CN110257646A - A kind of process for smelting magnesium and device - Google Patents
A kind of process for smelting magnesium and device Download PDFInfo
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- CN110257646A CN110257646A CN201910515097.2A CN201910515097A CN110257646A CN 110257646 A CN110257646 A CN 110257646A CN 201910515097 A CN201910515097 A CN 201910515097A CN 110257646 A CN110257646 A CN 110257646A
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- magnesium
- raw material
- smelting
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Classifications
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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
- 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
Abstract
The invention discloses a kind of process for smelting magnesium and devices.Disclosed process for smelting magnesium includes: to prepare pressure forming after raw material mixes for siliceous and magnesium mine, it is characterized in that, under the conditions of 13-4000Pa, after shaping raw material is heated to 600-1100 DEG C, directly apply voltage on shaping raw material, application voltage swing is 10-200V/mm, applies a length of 1-5min when voltage.Disclosed magnesium smelting device includes vacuum smelting furnace, and a pair of electrodes is equipped in the vacuum smelting furnace, for directly applying voltage to the shaping raw material during refining magnesium.The present invention overcomes the series of problems such as traditional ferrosilicon process reducing metal magnesium temperature height, time length, reduction apparatus temperature is greatly lowered, increases substantially magnesium metal reduction speed, metal magnesium slag can be used as cement class materials'use, it is environmentally protective, there is important economic benefit and social benefit.
Description
Technical field
The invention belongs to metallurgical industry fields, and in particular to a kind of magnesium metal silicothermic reduction technique and device.
Background technique
Silicothermic process carries out reduction reaction as reducing agent under high temperature, high vacuum condition, with silicon, produces magnesium metal.This
Method is known as magnesium-smelting silicothermic process.Since ferrosilicon property is stable, reproducibility is strong, relative low price, reduction reaction conditions are easy to reach
To and control so that silicothermic process smelting magnesium technique become the world today refining magnesium industry in other than electrolysis method the most
A kind of widely applied process for smelting magnesium.Especially almost become the main method of production magnesium metal in Chinese magnesium-smelting silicothermic process.
According to the technical process and equipment difference of refining magnesium, silicothermic process specifically includes that Pidgeon process (Pidgeon
Process), bohr letter promise method (Bolzano Process) and mug(unit of measure) Nei Mufa (Magnetherm Process), Pidgeon process category
In external heating, bohr pricks nurse technique in promise technique and mug(unit of measure) and belongs to synthesis by internal resistance electric melting.
Pidgeon process thermal reduction process for smelting magnesium is the main method for producing magnesium metal, and production of magnesium by pidgeonprocess technique is in high temperature
White (MgO is forged with what No. 75 ferrosilicon were formed after dolomite calcination under the conditions of (1150~1250 DEG C) and high vacuum (1~13Pa)
CaO extraction of metal magnesium in), reaction generates metal magnesium vapor in reductive jar, and magnesium metal steam obtains crude magnesium by condensation-crystallization,
Crude magnesium obtains the higher commodity magnesium of purity using refining later.
The also known as interior thermal reduction of bohr letter promise method (Bolzano), raw material used is as principle and Pidgeon process.It will forge
Forging after white powder, ferrosilicon powder and Fluorspar Powder mix well according to a certain percentage after burning is pressed into bricked pelletizing, and pelletizing is put into
Vacuum-thermal reduction is carried out in vacuum reduction furnace, reduction furnace size is about φ 2m × 5m, outer steel shell, interior block refractory material.With Pi Jiang
Method is used using lump coal or coal gas as reductive jar, the mode difference of indirect heating pelletizing, bohr letter promise method is heated outside heat source
Be internal heating method, there are several concatenated resistance rings in inside, and brick shape pelletizing, which is placed directly on resistance ring, realizes heating, energy
The utilization rate in source is higher than Pidgeon process, and thermal losses is few, there is higher heating efficiency, allows the technique using bigger true of internal diameter
Empty reductive jar is conducive to the raising of production capacity.The technique is carried out at 1250 DEG C and lower than under 400Pa, and reaction temperature is higher, the production of magnesium
Extracting rate is high, and the consumption of raw material is few.This method due to using inside heating method, only play storage and insulation effect, be not required to by reduction room
Expensive high temperature resistant chrome-nickel steel reductive jar is consumed, equipment cost reduces.The advantages of this method is to greatly improve
The heat utilization efficiency of the energy;Disadvantage has that mechanization degree is low, and loading and unloading is difficult, and resistance heater is easy to be corroded by reaction mass, makes
Unstable at the electric heating parameter of electric heating element, the service life is short, high production cost.
