CN102041398B - 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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- CN102041398B CN102041398B CN2010105504001A CN201010550400A CN102041398B CN 102041398 B CN102041398 B CN 102041398B CN 2010105504001 A CN2010105504001 A CN 2010105504001A CN 201010550400 A CN201010550400 A CN 201010550400A CN 102041398 B CN102041398 B CN 102041398B
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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 under vacuum, to produce MAGNESIUM METAL 99 with ferro-silicon reduction calcined dolomite.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 99 as reductive agent, i.e. carbothermy; 2, in semicontinuous resistance furnace, mix with forging in vain with bauxite, form slag, make reductive agent with ferrosilicon, produce MAGNESIUM METAL 99, 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 through constantly feeding in raw material and realize continuous production in semicontinuous resistance furnace, improved production efficiency, but semi-continuous process adopts mostly still ferrosilicon to make reductive agent; Raw material follows Pidgeon process the same basically; 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
Above-mentioned deficiency to prior art exists the object of the present invention is to provide a kind of reduction raw materials cost, fast reaction speed and realizes 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 quicklime, 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 subsequent use through calcining;
(2) basic slag preparation-Ji slag adopts quicklime, aluminum oxide and three kinds of materials of silicon-dioxide to be made into, and the scope of basicity quicklime/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 drum 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 promptly gets MAGNESIUM METAL 99 through condensation and collection.
Said (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.
Said wagnerite and carbon granules granularity are greater than 60 orders.
Said 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, furnace shell and bell are interior to be vacuum; 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; Outside furnace shell, be provided with charging mechanism, the filling tube of charging mechanism passes furnace shell and fire brick layer gets into the charging crucible; Above charging crucible opening, be provided with the graphite thermally-insulated body, 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 mold over against through hole.
Further, in mold, be provided with dw, dw covers graphite thermally-insulated body central through hole, is provided with some ventilating pits in the dw registration collar.
Simultaneously; In bell, be provided with the cooling cowl of sandwich structure; Cooling cowl is corresponding with mold shape and cover on the mold, 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 through coolant pipe respectively with cooling liquid outlet and is connected with quench liquid.
Between charging crucible bottom and fire brick layer, be provided with the refractory brick cushion block.
Said charging mechanism comprises blowing jar and stock kettle, and blowing jar and stock kettle are communicated with through pipeline, on pipeline, are provided with variable valve, and filling tube is communicated with the blowing jar.
Being collected in the same reactor drum 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-mold; 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 quicklime, 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 subsequent use through calcining;
(2) basic slag preparation-Ji slag adopts quicklime, 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 the little wagnerite of granularity and reductive agent particle, such as mistake 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 carbon thermal 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 low vacuum, the easy magnesia 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 promptly gets MAGNESIUM METAL 99 through condensation and collection.
Said (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 through 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 through 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 distortion 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; For cavity forms the heating zone, be provided with the charging crucible 11 of splendid attire slag 12 in the heating zone in the middle of the fire brick layer 2, 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.Outside furnace shell 1, be provided with charging mechanism 10, the filling tube 13 of charging mechanism passes furnace shell 1 and gets into charging crucible 11 with fire brick layer 2.Above charging crucible 11 openings, be provided with it over against mold 7, mold 7 is placed on the fire brick layer 2.Mold 7 is up-small and down-big tubular structure.
Said charging mechanism 10 comprises blowing jar 14 and stock kettle 15, and blowing jar 14 is communicated with through pipeline with stock kettle 15, on pipeline, is provided with variable valve 16, 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, through pumped vacuum systems 9 vacuumize and begin the heating.After treating that slag 12 melts fully, add mixed in proportion raw material through charging mechanism 10.When the raw material reaction of charging in the crucible 11 gets when similar, can feed in raw material through 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 can be processed in through the pumped vacuum systems 9 that filtration unit is housed.
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 mold 7, therefore between charging crucible 11 and mold 7, places graphite thermally-insulated body 5; Graphite thermally-insulated body 5 is provided with central through hole 17, and mold 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 let reduction produce again smoothly passes through smoothly.
In order to prevent to vacuumize and to have the dirt slag to pollute mold 7 when reacting through the central through hole of graphite thermally-insulated body, in mold 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 through the central through hole of graphite thermally-insulated body 5, and magnesium steam is enriched on the mold 7 through the ventilating pit around the dw.
When capturing magnesium steam, the temperature of mold is very crucial, crosses the low too high yield and the quality that all can influence magnesium.This device is equipped with the temperature of thermopair monitoring mold, if temperature is too high, can regulate through 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 mold 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 through coolant pipe 19 respectively with cooling liquid outlet and is connected with quench liquid.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 passes through charging mechanism to charging crucible transferring raw material, and raw material is calcining wagnerite and carbon granules, and 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 through charging mechanism to charging crucible transferring raw material.The magnesium vapor enrichment that reduction produces for guaranteeing crystallization effect, guarantees that through oil cooling mould temperature is controlled near 500 ℃ on mold.Mold obtains reguline metal magnesium, and after the reaction, the MgO content in the slag is 5%, and magnesian reduction ratio reaches 85%.
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 quicklime, aluminum oxide and silicon-dioxide are slag former, and carbon is reductive agent; Its preparation process is:
(1) calcining-wagnerite obtains the calcining wagnerite with subsequent use through calcining;
(2) basic slag preparation-Ji slag adopts quicklime, aluminum oxide and three kinds of materials of silicon-dioxide to be made into, and the scope of basicity quicklime/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 drum 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 promptly gets MAGNESIUM METAL 99 through condensation and collection.
2. melting and reducing carbothermy system magnesium technology according to claim 1; It is characterized in that: the reinforced of said (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: said carbon is carbon granules, said 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: said 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, furnace shell and bell are interior to be vacuum; 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); Outside furnace shell (1), be provided with charging mechanism (10), the filling tube of charging mechanism (13) passes furnace shell and fire brick layer gets into 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); Be provided with mold (7) in graphite thermally-insulated body (5) top over against through hole.
6. system magnesium apparatus according to claim 5 is characterized in that: in mold (7), be provided with dw (6), dw (6) covers graphite thermally-insulated body central through hole (17), is provided with some ventilating pits in the dw registration collar.
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 mold (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 through coolant pipe respectively with cooling liquid outlet and is connected with quench liquid.
8. system magnesium apparatus according to claim 7 is characterized in that: between charging crucible (11) bottom and fire brick layer, be provided with refractory brick cushion block (3).
9. system magnesium apparatus according to claim 8; It is characterized in that: said charging mechanism (10) comprises blowing jar (14) and stock kettle (15); Blowing jar (14) and stock kettle (15) are communicated with through pipeline; On pipeline, be provided with variable valve (16), filling tube (13) is communicated with blowing jar (14).
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US5782952A (en) * | 1996-08-30 | 1998-07-21 | Massachusetts Institute Of Technology | Method for production of magnesium |
RU2149198C1 (en) * | 1999-11-09 | 2000-05-20 | Кожевников Георгий Николаевич | Method of magnesium production |
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