4.0%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 24h;
步骤 2: 球团煅烧
将风干好的球团， 放在高温炉中升温到 200°C， 保温 50min脱水， 然后在氩气气氛下升 温到 1000°C， 保温煅烧 30min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1350°C， 还原时间 90min, 氩气流量为 4.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 90%。
实施例 14
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： Ca: 75Si-Fe合金： CaO: 萤石按照质量比为 45 : 17.6： 3： 16： 2.0配 料， 添加上述四种物料总质量的 2.0%的水玻璃作为粘结剂和四种物料总质量的 6.0%的水； 造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 20h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 210°C， 保温 35min脱水， 然后在氩气气氛下升 温到 1050°C， 保温煅烧 40min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入高温电阻炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出高温电阻炉； 其中还原温度为 1320°C， 还原时间 85min, 氩气流量为 3.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出高温电阻炉， 然后通过密封管路输送到射流雾化 器， 直接雾化冷凝得到金属镁颗粒， 金属镁的回收率 92%。
实施例 15
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： Al: Ca: 75Si-Fe合金： 萤石按照质量比为 110: 2.7： 8.8： 5： 4.0配 料， 添加上述四种物料总质量的 2.0%的水玻璃作为粘结剂和四种物料总质量的 4.0%的水； 造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 15h;
步骤 2: 球团煅烧 将风干好的球团， 放在流化床中升温到 240°C， 保温 40min脱水， 然后在高纯氮气气氛 下升温到 980°C， 保温煅烧 60min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉； 其中还原温度为 1500°C， 还原时间 20min, 氩气流量为 5.0m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路输送到射流雾化 器， 直接雾化冷凝得到金属镁颗粒， 金属镁的回收率 91%。
实施例 16
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将菱镁矿： Al: 75Si-Fe合金： CaO: 萤石按照质量比为 48: 4.6： 7： 15： 2.0配 料， 添加上述五种物料总质量的 2.0%的水玻璃作为粘结剂和五种物料总质量的 6.0%的水； 造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~25mm的球团， 将球团自 然风干 10h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 45min脱水， 然后在氩气气氛下升 温到 950°C， 保温煅烧 120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉， 其中还原温度为 1400°C， 还原时间 75min, 氩气流量为 3.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 91%。
实施例 17
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球 配料： 将白云石： Al: Ca: 75Si-Fe合金： 萤石按照质量比为 115 : 6.6： 6.6： 2.5： 3.0配 料， 添加上述五种物料总质量的 2.0%的水玻璃作为粘结剂和五种物料总质量的 2.0%的水； 造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 18h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 200°C， 保温 50min脱水， 然后在氩气气氛下升 温到 900°C， 保温煅烧 60min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉， 其中还原温度为 1500°C， 还原时间 25min, 氩气流量为 4.5m3/h;
步骤 4: 高温镁蒸汽的冷凝
将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 凝罐， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 94%。