Nurse (Magnetherm) method is a kind of production magnesium metal to grow up in France in the sixties in 20th century in mug(unit of measure)
Technique.Its main equipment is similar to a vacuum mineral hot furnace, and stove is had outside the steel of thermal insulation material using carbon lining and interior block
Shell sealing, is heated using inside resistance material.Reaction furnace charge is added in reduction furnace in the form of block-like, the reaction in reduction furnace
For temperature between 1400~1600 DEG C, vacuum condition is 400~4000Pa.In reaction furnace charge, except dolime and reduction
Outside agent ferrosilicon, there are also calcined bauxite, the purpose that bauxite is added is fusing point in order to reduce slag, the aluminium oxide in bauxite
Can with ferrosilicon with forge it is white react generate reduzate calcium orthosilicate chemical combination generate be in molten condition slag.Utilize electrical conductivity of molten slag
The heat of generation heats furnace charge, increase heat transfer efficiency and ferrosilicon between furnace charge and forges the contact area between white, can be with
It carries out the reduction process of magnesia more thorough, improves magnesium metal reduction efficiency.Mug(unit of measure) Nei Mufa realizes method for smelting magnesium by hot half
Continuous operations, can continuous charging, slagging-off, it is semicontinuous go out magnesium.The advantages of this method is that reaction speed is fast, and single furnace output is big, is lacked
Point is reaction temperature height, and technique is unstable, and the purity of product is not high.Therefore this method is not widely applied.
Summary of the invention
For domestic and international the deficiencies in the prior art, the present invention provides a kind of process for smelting magnesium and device.
Process for smelting magnesium provided by the invention includes: to prepare pressure forming after raw material mixes for siliceous and magnesium mine, 13-
Under the conditions of 4000Pa, after shaping raw material is heated to 600-1100 DEG C, directly applies voltage on shaping raw material, it is big to apply voltage
Small is 10-200V/mm, applies a length of 1-5min when voltage.
Optionally, the raw material for preparing is made of the ferrosilicon, dolime and fluorite of rational proportion.
Optionally, the shaping raw material shape is regular cylinder or regular block shape.
Magnesium smelting device provided by the invention includes vacuum smelting furnace, which is characterized in that one is equipped in the vacuum smelting furnace
Vacuum condition control to electrode, for directly applying voltage to the shaping raw material during refining magnesium, in the vacuum smelting furnace
Range are as follows: 13-4000Pa, temperature controlling range are as follows: 600-1100 DEG C.
Optionally, multipair electrode is equipped in the vacuum smelting furnace.
Compared with prior art, the beneficial effect of magnesium metal reduction method of the invention is:
Compared to existing smelting silicothermic process magnesium method, vacuum condition of the present invention requires low (existing to require to be lower than 13Pa), furnace
Temperature is low, preparation time is fast, has the advantages that high production efficiency and energy conservation.
Metal magnesium slag can comprehensively utilize in the further improved scheme of the present invention, open up a kind of green of magnesium metal reduction
New technology.
Detailed description of the invention
Fig. 1 is one of the structural schematic diagram of apparatus of the present invention;
Fig. 2 is the second structural representation of apparatus of the present invention.
Specific embodiment
It is identical as the raw material of magnesium-smelting silicothermic process to be suitable for the invention raw material, silicon and magnesium mine are at least contained in raw material.Wherein
The raw material sources of silicon are Antaciron, silico-aluminum etc., magnesium mine such as dolomite, magnesite etc..
Raw material proportioning involved in present invention process, mixing, pressure forming method are identical as magnesium-smelting silicothermic process, difference
It is in raw material of the invention is blocky in regular columnar, such as cylindrical body, square columns, or rule after forming, can be effective
Apply voltage, carries out energization reaction.
" V/mm " of the invention is that alive unit is directly applied on shaping raw material, indicates every millimeter in shaping raw material
Alive size is applied in length, wherein the length direction of shaping raw material is that shaping raw material is mounted on the latter between one group of electrode
Electrode is to the direction of another electrode.
In view of the comprehensive utilization of cinder, of the invention preparing can add bauxite or aluminium hydroxide etc. in raw material former containing aluminium
Material, resulting metal magnesium slag can be used as cement class materials'use after adding aluminum-containing raw material, for convenient for considering metal cinder conduct
The quality of cement class material, each ingredient under the technique in raw material can be according to silicon rate, the size of aluminium rate and lime saturation factor
Control, silicon rate expression therein prepare the mass ratio of the sum of silica content and aluminium oxide and iron oxide in raw material;Aluminium rate indicates
Prepare quality of alumina and iron oxide mass ratio in raw material;Lime saturation factor expression prepares silica in raw material and is oxidized
Calcium is saturated the degree at tricalcium silicate.
