WO2011127672A1 - 一种真空还原制取金属镁的方法 - Google Patents

一种真空还原制取金属镁的方法 Download PDF

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WO2011127672A1
WO2011127672A1 PCT/CN2010/073128 CN2010073128W WO2011127672A1 WO 2011127672 A1 WO2011127672 A1 WO 2011127672A1 CN 2010073128 W CN2010073128 W CN 2010073128W WO 2011127672 A1 WO2011127672 A1 WO 2011127672A1
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cao
aluminum
mgo
magnesium
reducing agent
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French (fr)
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冯乃祥
王耀武
胡文鑫
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Northeastern University China
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Northeastern University China
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    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • C—CHEMISTRY; METALLURGY
    • 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
    • C22B5/16—Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced

Definitions

  • the present invention relates to a method for preparing magnesium metal, and more particularly to a method for preparing magnesium metal by vacuum reduction using a material having a molar ratio of MgO/CaO of more than 1 using aluminum or an aluminum alloy as a reducing agent.
  • the former method uses electrolytic cells using graphite as an anode to electrolyze magnesium chloride, and the electrolytic reaction is to form Cl 2 at the anode, to form magnesium metal at the cathode, to use a chloride electrolyte system by electrolysis, and to generate chlorine gas on the anode, which is liable to cause an environment. Pollution, the investment in environmental protection costs of treating waste gas residue is large, and the energy consumption of electrolysis is high.
  • the vacuum metal thermal reduction method has no environmental pollution like electrolysis, equipment corrosion is small, and the method has small investment, simple process, and low production cost, so the method is widely used in China, but the method is widely used.
  • silicon iron is mostly used as a reducing agent of 75% Si, which is generally called a silicon thermal method.
  • the reason for the high energy consumption and low productivity of silicon thermal smelting is the ratio of the reduced material to the produced magnesium, which is commonly referred to as the material/magnesium ratio.
  • the feed/magnesium ratio is about 6:1, which means that 6 tons of reduced material is needed to produce one ton of magnesium metal.
  • Dolomite is used as raw material.
  • the molecular formula of dolomite is MgC0 3 ⁇ CaC0 3 , that is, dolomite consists of one molecule of MgCO 3 and one molecule of CaC0 3 . After calcination, it becomes a molecule of MgO and a molecule of CaO.
  • the reduction material used in the current metal thermal reduction method is a reduction reaction material having a molar ratio of MgO/CaO of 1. It is compounded with silicon in ferrosilicon according to reaction formula (1), and reduced to magnesium metal under vacuum conditions and at a temperature higher than 120 CTC.
  • silicon-aluminum alloy is also used as a reducing agent, but the raw material used is still dolomite, so it does not change the molar ratio of MgO/CaO in the reducing material.
  • the magnesium/magnesium ratio cannot be lowered, so the productivity of the metal thermal reduction magnesium smelting can not be improved, and the energy consumption can be reduced.
  • the magnesium smelting technology of the silicon aluminum alloy as a reducing agent has not been experimentally carried out in industrial life. Summary of the invention:
  • the present invention provides a method for vacuum-reducing magnesium metal by using aluminum or aluminum alloy as a reducing agent with a MgO/CaO molar ratio of more than 1. It is to reduce the consumption of raw materials, greatly increase the productivity of magnesium and greatly reduce the energy consumption of magnesium smelting, so that the economic efficiency of the magnesium plant can be greatly improved.
  • a specific solution for implementing the present invention includes the following steps:
  • the dolomite, magnesite ore, brucite and limestone are used as raw materials for calcination.
  • the calcination temperature of dolomite is 1000 ⁇ 1200 °C, and the CaO ⁇ MgO material is obtained after calcination;
  • the calcination temperature of magnesite ore is 800 ⁇ 1000 ° C, after calcination to obtain MgO-containing materials;
  • Two or more of the above four materials are mixed to prepare a raw material having a MgO/CaO molar ratio of more than 1.
  • the raw materials prepared above are ground to less than 100 mesh in a ball mill and uniformly mixed to obtain a powder to be reduced.
  • the reaction equation based on the reaction theory is:
  • the reducing agent is industrial aluminum powder, industrial aluminum silicon alloy powder and industrial aluminum magnesium alloy powder, or recycled aluminum, aluminum silicon alloy or aluminum magnesium alloy powder prepared.
