CN102041398A - Process and device for preparing magnesium by utilizing smelting reduction carbothermy - Google Patents
Process and device for preparing magnesium by utilizing smelting reduction carbothermy Download PDFInfo
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- CN102041398A CN102041398A CN 201010550400 CN201010550400A CN102041398A CN 102041398 A CN102041398 A CN 102041398A CN 201010550400 CN201010550400 CN 201010550400 CN 201010550400 A CN201010550400 A CN 201010550400A CN 102041398 A CN102041398 A CN 102041398A
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Abstract
The invention discloses a process and device for preparing magnesium by utilizing smelting reduction carbothermy. The process comprises the following steps: proportioning calcium oxide, aluminum oxide and silicon dioxide into base slag; mixing calcined magnesite, reductant coal and carbon or graphite to prepare a raw material; putting the prepared base slag into a charging crucible, and then putting the charging crucible into a vacuum reactor; heating the base slag in the vacuum reactor so that the base slag is in a complete melting state; adding the prepared raw material to the melted base slag so that MgO in the raw material is completely dissolved in the base slag; carrying out the reduction reaction of the MgO under the condition that the temperature is 1550-1650 DEG C; and collecting the magnesium steam obtained from the reduction reaction to prepare metal magnesium. The invention reduces the cost of the raw material by taking the coal with low price as a reductant, increases the reaction speed because the reaction is carried out in the slag completely melted, realizes the continuous production of the magnesium because the raw material can be continuously added to a reaction furnace, effectively reduces the labor strength and enhances the utilization rate and production efficiency of equipment.
Description
Technical field
The present invention relates to a kind of process for smelting magnesium, specifically refer to a kind of melting and reducing carbothermy system magnesium technology.The present invention also relates to a cover system magnesium apparatus that utilizes this technological design simultaneously, belongs to metallurgical technology field.
Background technology
Pidgeon process is present most popular a kind of method for smelting magnesium by hot technology, and it is to produce MAGNESIUM METAL with ferro-silicon reduction calcined dolomite under vacuum.Problems such as contaminate environment, production efficiency are low because Pidgeon process exists, energy consumption height are developed the inexorable trend that new process for smelting magnesium becomes the magnesium industry development.At present, method for smelting magnesium by hot mainly contains two developing direction: 1, adopt cheap carbon to replace ferro-silicon to produce MAGNESIUM METAL as reductive agent, i.e. carbothermy; 2, in semicontinuous resistance furnace, with bauxite and the white mixing of forging, form slag, make reductive agent with ferrosilicon, produce MAGNESIUM METAL, promptly semicontinuous reduction method.These two kinds of methods all have certain progress than Pidgeon process, but still come with some shortcomings.Carbothermy adopts cheap carbon to replace ferro-silicon as reductive agent, greatly reduce raw materials cost, but carbothermy still is the reaction between the solid, so reduction rate is still not high, can't reach continuous production yet.Thereby semi-continuous process can form slag by constantly feeding in raw material and realize continuous production in semicontinuous resistance furnace, improved production efficiency, but semi-continuous process mostly still adopts ferrosilicon to make reductive agent, raw material follows Pidgeon process the same substantially, so raw materials cost is higher, and be that solid-liquid mixes in the reaction, the liquid phase proportion is less, speed of response is restricted by the liquid phase proportion, and increase rate is little.
Summary of the invention
At the prior art above shortcomings, the object of the present invention is to provide a kind of reduction raw materials cost, fast reaction speed and realize quantity-produced melting and reducing carbothermy system magnesium technology.
Another object of the present invention is based on above-mentioned melting and reducing carbothermy system magnesium technology and the cover system magnesium apparatus that designs.
Technical scheme of the present invention is achieved in that a kind of melting and reducing carbothermy system magnesium technology, and this technology is main raw material with the wagnerite, and calcium oxide, aluminum oxide and silicon-dioxide are slag former, and coal, carbon or graphite are reductive agent; Its preparation process is:
(1) calcining-wagnerite obtains the calcining wagnerite with standby by calcining;
(2) basic slag preparation-Ji slag adopts calcium oxide, aluminum oxide and three kinds of materials of silicon-dioxide to be made into, and the scope of basicity calcium oxide/silicon-dioxide is controlled between 1～1.8, and aluminum oxide accounts for 20%～40% of basic slag gross weight;
(3) the calcining wagnerite of preparation of raw material-will prepare and reductive agent mix, in the reductive agent in C and the calcining wagnerite MgO mol ratio be 1.1～1.4;
(4) the basic slag that vacuumizes-will prepare pack into the charging crucible in, again with basic slag together with the charging crucible put into vacuum reactor, the reactor vacuum control is between 10Pa～1000Pa;
(5) slag fusing-in vacuum reactor, make basic slag be in complete molten state to basic slag heating;
(6) reinforced-(3) step confected materials is joined in the fused base slag, the MgO in the raw material is dissolved in the basic slag fully, form CaO-MgO-Al
2O
3-SiO
2The quaternary slag, and make the MgO quality control at below 20% of quaternary slag;
(7) reduction reaction-in temperature is to make MgO that reduction reaction takes place under 1550 ℃～1650 ℃;
(8) magnesium vapor that obtains of collection-reduction reaction is collected by condensation and is promptly got MAGNESIUM METAL.
