CN105525108B - A kind of method that magnesium calcium alloy is produced in aluminothermic reduction - Google Patents
A kind of method that magnesium calcium alloy is produced in aluminothermic reduction Download PDFInfo
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- CN105525108B CN105525108B CN201510945660.1A CN201510945660A CN105525108B CN 105525108 B CN105525108 B CN 105525108B CN 201510945660 A CN201510945660 A CN 201510945660A CN 105525108 B CN105525108 B CN 105525108B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- 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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
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Abstract
A kind of method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：Step 1, by MgO powder, CaO powder and Al powder are well mixed；Step 2, mixed material is pressed into agglomerate；Step 3, after agglomerate is put into reductive jar and vacuumized, reductive jar is incubated 3~6h at 1150~1300 DEG C, reducing magnesia and calcium oxide turns into magnesium vapor and calcium steam；Step 4, after magnesium vapor and calcium steam are condensed, magnesium calcium alloy is generated in crystallizer.The method that magnesium calcium alloy is produced in the aluminothermic reduction of the present invention, using magnesia, calcium oxide as raw material, using aluminium powder as reducing agent, magnesium calcium alloy obtained by the step of vacuum-thermal reduction one, it is to avoid convert the burning problems for mixing method formation, production efficiency is high, cost is low, environment is good, and product purity is high, and the waste residue of generation can be completely used for production high-strength cement or for extracting aluminium hydroxide.
Description
Technical field
The invention belongs to field of metallurgy, the method that magnesium calcium alloy is produced in more particularly to a kind of aluminothermic reduction.
Background technology
Calcium is a kind of alloy element of magnesium alloy, can improve the structure refinement of magnesium alloy, creep resistance.Magnesium calcium alloy
Itself it can not only be used as heat-resisting alloy, and magnesium calcium alloy can largely be used as nodulizer, the steel-making of production spheroidal graphite cast-iron
Desulfurizing agent, deoxidier.Steel grade especially to some low silicon or without silicon, depth deoxidation and field trash of the magnesium calcium alloy to molten steel
Denaturation treatment effect it is more prominent.In addition, magnesium calcium density is small, modulus of elasticity is high, and corrosion resistance is strong, and has well with human body
Biocompatibility, therefore magnesium calcium alloy also gradually causes the attention of people as a kind of biomedical material.
The production method of magnesium metal is mainly including the fused salt electrolysis process using magnesium chloride as raw material and using magnesia as raw material
Vacuum-thermal method.Fused salt electrolysis process is that direct current is passed through in the fused electrolyte containing magnesium chloride, by magnesium chloride decomposition
The method of magnesium metal is made.According to the raw materials used difference of magnesium chloride is produced, a variety of electrolytic magnesium production technologies have been gradually formed.Very
Empty smelting magnesium by thermal reduction process is that magnesia is mixed to and suppressed agglomerating with reducing agent, and metal is prepared by thermal reduction in vacuum tank
The method of magnesium.According to the difference of reducing agent species, the production technology that a variety of vacuum reductions prepare magnesium metal has also been gradually formed.
The smelting process of calcium also mainly uses fused salt electrolysis process and vacuum-thermal method.Its technological principle and production technology
It is close with magnesium, wherein fused salt electrolysis process complex process, and the thermal reduction rate of recovery is relatively low.
The existing method for producing magnesium calcium alloy adds calcium metal or calcium hydride (hydrogen mainly to the method for mixing that is, into molten magnesium
Change calcium to decomposite calcium metal at high temperature and release hydrogen), the magnesium calcium alloy of certain ingredients is prepared in holding furnace.Due to magnesium,
The activity of calcium is higher, is easily oxidized, greater loss can be caused in mixed process.Therefore operating process need to take solvent or indifferent gas
Body is protected, and production process is complicated, and cost is higher.Therefore, the short-cut method for preparing magnesium calcium alloy is constantly among exploration.
CN103205573A discloses a kind of method that carbon thermal reduction prepares magnesium and calcium.This method is with dolomite calcination product
For raw material, using simple substance carbon as reducing agent, magnesium and calcium are prepared by thermal reduction reaction under vacuum, metal is then collected respectively
Magnesium and calcium metal.Although this method flow is short, residue is few, it should not collect and produce there is also secondary response more fierce, product
The problems such as product purity is relatively low.
The content of the invention
Present invention aims to overcome that problems of the prior art produce magnesium calcium alloy there is provided a kind of aluminothermic reduction
Method.The process of this method manufacture magnesium calcium alloy is easy, and magnesium calcium alloy safe preparation process is stable, and with low cost.
