CN101560603A - Method for preparing magnesium metal and by-product by vacuum carbothermic reduction with serpentine minerals - Google Patents
Method for preparing magnesium metal and by-product by vacuum carbothermic reduction with serpentine minerals Download PDFInfo
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Abstract
The invention discloses a method for preparing a magnesium metal and a by-product by vacuum carbothermic reduction with serpentine minerals. The method comprises the following steps: using serpentine mineral powder as a raw material; adding a carbonaceous reducing agent which is 1 to 2 times of the theoretical quantity of carbon required for completely reducing magnesium silicate in the serpentine; adding a catalyst, and mixing the materials evenly to obtain a mixed raw material; pressing the mixed raw material into spherical or blocky ball agglomerations and drying the ball agglomerations; putting the dried ball agglomerations into a vacuum furnace, controlling the vacuum degree in the furnace to between 10 and 500 Pa, raising the temperature to between 500 and 700 DEG C, and keeping the temperature for 20 to 60 minutes to remove crystal water and clinker the materials; keeping the vacuum degree in the furnace, raising the temperature to between 1,200 and 1,500 DEG C, and reducing the magnesium silicate and oxides of metallic iron and nickel at a constant temperature for 30 to 60 minutes; and condensing magnesium vapor obtained from the reduction on a magnesium condenser into crystallized magnesium, recycling the metallic iron and the metallic nickel in the slag through magnetic separation, and preparing the slag after the magnetic separation into industrial silicon carbide through decarburization and purification.
Description
Technical field
The present invention relates to a kind of method for preparing MAGNESIUM METAL of reducing, particularly provide a kind of serpentine minerals of reduction with carbon in a vacuum to prepare MAGNESIUM METAL, and the method for by-product silicon carbide, metallic nickel, iron, the vacuum metallurgy technology field belonged to.
Background technology
Magnesium is one of the abundantest light metal of reserves on the earth.Magnesium is as a kind of lightweight metal material, and development and use can not show a candle to metal maturations such as iron and steel, copper, aluminium, and its potentiality are not fully excavated as yet.At present, the application of magnesium mainly concentrates on aluminium alloy production, die casting production, steel desulfurization three big fields, and also uses to some extent in rare earth alloy, metallic reducing and other fields.The light specific gravity of magnesium alloy, specific tenacity and specific rigidity height, heat-conductivity conducting are good, have good damping shock absorption and capability of electromagnetic shielding concurrently, have advantages such as easy machine-shaping, the easy recovery of waste material simultaneously, therefore along with the breakthrough of technology and Price Bottleneck, magnesium alloy has become the preferred material of industries such as modern national defense, aviation, automobile, electronics, communication, instrument, household electrical appliances, be described as " the green engineering material of 21 century " by people, wide application prospect is arranged.The fast development of world's magnesium alloy industry has driven the sharp increase that former magnesium is produced, and magnesium becomes the fifth-largest non-ferrous metal after aluminium, zinc, copper, lead.
The smelting process of present former magnesium mainly is divided into two kinds: the one, and hot reducing method; The 2nd, electrolytic process.Hot reducing method mainly adopts reductive agent heating reduction-oxidation magnesium, and according to the reductive agent difference, hot reducing method is divided into silicothermic process, carbide reduction process and carbothermic method again, wherein back two kinds in industrial less employing.Pidgeon process adopts ferrosilicon reduction-oxidation magnesium, belongs to a kind of of silicothermic process, is the thermal reduction magnesium refining method that generally adopts at present.Pidgeon process is reductive agent with the ferrosilicon, under certain vacuum degree and temperature, will be through the reduction of the rhombspar after the calcining, and magnesium obtains MAGNESIUM METAL through condensation after being reduced into steam again.The shortcoming of this kind technology is that the cost of reductive agent ferrosilicon is higher, and reduction jar costs an arm and a leg, and work-ing life is short, produces discontinuously, and labour intensity is big, the energy consumption height, and environmental pollution is serious etc., finally causes product cost higher.The fusion electrolysis method is to be raw material with the Magnesium Chloride Anhydrous, and metal alloy is a cathode and anode, feeds direct current and carry out electrolysis under the magnesium chloride molten state, and negative electrode obtains the MAGNESIUM METAL deposition, and anode is emitted chlorine.The shortcoming of its technology is a magnesium chloride hexahydrate dewatering process complexity, and the intractability of waste gas, waste water, waste residue is big, the expense height, and production unit and factory building seriously corroded, and also facility investment is big, and its equipment input is more than ten times of Pidgeon process.