Described (6) step reinforced reinforced or reinforced at interval for continuing so that the reduction reaction in (7) step continues to carry out, and remains the MgO quality at below 20% of quaternary slag.
Described wagnerite and carbon granules granularity are greater than 60 orders.
Described basic slag of (4) step accounts for charging crucible volumetrical 1/3～1/2.
According to the system magnesium apparatus of above-mentioned melting and reducing carbothermy system magnesium technological design, it comprises the open furnace shell in upper end and with the bell of furnace shell upper end capping, is vacuum in furnace shell and the bell; In furnace shell bottom be provided with fire brick layer on every side, for cavity forms the heating zone, be provided with the charging crucible of splendid attire slag in the heating zone in the middle of the fire brick layer, be provided with heating unit all around and between the fire brick layer at the charging crucible; Be provided with charging mechanism outside furnace shell, the filling tube of charging mechanism passes furnace shell and fire brick layer enters the charging crucible; Be provided with the graphite thermally-insulated body above charging crucible opening, supported by fire brick layer around the graphite thermally-insulated body, graphite thermally-insulated body center is provided with through hole; Above the graphite thermally-insulated body, be provided with crystallizer over against through hole.
Further, be provided with dw in crystallizer, dw covers graphite thermally-insulated body central through hole, is provided with some ventilating pits on every side in the dw lower end.
Simultaneously, in bell, be provided with the cooling cowl of sandwich structure, cooling cowl is corresponding with mold shape and cover on the crystallizer, and cooling cowl is provided with cooling liquid inlet and the cooling liquid outlet that communicates with interlayer, and cooling liquid inlet is drawn bell by coolant pipe respectively with cooling liquid outlet and is connected with cooling fluid.
Between charging crucible bottom and fire brick layer, be provided with the refractory brick cushion block.
Described charging mechanism comprises blowing jar and stock kettle, and blowing jar and stock kettle are communicated with by pipeline, is provided with variable valve on pipeline, and filling tube is communicated with the blowing jar.
Being collected in the same reactor of the magnesian reduction of the present invention, magnesium steam carried out.The coal of this technology utilization cheapness has reduced raw materials cost as reductive agent; Be reflected in the slag that melts fully and carry out, accelerated speed of response; Raw material need not made ball, and can constantly add in the Reaktionsofen, has realized the continuous production of magnesium, has effectively reduced labour intensity, and has improved plant factor and production efficiency.
Description of drawings
Fig. 1-the present invention makes the magnesium apparatus structural representation.
Wherein, 1-furnace shell; The 2-fire brick layer; 3-refractory brick cushion block; The 4-heating unit; 5-graphite thermally-insulated body; The 6-dw; The 7-crystallizer; The 8-bell; The 9-pumped vacuum systems; The 10-charging mechanism; The 11-crucible of feeding; The 12-slag; The 13-filling tube; 14-blowing jar; The 15-stock kettle; The 16-variable valve; The 17-through hole; The 18-cooling cowl; The 19-coolant pipe.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is described further.
Melting and reducing carbothermy system magnesium technology of the present invention is main raw material with magnesite, and calcium oxide, aluminum oxide and silicon-dioxide are slag former, and coal, carbon or graphite are reductive agent; Its preparation process is:
(1) calcining-wagnerite obtains the calcining wagnerite with standby by calcining;
(2) basic slag preparation-Ji slag adopts calcium oxide, aluminum oxide and three kinds of materials of silicon-dioxide to be made into basicity CaO/SiO
2Scope be controlled between 1 ~ 1.8 Al
2O
3Account for the 20% ~ 40% more suitable of slag total amount;
(3) the calcining wagnerite of preparation of raw material-will prepare and reductive agent carbon granules (coal or graphite) mix, and in order to strengthen contact area, can adopt little wagnerite of granularity and reductive agent particle, such as crossing 60 mesh sieves.In order to improve reduction rate, need to add excessive reductive agent, the C/MgO mol ratio is 1.1 ~ 1.4 in the reductive agent; The C here is meant the simple substance carbon that can be used for reacting in carbon, coal or the graphite.