The method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：
Step 1, by MgO powder, CaO powder and Al powder are well mixed as raw material by the proportioning of magnesium calcium alloy；Wherein, MgO powder
Granularity be 61~147 μm, the granularity of CaO powder is 61~147 μm, and the granularity of Al powder is 74~175 μm；
Step 2, mixed material is pressed into agglomerate；
Step 3, after agglomerate is put into reductive jar and vacuumized, reductive jar is incubated 3~6h at 1150~1300 DEG C, makes oxygen
Changing magnesium and calcium oxide reduction turns into magnesium vapor and calcium steam；
Step 4, after magnesium vapor and calcium steam are condensed, magnesium calcium alloy is generated in crystallizer.
In above-mentioned steps 1, MgO powder and CaO powder are as raw material, and Al powder is used as reducing agent；
In above-mentioned steps 2, mixed material is pressed into agglomerate, the forming pressure of agglomerate is 40~100MPa, the thickness of agglomerate
Spend for 4~10mm；
In above-mentioned steps 3, the vacuum vacuumized is 1~10Pa.
In reductive jar, the reaction that dispensing occurs is as follows：
12CaO+21MgO+14Al=21Mg+12CaO7Al2O3
33CaO+14Al=21Ca+12CaO7Al2O3
According to the proportioning of reaction and required magnesium calcium alloy as described above, addition raw material MgO powder, CaO powder and Al can be calculated
The amount of powder.
In above-mentioned step 1, raw material MgO powder and CaO powder can use forging for being obtained after dolomite or magnesium dolomite calcination
White to substitute, it can be low grade magnesite or lime stone that MgO and the additive of CaO content are adjusted during dispensing.
The method that magnesium calcium alloy is produced in the aluminothermic reduction of the present invention, compared with prior art, beneficial effect is：
1st, the method that magnesium calcium alloy is produced in aluminothermic reduction of the present invention, using magnesia, calcium oxide as raw material, using aluminium powder as reduction
Agent, magnesium calcium alloy is obtained by the step of vacuum-thermal reduction one, it is to avoid convert the burning problems for mixing method formation, and production efficiency is high, cost
It is low.
2nd, the method that magnesium calcium alloy is produced in aluminothermic reduction of the present invention, good operational environment when technique produces magnesium calcium alloy, product
Purity is high, and the waste residue of generation can be completely used for production high-strength cement or for extracting aluminium hydroxide.
Brief description of the drawings
Fig. 1 is the process chart of the embodiment of the present invention；
Embodiment
Embodiment 1
The method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：
Step 1, granularity is 61 μm of MgO powder, the Al powder that granularity is 61 μm of CaO powder and granularity is 175 μm, in mass ratio
For MgO powder：CaO powder：Al powder=100：87：46 are well mixed；
Step 2, mixed material is pressed into thickness about 4mm agglomerate using forcing press under 100MPa pressure；
Step 3, agglomerate is put into reductive jar and is evacuated to after 1Pa, and reductive jar is incubated into 6h at 1150 DEG C, makes magnesia
Turn into magnesium vapor and calcium steam with calcium oxide reduction；
Step 4, after magnesium vapor and calcium steam are condensed, the magnesium that calcium content is 2.5~3.5wt.% is obtained in crystallizer
Calcium alloy.
The process chart that the method for magnesium calcium alloy is produced in the aluminothermic reduction of the present embodiment is shown in Fig. 1.
Embodiment 2
The method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：
Step 1, the MgO powder of 74 μm of granularity, 74 μm of CaO powder and 125 μm of Al powder are chosen, is in mass ratio MgO powder：
CaO powder：Al powder=100:96：48 are well mixed；
Step 2, mixed material is pressed into thickness about 6mm agglomerate using forcing press under 80MPa pressure；
Step 3, agglomerate is put into reductive jar and is evacuated to after 4Pa, and reductive jar is incubated into 5h at 1200 DEG C, makes magnesia
Turn into magnesium vapor and calcium steam with calcium oxide reduction；
Step 4, after magnesium vapor and calcium steam are condensed, calcium content is obtained in crystallizer and is closed for 5~7wt.% magnesium calcium
Gold.
The process chart that the method for magnesium calcium alloy is produced in the aluminothermic reduction of the present embodiment is shown in Fig. 1.
Embodiment 3
The method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：
Step 1, the MgO powder of 104 μm of granularity, 104 μm of CaO powder and 96 μm of Al powder are chosen, is in mass ratio MgO powder：
CaO powder：Al powder=100：103：50 are well mixed；
Step 2, mixed material is pressed into thickness about 8mm agglomerate using forcing press under 60MPa pressure；
Step 3, agglomerate is put into reductive jar and is evacuated to after 7Pa, and reductive jar is incubated into 4h at 1250 DEG C, makes magnesia
Turn into magnesium vapor and calcium steam with calcium oxide reduction；
Step 4, after magnesium vapor and calcium steam are condensed, the magnesium that calcium content is 7.5~10.5wt.% is obtained in crystallizer
Calcium alloy.