  • the reaction material is pressed into a dough or a block.
  • the lumps or block reaction materials are placed in a high-temperature vacuum reduction reactor with a magnesium crystallizer for vacuum reduction reaction.
  • the pressure in the reaction furnace is less than 30 Pa, and the reaction temperature is 900-1250 ° C.
  • the reaction produces gaseous magnesium metal.
  • the magnesium crystallizer condenses and crystallizes into metal magnesium and forms a slag.
  • the composition of the slag block includes CaO ⁇ 2A1 2 0 3 , CaO ⁇ A1 2 0 3 , CaO ⁇ 6A1 2 0 3 and 12CaO ⁇ 7Al 2 0
  • the ratio of CaO and MgO in the batch should also take into account the reduction of the component content of silicon in the reducing agent during the reduction process, and the reaction with CaO and MgO in the compound is satisfied.
  • the above MgO/CaO molar ratio is greater than 1, and the molar ratio thereof may be selected from 1.5 to 18.
  • the invention adopts the molar ratio of MgO/CaO in the reducing reaction material to be 1.5-18, and prepares magnesium metal by metal thermal reduction technology, for example, the molar ratio of MgO/CaO in the reducing reaction material is 6, and when industrial aluminum is used as a reducing agent, The material/magnesium ratio of the method is about 3.0, so that the energy consumption of the metal thermal reduction magnesium smelting can be reduced by more than 40%, and the productivity can be increased by more than 40%, so that the economic efficiency of the magnesium plant is greatly improved.
  • the reducing agent aluminum powder, the aluminum silicon alloy powder and the aluminum magnesium alloy powder used in the embodiment of the invention have a particle size of less than 1 mm; the reducing agent is industrial aluminum powder, industrial aluminum silicon alloy powder or industrial aluminum magnesium alloy powder, or recycled aluminum , powder prepared from aluminum-silicon alloy or aluminum-magnesium alloy.
  • the raw material after calcination is ground in a ball mill to below 100 mesh and uniformly mixed.
  • Metallic magnesium is prepared by vacuum aluminothermic reduction using dolomite and magnesite ore as raw materials and aluminum powder having a particle size of 1.0 mm or less as a reducing agent.
  • the dolomite with a molar ratio of CaC0 3 to MgCO 3 of 1:1 is calcined at a temperature of 1000 to 1200 ° C to obtain a material having a molar ratio of CaO to MgO of 1:1, and magnesite ore (main component is MgC0 3 ) Calcination is carried out at a temperature of 800 to 1000 ° C to obtain a magnesium oxide material.
  • the dolomite calcined product CaO*MgO is compounded with the calcined product MgO of magnesite ore, and the molar ratio of MgO/CaO in the calcined dolomite to the calcined magnesite mixture is 6.
  • the above two kinds of calcined materials are prepared in the above ratio, they are placed in a ball mill for grinding, and the above two kinds of calcined materials may be separately ground and then the above ingredients are uniformly mixed.
  • the above-mentioned uniformly mixed fine powder is blended into aluminum powder according to the ratio of the raw material and the reducing agent in the chemical reaction formula (1), and the aluminum powder is added in an amount of 3 to 10% more than the theoretical blending amount.
  • the actual amount of blending is more than the theoretical blending amount because the aluminum powder often contains some oxidized alumina.
  • the alumina does not reduce, but consumes the CaO component in the raw material.
  • the reducing agent aluminum powder also reduces some of the metal impurities in the reaction material during the reduction reaction to cause additional consumption of the reducing agent aluminum powder.
  • the reduction reaction material and the reducing agent aluminum powder are thoroughly mixed, they are pressed into a mass or other shaped block material, and then the agglomerates mixed with the reducing agent aluminum powder are placed in a high temperature vacuum reduction reaction with a magnesium crystallizer.
  • a magnesium crystallizer In the furnace, under the vacuum pressure of less than 20 Pa and the temperature of 900 ⁇ 1250 °C, the gaseous magnesium metal formed by the reaction of CaO, MgO and A1 in the material, the gaseous magnesium metal is condensed and crystallized on the magnesium crystallizer. magnesium.
