CN102864315B - Vacuum magnesium making method using magnesium-silicon alloy as reducing agent - Google Patents
Vacuum magnesium making method using magnesium-silicon alloy as reducing agent Download PDFInfo
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- CN102864315B CN102864315B CN201210336399.1A CN201210336399A CN102864315B CN 102864315 B CN102864315 B CN 102864315B CN 201210336399 A CN201210336399 A CN 201210336399A CN 102864315 B CN102864315 B CN 102864315B
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Abstract
The invention belongs to the field of metallurgy, and particularly relates to a vacuum magnesium making method using magnesium-silicon alloy as a reducing agent. The method comprises the following steps of: calcining and finely grinding a mixture of dolomite or magnesite and limestone as a raw material; proportioning and mixing the calcined and finely ground powdery raw material and the silicon-magnesium alloy powder reducing agent; pressing in a blocky material or a pellet material under the pressure of 40-300 MPa; filling the blocky material or the pellet material in vacuum reactor; reducing at the temperature of 1,000-1,300 DEG C and under the vacuum condition with vacuum degree of less than 80 Pa; forming steam by magnesium produced by reduction of magnesium oxide in the reducing material by the magnesium silicon reducing agent; and crystallizing on a crystallizer on the upper part of the vacuum reactor to form metal magnesium. Compared with the conventional pidgeon process, the vacuum metallothermic reduction magnesium making method using the magnesium-silicon alloy as the reducing agent has the advantages of greatly reducing the energy consumption of magnesium production, greatly reducing the material-magnesium ratio and greatly improving the production efficiency.
Description
Technical field
The invention belongs to field of metallurgy, particularly a kind ofly take the vacuum magnesium refining method that mg-si master alloy is reductive agent.
Background technology
The method of current industrial production MAGNESIUM METAL mainly contains two kinds: a kind of is to take the fused salt electrolysis process that muriate is raw material, and another kind is to take the vacuum metal hot reducing method that ferro-silicon is reductive agent.Metallothermics is because technique is simple, invests littlely, and the low and non-corrosiveness γ-ray emission of cost, is little by little replacing fused salt electrolysis process.
In recent years, scholars have carried out in depth research to vacuum metal hot reducing method, " a kind of take the vacuum-thermal method refining magnesium technology that wagnerite and rhombspar mixed mineral be raw material " (Feng Naixiang wherein, Wang Yaowu, < < China YouSe Acta Metallurgica Sinica > > 10 phases in 2011), and the application number Chinese patent that is 201210059438 " a kind of take the vacuum magnesium refining method that silicon calcium powder is reductive agent " in succession discloses and take respectively the vacuum magnesium refining method that aluminium powder and silicocalcium be reductive agent, the core content of these methods is in order to reduce the material magnesium ratio of vacuum-thermal method and to adopt new reductive agent to improve to greatest extent single furnace output of MAGNESIUM METAL, reduce energy consumption and production costs.This wherein, " a kind of take the vacuum magnesium refining method that silicon calcium powder is reductive agent " disclosed technical scheme reaches 3.4 at Theoretical Calculation material loading magnesium ratio, and reductive agent price is relatively cheap, although this method is compared the material magnesium ratio that can reach lower with silicothermic process, but produce one ton of MAGNESIUM METAL, in the situation that magnesium reduction rate reaches 100%, need the raw material of 3.4 tons.And during actual production, the reduction ratio of magnesium may be in 80% left and right, the excess coefficient of reductive agent at least will be more than 5%, although the material magnesium specific energy of its best reaches 3.4:1, the material magnesium ratio of its reality may surpass 4.0:1.
Summary of the invention
For the problems referred to above, the invention provides a kind of vacuum magnesium refining method that mg-si master alloy is reductive agent of take, be with rhombspar or take the vacuum-thermal method production MAGNESIUM METAL that the mixture of wagnerite and Wingdale formed CaOMgO or CaO and MgO mixture after calcining be raw material, object is to reduce to greatest extent the material magnesium ratio of vacuum-thermal reduction refining magnesium, thereby reach and improve to greatest extent economic benefit and the production efficiency that magnesium is smelted production, in addition, the smelting enterprise that the method is specially adapted to take the employing metallothermics production MAGNESIUM METAL that dolomite mineral is raw material is used.