It is the thermite process of raw material with magnesite and rhombspar that China's patent application 93115701.3 discloses a kind of, is reductive agent with the aluminium powder, calcined magnesite and rhombspar under 1100～1170 ℃ and vacuum condition, and the reduction through 6～8 hours prepares MAGNESIUM METAL.It is the method that reductive agent is produced MAGNESIUM METAL with the silumin that China patent ZL 200410020666.X discloses a kind of, this method is a raw material with rhombspar and magnesite, makes reductive agent with silumin, under high temperature and vacuum condition, reduction calcined dolomite and magnesite, the preparation MAGNESIUM METAL.China patent ZL200510011049.8 discloses a kind of smelting process of utilizing magnesium oxide pit coal carbon heat reducing extraction of metal magnesium, adopting magnesium oxide or its mineral white marble is raw material, with coal is reductive agent, with raw material and coal through fragmentation, after batch mixing and the granulation, in the internal heat type vacuum oven, under vacuum tightness 5～45Pa condition, control close-burning temperature is at 500～800 ℃, time 30～60min, finish the material close-burning, carried out reduction reaction 45-60 minute 1300～1600 ℃ of temperature again,, obtain purity and reach 90% or above crystal metal MAG block at last in 600～800 ℃ of condensations of temperature.China patent ZL 95100495.6 relates to a kind of electric furnace refining magnesium novel method and device thereof, it is characterized in that with rhombspar bauxitic clay, ferrosilicon is a raw material, will calcining back temperature at the rhombspar more than 700 ℃, bauxitic clay and the ferrosilicon electric furnace of packing into, silicon reduction system magnesium under vacuum condition.
Can find by above background technology, what no matter reductive agent adopted is ferrosilicon, aluminium, silumin, carbon or carbide, raw material all is to adopt magnesium oxide and mineral white marble and magnesite, and for the huge Magnesium Silicate q-agent mineral of the another kind of reserves of magnesium---serpentine is used for direct heat reduction method production MAGNESIUM METAL, the research of but not being correlated with, the domestic space state that is at present.Serpentine is that chemical constitution is Mg
6[Si
4O
10] (OH)
8The general name of gang's layer silicate mineral, theoretical Mg content wherein is about 18wt%.Based on this situation, we further investigate serpentine minerals hot reducing method production MAGNESIUM METAL, have invented the method that the serpentine minerals vacuum carbothermal reduction prepares MAGNESIUM METAL.
Summary of the invention
Main purpose of the present invention provides the method that a kind of serpentine minerals vacuum carbothermal reduction prepares MAGNESIUM METAL, by-product metallic iron nickel and silicon carbide.
To achieve these goals, the present invention is by the following technical solutions:
A kind ofly prepare the method for MAGNESIUM METAL and byproduct, finish according to the following steps with the serpentine minerals vacuum carbothermal reduction:
1) be raw material with the serpentine breeze, according to the Magnesium Silicate q-agent in the serpentine reduced fully required carbon theoretical amount 1～2 extraordinarily go into carbonaceous reducing agent, and add catalyzer, obtain mixing raw material after mixing;
2) described mixing raw material is pressed into spherical or blocky pelletizing feed with 5MPa～50Mpa pressure, pelletizing feed is carried out drying;
3) described pelletizing feed is packed in the vacuum oven, vacuum degree control rises to 500～700 ℃ with temperature in the stove, constant temperature 20～60min at 10～500Pa with the temperature rise rate of 5～15 ℃/min in the stove;
4) keep vacuum tightness 10～500Pa in the stove, temperature in the stove is risen to 1200～1500 ℃, constant temperature 30～60min, Magnesium Silicate q-agent in the reducting pellet material and ferric oxide and nickel oxide with the temperature rise rate of 5～15 ℃/min;
5) the magnesium steam that restores is condensed into crystallization magnesium on 200～600 ℃ magnesium condenser, the magnesium condenser is cooled to room temperature, collects crystallization magnesium;
6) metallic iron in the slag and metallic nickel reclaim by magnetic separation;
7) remove through magnetic separation and become industrial silicon carbide after slag behind de-iron and the nickel is purified through decarburization.