  • Magnesium dolomite and magnesite are used as raw materials, aluminum powder is used as reducing agent, and high-temperature vacuum is used to obtain magnesium metal.
  • Magnesia dolomite is calcined at a temperature of 1000-115 CTC and magnesite at a temperature of 800-100 CTC, respectively, and magnesia dolomite containing about 73% MgO and about 27% CaO is prepared.
  • the two calcined materials are proportioned in proportion, and the ratio of the ratio of the two materials to the molar ratio of CaO to MgO is 1:6. If there are other impurities in the original mineral raw material, such as Si0 2 , press Si0. 2 In the high temperature reaction, it reacts with CaO to form 2CaOSi (CaO in the V-consuming raw material, and corrects the raw material ratio of the two calcined materials.
  • the aluminum powder is blended in an amount of 3 to 10% more than the theoretical blending amount of the chemical reaction formula (1). Then, the mixture is uniformly mixed, pressed into a dough, and then the mass is placed in a high-temperature vacuum reduction reactor with a magnesium crystallizer, and the reaction materials are reacted at a temperature of less than 20 Pa and 900 to 1250 ° C.
  • magnesium metal Using limestone and magnesite as raw materials, aluminum powder as reducing agent, and high-temperature vacuum reduction to obtain magnesium metal. It is assumed that the main chemical components of the two raw materials are CaC0 3 and MgCO 3 , respectively, and the impurity content thereof is small and negligible.
  • the above two mineral raw materials are calcined into CaO and MgO at a temperature of 1000-120 CTC (limestone) and 800-1000 ° C, respectively.
  • Calcined CaO and MgO are dosed 1:6, then mixed and ground, such as other chemical impurities in the raw material, reacting with CaO and MgO in the raw material at high temperature to cause CaO and MgO in the batch.
  • the ratio of the two calcined mineral ingredients can be appropriately adjusted and corrected.
  • the above-mentioned two kinds of calcined mineral ingredients after grinding are uniformly mixed with aluminum powder reducing agent exceeding 3 ⁇ 10% of the theoretical amount according to the reaction formula (1), and then pressed into agglomerates, and then the mass is placed into the belt.
  • the reaction mass is reacted at a temperature of less than 20 Pa and a temperature of 900-125 CTC, and the reaction is a gaseous magnesium metal formed, which is condensed and crystallized into magnesium metal on a crystallizer.
  • the dolomite and magnesite are used as raw materials, and the Al-Si alloy is used as a reducing agent for high-temperature vacuum reduction to obtain magnesium metal.
  • the Al-Si alloy in this embodiment is mainly a recovered silicon-containing cast Al-Si alloy. It is assumed that the aluminum-silicon alloy for casting is a eutectic aluminum-silicon alloy, and the content of silicon in the alloy is 12%.
  • the above two mineral raw materials are calcined at a temperature of 1000-1200 ° C (dolomite) and 800-1000 ° C (magnesite), and the product after calcination is CaO * MgO, magnesite calcined product For MgO.
  • the ground calcined dolomite and the calcined magnesite are compounded, and then a reducing agent Al-Si alloy powder is blended.
  • the reducing agent used is a reducing agent of a eutectic aluminum-silicon alloy containing 12% Si
  • the doping amount of the calcined dolomite and the calcined magnesite is respectively involved in the high-temperature reduction reaction of A1 and Si in the reducing agent.
  • the reaction is carried out, wherein the reduction reaction of A1 in the alloy requires the compounding of the raw material, and the molar ratio of CaO to MgO in the mixed mixture is 1:6; and the amount of the reducing reactant of Si in the alloy is mixed according to the mixture.
  • the molar ratio of CaO to MgO was 1:1. Since the main impurity in the two mineral raw materials is Si0 2 , it is considered in the compounding that the CaO reaction in the calcined material of the SiO 2 and the dolomite in the high temperature reaction process will produce the 2CaOSi0 2 compound to cause CaO in the raw material ratio. The loss, therefore, the CaO loss caused by Si0 2 is corrected in the ingredients.
  • the reducing agent uses recycled cast aluminum-silicon alloy, in which both A1 and Si are reducing agents, wherein A1 participates in the reduction reaction of the material according to the chemical reaction formula (1) in the high-temperature vacuum reactor.