(4) the basic slag that vacuumizes-will prepare pack into the charging crucible in, basic slag preferably account for the charging crucible 1/3 ~ 1/2, again with basic slag together with the charging crucible put into vacuum reactor (Reaktionsofen), low more the carrying out that helps reduction reaction more of vacuum tightness.Solid-state carbothermic reduction is under 1200 ℃, vacuum will reach 10Pa and could react, under 1600 ℃, vacuum only needs 10000Pa just can take place, and when adopting molten state to reduce, reacts more solid-state more easy, therefore the following carbon reduction liquid oxidatively of 10000Pa magnesium all can carry out, when adopting rough vacuum, the easy magnesium oxide steam of oxygen of the remnants in the stove, so this technology vacuum control within 10Pa ~ 1000Pa;
(5) slag fusing-in vacuum reactor, make basic slag be in complete molten state to basic slag heating.Reaktionsofen adopts the silicon molybdenum as heating unit, and the heating top temperature can reach 1700 ℃, CaO-Al
2O
3-SiO
2The ternary slag system can be realized complete molten state at 1200 ℃ ~ 1400 ℃;
(6) reinforced-(3) step confected materials is joined in the fused base slag, the MgO in the raw material is dissolved in the basic slag fully, form CaO-MgO-Al
2O
3-SiO
2The quaternary slag.For guaranteeing that slag is complete molten state under temperature of reaction, the MgO quality control is at below 20% of quaternary slag;
(7) reduction reaction-in temperature is to make MgO that reduction reaction takes place under 1550 ℃～1650 ℃;
(8) magnesium vapor that obtains of collection-reduction reaction is collected by condensation and is promptly got MAGNESIUM METAL.
Described (6) step reinforced reinforced or reinforced at interval for continuing so that the reduction reaction in (7) step continues to carry out, and remains the MgO quality at below 20% of quaternary slag.Because the triad slag can not consume in reaction process, only need calcining wagnerite and reductive agent by reinforced in good time postreaction consumption, reduction reaction can not interrupted, get final product but can not make the MgO quality surpass 20% of quaternary slag.
According to the system magnesium apparatus of above-mentioned melting and reducing carbothermy system magnesium technological design, this device essence is a vacuum reaction stove, and it comprises the open furnace shell 1 in upper end and with the bell 2 of furnace shell upper end capping, in furnace shell 1 and the bell 2 by pumped vacuum systems 9 vacuum pumpings.Furnace shell 1 is that the stainless steel plate with 10mm is welded, and thick steel plate can well prevent to be out of shape under vacuum state.In furnace shell 1 bottom with build on every side hollow foam ball fire brick layer 2 is arranged, can play function of heat insulation effectively, form the heating zone for cavity in the middle of the fire brick layer 2, be provided with the charging crucible 11 of splendid attire slag 12 in the heating zone, be provided with heating unit 4 all around and between the fire brick layer 2 at charging crucible 11, heating unit 4 adopts the Si-Mo rod heating, and the Heating temperature upper limit is up to 1700 ℃.Between charging crucible 11 bottoms and fire brick layer 2, be provided with the refractory brick cushion block 3 that the balance crucible is used.Be provided with charging mechanism 10 outside furnace shell 1, the filling tube 13 of charging mechanism passes furnace shell 1 and fire brick layer 2 enters charging crucible 11.Above charging crucible 11 openings, be provided with it over against crystallizer 7, crystallizer 7 is placed on the fire brick layer 2.Crystallizer 7 is up-small and down-big tubular structure.
Described charging mechanism 10 comprises blowing jar 14 and stock kettle 15, and blowing jar 14 and stock kettle 15 are communicated with by pipeline, are provided with variable valve 16 on pipeline, can stop effectively in the air admission Reaktionsofen.Filling tube 13 is communicated with blowing jar 14, also is provided with variable valve 16 on the filling tube 13.
Before carrying out reduction reaction,, be placed on the refractory brick cushion block 3 of heating zone the charging crucible 11 that slag 12 is housed.After covering bell 8, by pumped vacuum systems 9 vacuumize and begin the heating.After treating that slag 12 melts fully, add mixed in proportion raw material by charging mechanism 10.When the raw material reaction of charging in the crucible 11 gets when similar, can feed in raw material by charging mechanism 10 this moment again, so just arrived the quantity-produced purpose.Owing to adopt carbothermic reduction, can form CO and CO in the reduction reaction process
2, these gases are can be in by the pumped vacuum systems 9 that filtration unit is housed processed to be fallen.