The process chart that the method for magnesium calcium alloy is produced in the aluminothermic reduction of the present embodiment is shown in Fig. 1.
Embodiment 4
The method that magnesium calcium alloy is produced in aluminothermic reduction, is comprised the steps of：
Step 1, the MgO powder of 147 μm of granularity, 147 μm of CaO powder and 74 μm of Al powder are chosen, is in mass ratio MgO powder：
CaO powder：Al powder=100:113：52 are well mixed；
Step 2, mixed material is pressed into thickness about 10mm agglomerate using forcing press under 40MPa pressure；
Step 3, agglomerate is put into reductive jar and is evacuated to after 10Pa, and reductive jar is incubated into 3h at 1300 DEG C, makes oxidation
Magnesium and calcium oxide reduction turn into magnesium vapor and calcium steam；
Step 4, after magnesium vapor and calcium steam are condensed, the magnesium calcium that calcium content is 10~14wt.% is obtained in crystallizer
Alloy.
The process chart that the method for magnesium calcium alloy is produced in the aluminothermic reduction of the present embodiment is shown in Fig. 1.
Claims (2)
1. a kind of method that magnesium calcium alloy is produced in aluminothermic reduction, it is characterised in that comprise the steps of：
Step 1, by MgO powder, CaO powder and Al powder are well mixed as raw material by the proportioning of magnesium calcium alloy；Wherein, the grain of MgO powder
Spend for 61~147 μm, the granularity of CaO powder is 61~147 μm, the granularity of Al powder is 74~175 μm；
Step 2, mixed material is pressed into agglomerate；The wherein forming pressure of agglomerate is 40~100MPa, the thickness of agglomerate for 4~
10mm；
Step 3, after agglomerate is put into reductive jar and vacuumized, reductive jar is incubated 3~6h at 1150~1300 DEG C, makes magnesia
Turn into magnesium vapor and calcium steam with calcium oxide reduction；The vacuum wherein vacuumized is 1~10Pa；In reductive jar, dispensing hair
Raw reaction is as follows：
12CaO+21MgO+14Al=21Mg+12CaO7Al2O3
With
33CaO+14Al=21Ca+12CaO7Al2O3；
According to the proportioning of reaction and required magnesium calcium alloy as described above, the amount of addition raw material MgO powder, CaO powder and Al powder is calculated；
Step 4, after magnesium vapor and calcium steam are condensed, magnesium calcium alloy is generated in crystallizer.
2. the method that magnesium calcium alloy is produced in aluminothermic reduction according to claim 1, it is characterised in that in described step 1,
Raw material MgO powder and CaO powder forge white replacement with what is obtained after dolomite or magnesium dolomite calcination, and MgO and CaO is adjusted during dispensing and is contained
The additive of amount is low grade magnesite or lime stone.
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| CN108707772A (en) * | 2018-05-29 | 2018-10-26 | 苏州佑君环境科技有限公司 | A kind of preparation method of chitin modified magnesium calcium alloy |
| CN109536751B (en) * | 2018-12-04 | 2020-06-30 | 辽宁科技学院 | Method for producing magnesium-lithium alloy and by-product magnesium aluminate spinel by aluminothermic reduction |
| CN113249549B (en) * | 2021-05-18 | 2023-01-31 | 鞍钢实业集团有限公司冶金资源再生利用分公司 | Aluminum-manganese-calcium-barium-magnesium-iron alloy for steelmaking and manufacturing method thereof |
| CN114737057B (en) * | 2022-03-24 | 2024-03-26 | 东北大学 | Method for preparing high vapor pressure metal by carbothermal reduction |
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| CN102080164A (en) * | 2010-12-02 | 2011-06-01 | 重庆大学 | Method for preparing Mg-Li alloy by vacuum synchronous thermal reduction |
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| DE10332033A1 (en) * | 2003-07-15 | 2005-02-03 | Chemetall Gmbh | Process for the preparation of metal powders or of metal hydride powders of the elements Ti, Zr, Hf, V, Nb, Ta and Cr |
| CN1618999A (en) * | 2004-12-10 | 2005-05-25 | 青海中信国安科技发展有限公司 | Method of producing metal magnesium by bischofite drying calicing to make magnesium oxide to vacuum thermo reduction |
| CN101289708B (en) * | 2008-05-13 | 2010-06-23 | 辛卫亚 | Semi-continuous metallothermic reduction process |
| CN101698907B (en) * | 2009-11-04 | 2011-12-21 | 中国科学院青海盐湖研究所 | Method for preparing metal magnesium by silicothermic process |
| CN103205573A (en) * | 2013-05-06 | 2013-07-17 | 重庆大学 | Method for preparing magnesium and calcium through carbon thermal reduction |
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