The vacuum magnesium refining method that the mg-si master alloy of take is reductive agent, carries out according to following steps:
(1) raw material calcining: with rhombspar, or the mixture of wagnerite and Wingdale is raw material, dolomite calcination is arrived to 1000-1300 ℃, be finely ground into the powder of granularity < 1.0mm, or respectively wagnerite is calcined to 800-1000 ℃, limestone calcination to 1000-1300 ℃, is mixed after being then finely ground into the powder of granularity < 1.0mm, control CaCO in rhombspar
3and MgCO
3mol ratio is 1:1, and in the mixture of wagnerite and Wingdale, the mol ratio of MgO and CaO equals 1:1;
(2) batching: the Si-Mg alloy powder reductive agent of calcining and levigate rear powder stock and granularity < 1.0mm is prepared burden by chemical equation (1), and the amount of allocating into of reductive agent by the 1.01-1.20 of the theoretical dosage of chemical equation (1) doubly;
2(1-x)CaO + 2(1-x)MgO + Mg
xSi
(1-x) = (2-x)Mg + (1-x)[2CaO·SiO
2] (1)；
In formula: x is the weight percent of Mg in described Si-Mg alloy, and 0 < x < 3/4;
(3) briquetting: after above-mentioned batching is mixed, be pressed into agglomerate material or pelletizing feed under the pressure of 40-300MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, under the vacuum condition of the temperature of 1000-1300 ℃ and vacuum tightness < 80Pa, reduce, the magnesium that magnesium oxide in reducing material is generated by magnesium Si reduction agent reduction forms steam, on the crystallizer on vacuum reactor top, crystallize into MAGNESIUM METAL, remaining slag charge after reduction reaction, its main component is 2CaOSiO
2, as shown in vacuum reducing reaction equation (1).
Wherein, in step (1), control CaCO in rhombspar
3and MgCO
3mol ratio is that the method for 1:1 is: the CaCO in rhombspar raw material
3and MgCO
3mol ratio is less than at 1 o'clock, adds ore or compound that the rear composition of Wingdale or calcining is CaO, CaCO in rhombspar raw material
3and MgCO
3mol ratio is greater than at 1 o'clock, adds ore or compound that the rear chemical composition of wagnerite, brucite or calcining is MgO.
Control method that the mol ratio of MgO and CaO in the mixture of wagnerite and Wingdale equals 1:1 and be the mixed weight ratio that regulates wagnerite and Wingdale.
Compared with prior art, feature of the present invention and beneficial effect are:
The inventive method is with Mg
xsi
(1-x)alloy is reductive agent, and raw material is carried out to vacuum-thermal reduction, and the reaction equation of generation is: 2 (1-x) CaO+2 (1-x) MgO+Mg
xsi
(1-x)=(the 2-x) [2CaOSiO of Mg+(1-x)
2], by reduction reaction equation (1), can be found out:
(1) when x=2/3, reductive agent Mg
xsi
(1-x)can be write as Mg
2si, this Mg
2si is Mg and the formed comparatively stable metallic compound of Si in Mg-Si binary alloy phase diagram, and the reaction that MAGNESIUM METAL is produced in mg-si master alloy vacuum-thermal reduction now can be written as:
2CaO + 2MgO + Mg
2Si= 4Mg + 2CaO·SiO
2 (2)；
(2) when x=1/2, reductive agent Mg
xsi
(1-x)can be write as MgSi, the reaction that MAGNESIUM METAL is produced in mg-si master alloy vacuum-thermal reduction now can be written as:
2CaO + 2MgO + MgSi= 3Mg + 2CaO·SiO
2 (3)；
By vacuum reducing reaction formula (1) (2) (3), can be found out, work as Mg
xsi
(1-x)in alloy during 0 < x < 3/4,
Above-mentioned method of take the vacuum metal thermal reduction refining magnesium that mg-si master alloy is reductive agent of the present invention is compared with traditional Pidgeon process, can make the energy consumption of producing magnesium greatly reduce, and material magnesium is than also greatly reducing, and production efficiency is greatly improved.