Magnesium smelting device of the invention is that electricity is arranged in vacuum smelting furnace wherein on the basis of smelting silicothermic process magnesium apparatus
Pole directly applies voltage to shaping raw material in the process for refining magnesium.According to process requirement, multiple groups can be set in vacuum smelting furnace
Electrode, while energization reaction is carried out to shaping raw material.
It is identical with smelting silicothermic process magnesium apparatus to be, it may be implemented to vacuumize the function with temperature control on vacuum metling furnace body;And
And the heating method of vacuum smelting furnace has internal heat type and external-heat, wherein internal heat type is that the heat such as auxiliary heating element are equipped in furnace
Source, such as electrical-heating source;The structural formula of external-heat is externally provided with heating device in furnace body, such as flame or hot air heating apparatus.Into one
More set vacuum smelting furnaces can be arranged when using external-heat furnace body in step simultaneously, use unified external heat source for more set vacuum smelting furnaces
External heat source is provided.
It is the specific embodiment that inventor provides below, to be further explained explanation to technical solution of the present invention.
Embodiment 1:
It is that white (forge white is mineral aggregate after dolomite, magnesite pre-burning, main component to forging for 36wt% by content of magnesia
For magnesia and calcium oxide) with ferrosilicon, fluorite ingredient is carried out according to 100:20:5 mass ratio, ball milling arrived 200 mesh screen residues 8%,
25Mpa forming under the pressure is diameter 6mm, length is the cylindric of 12mm;
Shaping raw material is placed in vacuum reduction furnace between two electrodes, is evacuated to 100Pa, shaping raw material is heated to
After 700 DEG C, directly apply on shaping raw material voltage 600V (50V/mm), current control is at 0.4 ampere, and be powered reaction 3 minutes
After cool down.
The entire technique of the embodiment is time-consuming: heating 1 hour, energization 3min, 1.5 hours cooling.
The content of magnesia becomes 8% from 30.24% in measurement sample, magnesia reduction rate 74%.
Embodiment 2:
Forge white and sial, fluorite that content of magnesia is 35wt% are subjected to ingredient, ball milling according to 110:21:6 mass ratio
200 mesh screen residues 10% were arrived, 30Mpa forming under the pressure is diameter 7mm, length is the cylindric of 10mm;
Shaping raw material is placed in vacuum reduction furnace between two electrodes, is evacuated to 2000Pa, shaping raw material is heated to
After 1000 DEG C, sample applies voltage 600V (60V/mm), and at 0.4 ampere, the reaction that is powered cools down current control after five minutes.
The entire technique of the embodiment is time-consuming: heating 1.5 hours, energization 5min, 1 hour cooling.
The content of magnesia becomes 12% from 31.64% in measurement sample, magnesia reduction rate 85%.
Embodiment 3:
Forge white and ferrosilicon, fluorite that content of magnesia is 35wt% are subjected to ingredient, ball milling according to 105:18:4 mass ratio
200 mesh screen residues 3% were arrived, it is blocky in the rule that 15Mpa forming under the pressure is long 6mm, a height of 3mm, width are 5mm;
Shaping raw material is placed in vacuum reduction furnace between two electrodes, is evacuated to 4000Pa, shaping raw material is heated to
After 1100 DEG C, directly apply on shaping raw material voltage 600V (200V/mm), current control is at 0.4 ampere, and be powered 4 points of reaction
It is cooling after clock.
The entire technique of the embodiment is time-consuming: heating 1.5 hours, energization 4min, 1 hour cooling.
The content of magnesia becomes 10% magnesia reduction rate 79% from 32.01% in measurement sample.
Embodiment 4:
Forge white and ferrosilicon, fluorite that content of magnesia is 37wt% are subjected to ingredient, ball milling according to 107:20:4 mass ratio
200 mesh screen residues 4% were arrived, it is blocky in the rule that 15Mpa forming under the pressure is long 5mm, a height of 60mm, width are 5mm;
Shaping raw material is placed in vacuum reduction furnace between upper/lower electrode, 3000Pa is evacuated to, shaping raw material is heated to
After 900 DEG C, directly apply on shaping raw material voltage 600V (10V/mm), current control is at 0.4 ampere, and be powered reaction 3 minutes
After cool down.
The entire technique of the embodiment is time-consuming: heating 1.5 hours, energization 3min, 1 hour cooling.
The content of magnesia becomes 9% from 30.89% in measurement sample, magnesia reduction rate 95%.