Described carbonaceous reducing agent is coke, coal, refinery coke, Graphite Powder 99 or charcoal.
Described catalyzer is Calcium Fluoride (Fluorspan), magnesium fluoride, Potassium monofluoride, Sodium Fluoride or barium fluoride.
Described catalyzer is that purity is the Calcium Fluoride (Fluorspan) of 90～99wt%, and addition accounts for 1～10wt% of mixing raw material amount.
The granularity of the pelletizing that described mixing raw material is pressed into is 10～30mm.
Beneficial effect of the present invention is:
1) filled up the blank that China utilizes also original production MAGNESIUM METAL of serpentine ore direct heat, its advantage is: the magnesium content of serpentine reaches 26.3% in theory, far above rhombspar 13.2%; And serpentine is the Magnesium Silicate q-agent mineral, need not calcine de-carbon.
2) the present invention finishes raw material decomposition, close-burning, carbothermic reduction process in the same vacuum oven under different condition; Main component Magnesium Silicate q-agent in the serpentine and other composition ferric oxide, nickel oxide all are reduced, and product magnesium vapor, silicon carbide are easy to reclaim, and byproduct iron nickel reclaims by magnetic separation.Serpentine ore obtains fully utilizing valuable elements such as wherein silicon, iron, nickel.Utilize fully MAGNESIUM METAL well-crystallized.
3) entire reaction course of the present invention is all carried out in a vacuum, has reduced the pollution to environment.
Description of drawings
Fig. 1 be the present invention reduce the preparation MAGNESIUM METAL process flow sheet.
Fig. 2 is the X-ray diffraction spectroscopic analysis collection of illustrative plates of the embodiment of the invention 1 experiment back gained slag composition.
Embodiment
Embodiment 1 usefulness serpentine ore vacuum carbothermal reduction prepares the method for MAGNESIUM METAL and byproduct
Serpentine is a kind of natural magnesium silicate minerals that contains, metamorphosed rock for peridotites, be by the 1:1 type layer silicate mineral of silicon-oxy tetrahedron wafer and the octahedra wafer be combined into of oxyhydrogen magnesium, be divided into lizardite, antigorite and chrysotile by its internal structured layer shape.Be MgO43.0% its theoretical composition, SiO
244.1%, H
2O12.9%, but component in the actual mineral and ratio can be different, often contain Fe, Ni, Mn, Al etc. and sneak into element.The purpose of test is that the method by carbon (coke, coking coal, refinery coke or Graphite Powder 99 etc.) thermal reduction is a MAGNESIUM METAL with the Magnesium Silicate q-agent mineral reduction in the serpentine, simultaneously with the SiO in the serpentine
3 2-Be reduced to gaseous state SiO, SiO generates SiC with CO or C reaction again, collects MAGNESIUM METAL by the magnesium condenser; SiC then stays in the slag, through the back manufacture level SiC that purifies; Iron-cobalt-nickel also is reduced simultaneously and stays in the slag, comprehensively reclaims after magnetic separation.Wherein, the effect of catalyzer is the crystalline structure that destroys serpentine, and Calcium Fluoride (Fluorspan), magnesium fluoride, Potassium monofluoride, Sodium Fluoride or barium fluoride can realize that all what adopt in the present embodiment is that purity is the Calcium Fluoride (Fluorspan) of 90wt%.
What this tested used serpentine employing is the two imperial mining industry serpentines that company limited produces in Alukeerqin Banner, the Inner Mongol.
This test of table 1 chemical ingredients/wt% of serpentine
| MgO | SiO 2 | FeO | NiO | Cr 2O 3 | Al 2O 3 | MnO |
| 36.36 | 40.55 | 4.62 | 0.26 | 0.12 | 0.41 | 0.12 |
A kind of method for preparing MAGNESIUM METAL and byproduct with the serpentine minerals vacuum carbothermal reduction as shown in Figure 1.