实施例 18
快速连续炼镁的方法， 具体包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： Ca: 75Si-Fe合金： 萤石按照质量比为 115 : 15.4： 6： 2.0配料， 添加 上述四种物料总质量的 1.0%的水玻璃作为粘结剂和四种物料总质量的 4.5%的水；
造球： 将配料混合均匀， 采用圆盘造球机造球， 得到粒径为 5~20mm的球团， 将球团自 然风干 10h;
步骤 2: 球团煅烧
将风干好的球团， 放在回转窑中升温到 180°C， 保温 55min脱水， 然后在氩气气氛下升 温到 850°C， 保温煅烧 120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下通过密封管路连续送入中频感应炉中， 然 后在流动的氩气气氛中进行连续高温还原反应， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把还原渣连续排出中频感应炉， 其中还原温度为 1350°C， 还原时间 80min, 氩气流量为 3.5m3/h;
步骤 4: 高温镁蒸汽的冷凝 将高温镁蒸汽通过流动的氩气流携带出中频感应炉， 然后通过密封管路直接携带入镁冷 ， 进行循环水冷冷凝， 得到金属镁铸锭， 金属镁的回收率 93%。

Claims

权 利 要 求 书
1.一种快速连续炼镁的方法， 其特征在于， 包括如下步骤：
步骤 1 : 配料造球
配料： 将白云石： 75Si-Fe合金: 萤石， 按照质量比为 110: ( 10-13 )： ( 3.0~4.0 ) 配料， 混合均匀， 然后添加配料总质量的 1.0~2.0%的水玻璃作为粘结剂和配料总质量的 2.0~5.0%的 水；
或将白云石： A1: 萤石， 按照质量比为 115 : ( 10-13 )： (2.0-3.0) 配料， 混合均匀， 然 后添加配料总质量的 1.0~2.0%的水玻璃作为粘结剂和配料总质量的 2.0~5.0%的水；
造球： 将配料混合均匀， 造球， 得到粒径为 5~20mm的球团， 将球团自然风干 10~24h; 步骤 2: 球团煅烧
将风干好的球团， 放在高温炉、 回转窑或流化床中升温到 150~250°C， 保温 30~60min脱 水， 然后在氩气或氮气气氛下升温到 850~1050°C， 保温煅烧 30~120min;
步骤 3 : 煅烧球团连续高温还原
将煅烧后的高温球团， 不经冷却在氩气保护下连续送入到密闭的高温还原炉中， 然后在 流动的氩气气氛中进行高温还原反应， 还原温度为 1300 1600°C， 还原时间 20~90min， 氩气 流量为 2.0~5.0m3/h， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把 还原渣连续排出高温还原炉；
步骤 4: 高温镁蒸汽的冷凝
高温镁蒸汽通过流动的氩气流携带出高温还原炉， 通过密封管路输送到冷凝系统， 进行 冷凝， 得到金属镁。
2. 一种快速连续炼镁的方法， 其特征在于， 步骤 1中的配料方式为：
步骤 1 : 配料造球
配料：将菱镁矿： 75Si-Fe合金： CaO:萤石，按照质量比为 45： ( 10-13 )：( 16-20)： ( 2.0-3.0 ) 配料， 混合均匀， 然后添加配料总质量的 2.0~3.0%的水玻璃作为粘结剂和配料总质量的 2.0~6.0%的水；
或将菱镁矿： Al : CaO: 萤石按照质量比为 48： ( 10-13 )： ( 15-18)： ( 2.0-3.0) 配料， 混合均匀， 然后添加配料总质量的 2.0~3.0%的水玻璃作为粘结剂和配料总质量的 2.0~6.0%的 水；
步骤 2: 球团煅烧
将风干好的球团， 放在高温炉、 回转窑或流化床中升温到 150~250°C， 保温 30~60min脱 水， 然后在氩气或氮气气氛下升温到 850~1050°C， 保温煅烧 30~120min;
步骤 3 : 煅烧球团连续高温还原 将煅烧后的高温球团， 不经冷却在氩气保护下连续送入到密闭的高温还原炉中， 然后在 流动的氩气气氛中进行高温还原反应， 还原温度为 1300 1600°C， 还原时间 20~90min， 氩气 流量为 2.0~5.0m3/h， 连续得到高温镁蒸汽， 并与氩气混合在一起， 形成高温混合气， 同时把 还原渣连续排出高温还原炉；
步骤 4: 高温镁蒸汽的冷凝
高温镁蒸汽通过流动的氩气流携带出高温还原炉， 通过密封管路输送到冷凝系统， 进行 冷凝， 得到金属镁。
3. 如权利要求 1或 2所述的快速连续炼镁的方法， 其特征在于， 步骤 1中的配料 A1或 75Si-Fe合金， 用复合还原剂代替， 复合还原剂为以下三种中的一种：
( 1 ) Al+75Si-Fe合金； （2) Ca+75Si-Fe合金； （3 ) Al+Ca+75Si-Fe合金；
复合还原剂的用量标准为： 1质量单位的 A1可用 2.2倍质量单位的 Ca代替； 1质量单位 的 75Si-Fe合金可用 2.2倍质量单位的 Ca代替； 1质量单位的 A1和 1质量单位的 75Si-Fe合 金相当。
4. 如权利要求 1或 2所述的快速连续炼镁的方法， 其特征在于， 所述的步骤 4中的冷凝 方式为直接冷凝或雾化冷凝。
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