Embodiment 5:
Forge white and ferrosilicon, fluorite and bauxite that content of magnesia is 36wt% are carried out according to 100:20:5:6 mass ratio
Ingredient, ball milling arrived 200 mesh screen residues 4%, were diameter 6mm in 25Mpa forming under the pressure, length is the cylindrical sample of 12mm;
Shaping raw material is placed in vacuum reduction furnace between upper/lower electrode, 100Pa is evacuated to, shaping raw material is heated to
After 700 DEG C, directly apply on shaping raw material voltage 600V (10V/mm), current control is at 0.4 ampere, and be powered reaction 3 minutes
After cool down.
The content of magnesia becomes 8% from 30.24% in measurement sample, magnesia reduction rate 74%, silicic acid three in magnesium slag
Calcium content 9%.
Embodiment 6:
The embodiment provides a kind of magnesium smelting device, the device and existing smelting silicothermic process magnesium apparatus the difference is that, wherein
Vacuum smelting furnace in be equipped with electrode.
It is specifically as shown in Figure 1 the vacuum smelting furnace of the embodiment, including reductive jar cavity 2, reductive jar cavity 2 are equipped with
Top cover 6;2 side wall of reductive jar cavity is equipped with and vacuumizes stomata 4;Reductive jar cavity 2 is interior equipped with electric heater unit 3 and opposing upper and lower
Top electrode 5 and lower electrode 1;Shaping raw material 7 is mounted between top electrode 5 and lower electrode 1 in smelting process.
Embodiment 7:
The magnesium smelting device of the embodiment is on the basis of embodiment 5, and side wall of the reductive jar cavity 2 close to bottom is equipped with
High-temperature gas air inlet 8;Top cover 6 is equipped with heat gas gas vent 9 (referring to Fig. 1).
High-temperature gas air inlet 8 therein is for preheating in the furnace before vacuumizing, and heat gas gas vent 9 is for vacuumizing
Preheating gas is discharged in preceding furnace, to save the power consumption in heating process.
Embodiment 8:
The magnesium smelting device difference from Example 1 of the embodiment is that the vacuum smelting furnace heating method of embodiment 5 is
Internal heat type, the embodiment are that heating method is external-heat.
It is specific as shown in Fig. 2, the embodiment vacuum smelting furnace, including external furnace body 10 and interior reductive jar cavity 11, it is interior also
Former chamber body 11 is arranged in external furnace body 10, is equipped with external heat source channel therebetween;Outer hot gas is offered on 10 side wall of external furnace body
Body entrance 16 and outer heat outlet 17, outer hot gas enter internal reductive jar cavity 11 in channel and are heated;11 He of external furnace body
Interior reductive jar cavity 11 is equipped with top cover 12;It offers to be equipped on top cover and vacuumizes stomata 13;It is equipped in interior reductive jar cavity 11
Auxiliary heating element 13 and top electrode opposing upper and lower 14 and lower electrode 15;Shaping raw material is mounted on top electrode 14 in smelting process
Between lower electrode 15.
Claims (7)
1. a kind of process for smelting magnesium, comprising: prepare pressure forming after raw material mixes for siliceous and magnesium mine, which is characterized in that 13-
Under the conditions of 4000Pa, after shaping raw material is heated to 600-1100 DEG C, directly applies voltage on shaping raw material, it is big to apply voltage
Small is 10-200V/mm, applies a length of 1-5min when voltage.
2. process for smelting magnesium as described in claim 1, which is characterized in that the ferrosilicon for preparing raw material by rational proportion, calcining
Dolomite and fluorite composition.
3. process for smelting magnesium as described in claim 1, which is characterized in that described to prepare in raw material added with bauxite or hydroxide
Aluminium.
4. process for smelting magnesium as claimed in claim 3, which is characterized in that described to prepare in raw material: silicon rate is 2.0-2.5;Aluminium rate
For 0.8-1.0;Lime saturation factor is 0.7-0.9.
5. process for smelting magnesium as described in claim 1, which is characterized in that the shaping raw material shape is regular cylinder or regular block
Shape.
6. a kind of magnesium smelting device, device includes vacuum smelting furnace, which is characterized in that a pair of of electricity is equipped in the vacuum smelting furnace
Pole, for directly applying voltage to the shaping raw material during refining magnesium, the vacuum condition control range in the vacuum smelting furnace
Are as follows: 13-4000Pa, temperature controlling range are as follows: 600-1100 DEG C.
7. magnesium smelting device as claimed in claim 4, which is characterized in that be equipped with multipair electrode in the vacuum smelting furnace.
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Application publication date: 20190920 |