1) will be that the serpentine breeze of main component is as raw material with the Magnesium Silicate q-agent, add and go back the carbonaceous reducing agent of 1.5 times of the required carbon theoretical amount of magnesium orthosilicate, the carbonaceous reducing agent that this invention is selected can be coke, coal, refinery coke, Graphite Powder 99 or charcoal, adding the Calcium Fluoride (Fluorspan) that accounts for total material 5wt% mixes, select 30Mpa to be pressed into spherical or blocky pelletizing, granularity is about 20mm;
2) pelletizing is carried out drying;
3) material that drying is good is packed in the vacuum high temperature furnace, open vacuum system, behind vacuum tightness＜20Pa in the vacuum oven, begin to heat up, pelletizing feed is packed in the vacuum oven, temperature rise rate with about 10 ℃/min is warming up to 600 ℃, vacuum tightness raises with temperature at 10Pa when beginning to heat up, and pressure slowly raises, crystal water begins to decompose and removes in the time of 550 ℃, pressure obviously raises, and makes pressure be no more than 500Pa by adjust temperature rise rate within 5～15 ℃/min scope, after insulation for some time, pressure begins to reduce, constant temperature 30min makes the pelletizing material fully remove crystal water, and finishes close-burning; The interior vacuum degree control of stove is at 10～500Pa in the whole process;
4) continue to heat up, temperature rise rate is controlled at 5～15 ℃/min, pressure slowly raises thereupon, temperature reaches 1200 ℃, carbothermic reduction reaction begins, emitting gas increases sharply, this moment, pressure can reach 300～500Pa, by the adjustment heat-up rate pressure is controlled at and is no more than 500Pa, when temperature reaches 1500 ℃, constant temperature 40min, the serpentine pelletizing is magnesium steam and silicon carbide by carbon reduction, other composition ferric oxide in the serpentine, nickel oxide are reduced to metallic iron and metallic nickel, and magnesium steam is to be condensed into crystallization magnesium on 200～600 ℃ the magnesium condenser in temperature; The interior vacuum degree control of stove is at 10～500Pa in the whole process;
5) temperature that reduces the magnesium condenser is opened the magnesium condenser to room temperature, collects the metal MAG block that obtains the well-crystallized in condenser;
6) cooled slag is crushed to powdery, granularity is carried out magnetic separation less than＜0.5mm with magnetic separator, reclaims the ferronickel in the slag;
7) the slag main component after the magnetic separation is a silicon carbide, can get industrial silicon carbide behind the decarburization purifying.
This is tested resulting MAGNESIUM METAL test, shown in the examination table 2.The content of magnesium reaches 91.86% in the crystallization magnesium, can obtain the pure magnesium of technical grade by further processing.
This tests the chemical ingredients/wt% of resultant MAGNESIUM METAL table 2
| Mg | Si | C | Ca | O |
| 91.86 | 5.32 | 1.72 | 0.12 | 0.82 |
This is tested resulting slag test, assay is as follows:
Chemical ingredients/the wt% of this test slag of table 3
| Mg | Si | Fe | Ni | C | Al | Na |
| 0.54 | 33.49 | 6.36 | 0.55 | 12.20 | 0.60 | 0.25 |
Mg content has only 0.54% in the slag, shows that the reduction reaction of serpentine is very abundant, and serpentine carbothermic method production MAGNESIUM METAL is feasible.Si content in the slag has reached 33.49%, and C content has reached 12.20%.For the form of determining that main component exists, carry out the X-ray diffraction spectroscopic analysis to testing resulting slag, analytical results as shown in Figure 2, main thing is SiC mutually, graphite, Fe
3Si, Fe
5Si
3These four kinds of materials, wherein Fe
3Si and Fe
5Si
3Product for simple substance Fe and SiC reaction.It is recyclable metallic iron, nickel that slag is carried out magnetic separation, and the main component of slag is a silicon carbide after the magnetic separation, and it is relatively easy to recycle.Therefore the present invention can be used to by-product silicon carbide and metallic iron, nickel simultaneously.Table 4 is that slag is carried out the composition analysis that magnetic separation obtains product:
This test slag magnetic separation products therefrom of table 4 main component/wt%
| Fe | Si | Ni |
| 68.80 | 17.50 | 1.96 |
Embodiment 2 catalyzer Calcium Fluoride (Fluorspan) additions are to the influence of the magnesium rate of recovery
The effect of catalyzer Calcium Fluoride (Fluorspan) mainly is to destroy serpentine crystalline structure, and what of its add-on play important effect to the rate of recovery of magnesium in the serpentine ore.Adopt the preparation technology identical with embodiment 1, the ratio that accounts for mixing raw material by the Calcium Fluoride (Fluorspan) of adjusting interpolation is investigated its influence to the magnesium rate of recovery, and the result is as shown in table 5.As seen the Calcium Fluoride (Fluorspan) addition is 68.60% 1% o'clock rate of recovery, can be used for industrial production; At 1%～4% o'clock, the magnesium rate of recovery significantly increased along with the increase of Calcium Fluoride (Fluorspan) addition; And 4% when above, the magnesium rate of recovery has tended towards stability, about 95～96%.The Calcium Fluoride (Fluorspan) addition accounts for 1 of mixing raw material～10% and o'clock can realize that the present invention utilizes the purpose (it is serious to surpass 10% waste) of serpentine scale operation magnesium as can be seen.