Embodiment
To by following examples, describe new magnesium refining method of the present invention below, the present invention does not limit to and these embodiment, and the present invention, also can be according to Mg except following embodiment
xsi
(1-x)the chemical composition of alloy is adjusted and is implemented.
The Mg adopting in the embodiment of the present invention
xsi
(1-x)alloy all need before use levigate to its granularity be below 1.0mm, the rhombspar after calcining or Wingdale, wagnerite, brucite etc. all need levigate to its granularity be below 1.0mm.
Embodiment 1
(1) raw material calcining: with CaCO
3and MgCO
3mol ratio is that the rhombspar of 1:1 is raw material, by dolomite calcination to 1100 ℃, is finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and reductive agent Mg
2the ratio of components of Si excessive 10% is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into agglomerate material under the pressure of 40MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1000 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Embodiment 2
(1) raw material calcining: with CaCO
3and MgCO
3mol ratio is that the rhombspar of 1:1 is raw material, by dolomite calcination to 1000 ℃, is finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and the ratio of components of reductive agent MgSi excessive 1% is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into pelletizing feed under the pressure of 140MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1000 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Embodiment 3
(1) raw material calcining: with CaCO
3and MgCO
3mol ratio is that the rhombspar of 1:1 is raw material, by dolomite calcination to 1300 ℃, is finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and reductive agent Mg
3si
2excessive 20% ratio of components is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into agglomerate material under the pressure of 300MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1200 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Embodiment 4
(1) raw material calcining: the mol ratio of MgO and CaO of take equals the wagnerite of 1:1 and the mixture of Wingdale is raw material, wagnerite is calcined to 800 ℃ respectively, by limestone calcination to 1000 ℃, mix after being then finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and reductive agent Mg
3si
2excessive 20% ratio of components is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into pelletizing feed under the pressure of 100MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1000 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Embodiment 5
(1) raw material calcining: the mol ratio of MgO and CaO of take equals the wagnerite of 1:1 and the mixture of Wingdale is raw material, wagnerite is calcined to 1000 ℃ respectively, by limestone calcination to 1200 ℃, mix after being then finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and reductive agent Mg
3si
2excessive 20% ratio of components is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into agglomerate material under the pressure of 40MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1000 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Embodiment 6
(1) raw material calcining: the mol ratio of MgO and CaO of take equals the wagnerite of 1:1 and the mixture of Wingdale is raw material, wagnerite is calcined to 900 ℃ respectively, by limestone calcination to 1300 ℃, mix after being then finely ground into the powder of granularity < 1.0mm;
(2) batching: by calcining and levigate after the Si-Mg alloy powder reductive agent of powder stock and granularity < 1.0mm press chemical equation (2), and reductive agent Mg
3si
2excessive 10% ratio of components is prepared burden;
(3) briquetting: after above-mentioned batching is mixed, be pressed into pelletizing feed under the pressure of 50MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, reduce under the vacuum condition of the temperature of 1300 ℃ and vacuum tightness < 80Pa, the MAGNESIUM METAL that reaction generates enters magnesium crystallizer with gaseous form.Here the MAGNESIUM METAL of gaseous state generates solid-state Crystalline Magnesium on the crystallizer wall of crystallizer.After vacuum reducing reaction, generating its main component of residue is 2CaOSiO
2, stay in reactor.