Because reduction reaction is carried out in high-temperature slag, the heat of heating zone is very high, can be delivered to fast on the crystallizer 7, therefore places graphite thermally-insulated body 5 between charging crucible 11 and crystallizer 7, graphite thermally-insulated body 5 is provided with central through hole 17, and crystallizer 7 is over against the through hole 17 of graphite thermally-insulated body.Graphite thermally-insulated body 5 has a center by several piece and is made up of the graphite cake of through hole, is supported by fire brick layer on every side.Graphite thermally-insulated body 5 can effectively prevent the upwards transmission of temperature of heating zone, and the magnesium steam that central through hole can allow reduction produce again smoothly passes through smoothly.
In order to prevent to vacuumize and to have the dirt slag to pollute crystallizer 7 when reacting by the central through hole of graphite thermally-insulated body, in crystallizer 7, be provided with dw 6, dw 6 covers graphite thermally-insulated body central through hole 17.Dw 6 is the cylinder-like structure of back-off, and the top closure of dw 6 is provided with some ventilating pits around dw.The top of sealing can be good at preventing thermal radiation and the dust by the central through hole of graphite thermally-insulated body 5, and magnesium steam is enriched on the crystallizer 7 by the ventilating pit around the dw.
When capturing magnesium steam, the temperature of crystallizer is very crucial, crosses the low too high recovery rate and the quality that all can influence magnesium.This device is equipped with the temperature of thermopair monitoring crystallizer, if temperature is too high, can regulate by cooling body.Be specially, in bell 8, be provided with the cooling cowl 18 of sandwich structure, cooling cowl 18 is corresponding with mold shape and cover on the crystallizer 7, cooling cowl is provided with cooling liquid inlet and the cooling liquid outlet that communicates with interlayer, and cooling liquid inlet is drawn bell 8 by coolant pipe 19 respectively with cooling liquid outlet and is connected with cooling fluid.This cooling body can effectively play the effect of regulating mould temperature.
Embodiment 1
The charging crucible that basic slag is housed is put into the Reaktionsofen heating zone, and basic slag add-on highly is 1/2 of a crucible height for its fusing back, and basic slag ingredient is CaO:SiO
2: Al
2O
3=45%:30%:25%, basicity is 1.5.Then place graphite cake and dw, cover bell then, vacuumize and heat.It is 1000Pa that vacuum is evacuated to the stove internal gas pressure, and temperature of reaction is controlled at about 1550 ℃.Treat temperature-stable after for some time, basic slag melts fully, at this moment by charging mechanism to charging crucible transferring raw material, raw material is calcining wagnerite and carbon granules, wherein the C/MgO mol ratio is 1.1.The slag composition that the calcining wagnerite adds back formation is CaO:MgO:SiO
2: Al
2O
3=37%:18%:25%:20%.MgO under the high temperature in the carbon granules reduction liquid slag, along with the carrying out of reaction, during the continuous approach exhaustion of raw material, once more by charging mechanism to charging crucible transferring raw material.The magnesium vapor enrichment that reduction produces for guaranteeing crystallization effect, guarantees that by oil cooling mould temperature is controlled near 500 ℃ on crystallizer.Crystallizer obtains reguline metal magnesium, and after the reaction, the MgO content in the slag is 5%, and magnesian reduction ratio reaches 85%.
Embodiment 2
The used basic quantity of slag highly is 1/3 of charging crucible height for its fusing back, and basic slag ingredient is CaO:SiO
2: Al
2O
3=40%:30%:30%, basicity is 1.3.Vacuum is 10Pa, and temperature of reaction is controlled at about 1650 ℃.Raw material is calcining wagnerite and Graphite Powder 99, and wherein the C/MgO mol ratio is 1.4, and the slag composition that forms after the calcining wagnerite adds is CaO:MgO:SiO
2: Al
2O
3=35%:13%:26%:26%.Reinforced three times of whole process obtains reguline metal magnesium at last, and MgO content is 2.6% in the slag, and magnesian reduction ratio reaches 94%.