Table 5 Calcium Fluoride (Fluorspan) addition is to the influence of the magnesium rate of recovery in the ore deposit
| Calcium Fluoride (Fluorspan) addition (%) | 1 | 3 | 4 | 7 | 10 |
| Raw material Mg content (%) | 12.22 | 12.10 | 12.30 | 12.56 | 12.68 |
| Burn back slag Mg content (%) | 6.38 | 2.32 | 0.65 | 0.63 | 0.64 |
| The magnesium rate of recovery (%) | 68.60 | 88.38 | 95.52 | 96.16 | 95.78 |
Claims (5)
1, a kind ofly prepares the method for MAGNESIUM METAL and byproduct, it is characterized in that: finish according to the following steps with the serpentine minerals vacuum carbothermal reduction;
1) be raw material with the serpentine breeze, according to the Magnesium Silicate q-agent in the serpentine reduced fully required carbon theoretical amount 1～2 extraordinarily go into carbonaceous reducing agent, and add catalyzer, obtain mixing raw material after mixing;
2) described mixing raw material is pressed into spherical or blocky pelletizing feed with 5MPa～50Mpa pressure, pelletizing feed is carried out drying;
3) described pelletizing feed is packed in the vacuum oven, vacuum degree control rises to 500～700 ℃ with temperature in the stove, constant temperature 20～60min at 10～500Pa with the temperature rise rate of 5～15 ℃/min in the stove;
4) keep vacuum tightness 10～500Pa in the stove, temperature in the stove is risen to 1200～1500 ℃, constant temperature 30～60min, Magnesium Silicate q-agent in the reducting pellet material and ferric oxide and nickel oxide with the temperature rise rate of 5～15 ℃/min;
5) the magnesium steam that restores is condensed into crystallization magnesium on 200～600 ℃ magnesium condenser, the magnesium condenser is cooled to room temperature, collects crystallization magnesium;
6) metallic iron in the slag and metallic nickel reclaim by magnetic separation;
7) remove through magnetic separation and become industrial silicon carbide after slag behind de-iron and the nickel is purified through decarburization.
2, claim 1 is described prepares the method for MAGNESIUM METAL and byproduct with the serpentine minerals vacuum carbothermal reduction, and it is characterized in that: described carbonaceous reducing agent is coke, coal, refinery coke, Graphite Powder 99 or charcoal.
3, claim 1 is described prepares the method for MAGNESIUM METAL and byproduct with the serpentine minerals vacuum carbothermal reduction, and it is characterized in that: described catalyzer is Calcium Fluoride (Fluorspan), magnesium fluoride, Potassium monofluoride, Sodium Fluoride or barium fluoride.
4, claim 1 is described prepares the method for MAGNESIUM METAL and byproduct with the serpentine minerals vacuum carbothermal reduction, and it is characterized in that: described catalyzer is that purity is the Calcium Fluoride (Fluorspan) of 90～99wt%, and addition accounts for 1～10wt% of mixing raw material amount.
5, claim 1 is described prepares the method for MAGNESIUM METAL and byproduct with the serpentine minerals vacuum carbothermal reduction, and it is characterized in that: the granularity of the pelletizing that described mixing raw material is pressed into is 10～30mm.
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| CN101899581A (en) * | 2010-06-18 | 2010-12-01 | 东北大学 | Method for preparing metal magnesium and boron-enriched material from ascharite serving as raw material by vacuum thermal reduction method |
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