Claims (1)
1. the vacuum magnesium refining method that the mg-si master alloy powder of take is reductive agent, carries out according to following steps:
(1) raw material calcining: with rhombspar, or the mixture of wagnerite and Wingdale is raw material, dolomite calcination is arrived to 1000-1300 ℃, be finely ground into the powder of granularity < 1.0mm, or respectively wagnerite is calcined to 800-1000 ℃, limestone calcination to 1000-1300 ℃, is mixed after being then finely ground into the powder of granularity < 1.0mm;
It is characterized in that controlling CaCO in rhombspar
3and MgCO
3mol ratio is 1:1, and in the mixture of wagnerite and Wingdale, the mol ratio of MgO and CaO equals 1:1; Control CaCO in raw material rhombspar
3and MgCO
3mol ratio is that the method for 1:1 is: the CaCO in rhombspar raw material
3and MgCO
3mol ratio is less than at 1 o'clock, adds ore or compound that Wingdale or the rear composition of other calcining are CaO, CaCO in rhombspar raw material
3and MgCO
3mol ratio is greater than at 1 o'clock, adds ore or compound that the rear chemical composition of wagnerite, brucite or calcining is MgO; Control method that the mol ratio of MgO and CaO in the mixture of wagnerite and Wingdale equals 1:1 and be the mixed weight ratio that regulates wagnerite and Wingdale;
(2) batching: the Si-Mg alloy powder reductive agent of calcining and levigate rear powder stock and granularity < 1.0mm is prepared burden by chemical equation (1), and the amount of allocating into of reductive agent by the 1.01-1.20 of the theoretical dosage of chemical equation (1) doubly;
2(1-x)CaO+2(1-x)MgO+Mg
xSi
(1-x)＝(2-x)Mg+(1-x)[2CaO·SiO
2] (1)；
In formula: x is the weight percent of Mg in described Si-Mg alloy, and 0 < x < 3/4;
(3) briquetting: after above-mentioned batching is mixed, be pressed into agglomerate material or pelletizing feed under the pressure of 40-300MPa;
(4) reduction: agglomerate material or pelletizing feed are placed in to vacuum reactor, under the vacuum condition of the temperature of 1000-1300 ℃ and vacuum tightness < 80Pa, reduce, the magnesium that magnesium oxide in reducing material is generated by magnesium Si reduction agent reduction forms steam, on the crystallizer on vacuum reactor top, crystallize into MAGNESIUM METAL, remaining slag charge after reduction reaction, main component is 2CaOSiO
2, as shown in vacuum reducing reaction equation (1).
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| CN113278821A (en) * | 2021-04-30 | 2021-08-20 | 西安交通大学 | Method for directly reducing metal magnesium by taking pure silicon powder as reducing agent |
| CN116005007A (en) * | 2023-01-06 | 2023-04-25 | 濮阳濮耐高温材料（集团）股份有限公司 | Method for preparing magnesium metal and magnesium aluminate spinel by aluminothermic reduction |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049381A (en) * | 1990-01-25 | 1991-02-20 | 颜志明 | Obtaining metal magnesium with vacuum-thermal method by burning magnesite slightly in magnesite |
| CN1098143A (en) * | 1993-07-28 | 1995-02-01 | 东北大学 | With magnesite and rhombspar is the aluminothermy for smelting Mg of raw material |
| CN1584076A (en) * | 2004-06-04 | 2005-02-23 | 郭清富 | Method for preparing magnesium with silica-alumina alloy as electronating agent |
| CN101812599A (en) * | 2010-03-18 | 2010-08-25 | 吉林大学 | Method for preparing metal magnesium by using dolomite as raw material |
| 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 |
| CN102560149A (en) * | 2012-03-08 | 2012-07-11 | 东北大学 | Method for refining magnesium by taking silico-calcium alloy as reducing agent under vacuum |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5836656B2 (en) * | 1979-04-23 | 1983-08-10 | 日本重化学工業株式会社 | Manufacturing method of magnesium metal |
-
2012
- 2012-09-13 CN CN201210336399.1A patent/CN102864315B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049381A (en) * | 1990-01-25 | 1991-02-20 | 颜志明 | Obtaining metal magnesium with vacuum-thermal method by burning magnesite slightly in magnesite |
| CN1098143A (en) * | 1993-07-28 | 1995-02-01 | 东北大学 | With magnesite and rhombspar is the aluminothermy for smelting Mg of raw material |
| CN1584076A (en) * | 2004-06-04 | 2005-02-23 | 郭清富 | Method for preparing magnesium with silica-alumina alloy as electronating agent |
| CN101812599A (en) * | 2010-03-18 | 2010-08-25 | 吉林大学 | Method for preparing metal magnesium by using dolomite as raw material |
| 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 |
| CN102560149A (en) * | 2012-03-08 | 2012-07-11 | 东北大学 | Method for refining magnesium by taking silico-calcium alloy as reducing agent under vacuum |
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