Claims (9)
1. melting and reducing carbothermy system magnesium technology, it is characterized in that: this technology is main raw material with the wagnerite, and calcium oxide, aluminum oxide and silicon-dioxide are slag former, and coal, carbon or graphite are reductive agent; Its preparation process is:
(1) calcining-wagnerite obtains the calcining wagnerite with standby by calcining;
(2) basic slag preparation-Ji slag adopts calcium oxide, aluminum oxide and three kinds of materials of silicon-dioxide to be made into, and the scope of basicity calcium oxide/silicon-dioxide is controlled between 1～1.8, and aluminum oxide accounts for 20%～40% of basic slag gross weight;
(3) the calcining wagnerite of preparation of raw material-will prepare and reductive agent mix, in the reductive agent in C and the calcining wagnerite MgO mol ratio be 1.1～1.4;
(4) the basic slag that vacuumizes-will prepare pack into the charging crucible in, again with basic slag together with the charging crucible put into vacuum reactor, the reactor vacuum control is between 10Pa～1000Pa;
(5) slag fusing-in vacuum reactor, make basic slag be in complete molten state to basic slag heating;
(6) reinforced-(3) step confected materials is joined in the fused base slag, the MgO in the raw material is dissolved in the basic slag fully, form CaO-MgO-Al
2O
3-SiO
2The quaternary slag, and make the MgO quality control at below 20% of quaternary slag;
(7) reduction reaction-in temperature is to make MgO that reduction reaction takes place under 1550 ℃～1650 ℃;
(8) magnesium vapor that obtains of collection-reduction reaction is collected by condensation and is promptly got MAGNESIUM METAL.
2. melting and reducing carbothermy system magnesium technology according to claim 1, it is characterized in that: the reinforced of described (6) step is lasting reinforced or reinforced at interval, so that the reduction reaction in (7) step continues to carry out, and remain the MgO quality at below 20% of quaternary slag.
3. melting and reducing carbothermy system magnesium technology according to claim 1 and 2, it is characterized in that: described wagnerite and carbon granules granularity are greater than 60 orders.
4. melting and reducing carbothermy system magnesium technology according to claim 3 is characterized in that: described basic slag of (4) step accounts for charging crucible volumetrical 1/3～1/2.
5. the system magnesium apparatus of melting and reducing carbothermy system magnesium according to claim 1 technological design is characterized in that: it comprises upper end open furnace shell (1) and with the bell (8) of furnace shell upper end capping, is vacuum in furnace shell and the bell; In furnace shell (1) bottom be provided with fire brick layer (2) on every side, form the heating zone for cavity in the middle of the fire brick layer, be provided with the charging crucible (11) of splendid attire slag in the heating zone, and be provided with heating unit (4) between the fire brick layer (2) all around at charging crucible (11); Be provided with charging mechanism (10) outside furnace shell (1), the filling tube of charging mechanism (13) passes furnace shell and fire brick layer enters charging crucible (11); Be provided with graphite thermally-insulated body (5) in charging crucible (11) opening top, supported by fire brick layer around the graphite thermally-insulated body, graphite thermally-insulated body (5) center is provided with through hole (17); Above graphite thermally-insulated body (5), be provided with crystallizer (7) over against through hole.
6. system magnesium apparatus according to claim 5 is characterized in that: be provided with dw (6) in crystallizer (7), dw (6) covers graphite thermally-insulated body central through hole (17), is provided with some ventilating pits on every side in the dw lower end.
7. according to claim 5 or 6 described system magnesium apparatus, it is characterized in that: the cooling cowl (18) that in bell (8), is provided with sandwich structure, cooling cowl (18) is corresponding with mold shape and cover on the crystallizer (7), cooling cowl is provided with cooling liquid inlet and the cooling liquid outlet that communicates with interlayer, and cooling liquid inlet is drawn bell by coolant pipe respectively with cooling liquid outlet and is connected with cooling fluid.
8. system magnesium apparatus according to claim 7 is characterized in that: be provided with refractory brick cushion block (3) between charging crucible (11) bottom and fire brick layer.
9. system magnesium apparatus according to claim 8, it is characterized in that: described charging mechanism (10) comprises blowing jar (14) and stock kettle (15), blowing jar (14) and stock kettle (15) are communicated with by pipeline, be provided with variable valve (16) on pipeline, filling tube (13) is communicated with blowing jar (14).
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| CN103205583A (en) * | 2013-05-06 | 2013-07-17 | 重庆大学 | Method for preparing magnesium through carbon thermal reduction |
| CN103233133A (en) * | 2013-05-06 | 2013-08-07 | 重庆大学 | Device and method for preparing magnesium by carbothermic reduction |
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| CN103205583A (en) * | 2013-05-06 | 2013-07-17 | 重庆大学 | Method for preparing magnesium through carbon thermal reduction |
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