  • the Si in the alloy participates in the reduction reaction of the material according to the chemical reaction formula (2), and the common ingredients are calculated according to the components in the aluminum-silicon alloy according to the reaction formulas (1) and (2), considering that oxide impurities may be present in the reducing agent alloy.
  • oxide impurities may be present in the reducing agent alloy.
  • some metal oxide impurities in the raw materials are reduced at high temperature In the reaction, the reaction with aluminum and silicon participates in the loss of the reducing agent. Therefore, the compounding amount of the reducing agent needs to be larger than the theoretical dosage amount calculated by the reaction formula by 3 to 10%.
  • the dolomite calcined material and the magnesite calcined material are mixed and ground in a ball mill, and then mixed with a reducing agent (the reducing agent is added to the material as a fine powder). And then pressed into agglomerates, placed in a high-temperature vacuum reactor with a magnesium crystallizer, reacted at a temperature of less than 20 Pa and 900-125 CTC, and reacted to form gaseous magnesium metal. It is condensed and crystallized into magnesium metal on a crystallizer.
  • Magnesia and magnesite ore are used as raw materials, and aluminum powder is used as a reducing agent to reduce magnesium metal in a vacuum.
  • the dolomite with CaCO 3 and MgCO 3 molar ratio of 1:1 is calcined at a temperature of 1000-120 CTC to obtain a material having a CaO and MgO molar ratio of 1:1, and the magnesite ore (main component is MgCO 3 ) at 800 Calcination is carried out at a temperature of ⁇ 1000 ° C to obtain a magnesium oxide material.
  • the dolomite calcined product CaO*MgO is mixed with the magnesite ore calcined product MgO, so that the molar ratio of CaO and MgO in the mixture of calcined dolomite and calcined magnesite is 1: 18, when some other metals and non-metallic impurities are contained in the two minerals, the influence of the impurities on the reactants should be considered, and the above ingredients should be appropriately modified.
  • the molar ratio of CaO in the raw material mixture should be appropriately increased in the ratio of the two calcined raw materials. Or appropriately reduce the amount of MgO blended.
  • the above two kinds of calcined materials are prepared in the above ratio, they are placed in a ball mill for grinding, and the above two kinds of calcined materials may be separately ground and then the above ingredients are uniformly mixed.
  • the above-mentioned uniformly mixed milled material is blended into aluminum powder according to the ratio of the raw material and the reducing agent in the chemical reaction formula (1), and the aluminum powder is added in an amount of 3-10% more than the theoretical blending amount.
  • the actual amount of blending is more than the theoretical blending amount because the reducing agent aluminum powder also reduces some of the metal impurities in the reaction material during the reduction reaction to cause additional consumption of the reducing agent aluminum powder.
  • the reduction reaction material and the reducing agent aluminum powder are thoroughly mixed, they are pressed into a mass or a block of other shapes, and then the agglomerates mixed with the reducing agent aluminum powder are placed in a high temperature vacuum reactor with a magnesium crystallizer. Inside, under a vacuum pressure of less than 20 Pa and a temperature of 1150-135 CTC, the gaseous magnesium metal formed by the reaction of CaO, MgO and A1 in the material is condensed and crystallized into crystalline magnesium on a magnesium crystallizer.
  • Magnesia and magnesite ore are used as raw materials, and aluminum powder is used as a reducing agent to reduce magnesium metal in a vacuum.
  • the dolomite with CaCO 3 and MgCO 3 molar ratio of 1:1 is calcined at a temperature of 1000-120 CTC to obtain a material having a CaO and MgO molar ratio of 1:1, and the magnesite ore (main component is MgCO 3 ) at 800 Calcination is carried out at a temperature of -1000 ° C to obtain a magnesium oxide material.
  • the dolomite calcined product CaO * MgO and magnesite The calcined product MgO of the stone is compounded so that the molar ratio of CaO to MgO in the mixture of calcined dolomite and calcined magnesite is 12: 21, when the two minerals contain some other metallic and non-metallic impurities, The influence of impurities on the reactants should be considered. Appropriate corrections should be made to the above ingredients. For example, when there is SiO 2 impurity content in the raw material, it should be considered that Si0 2 reacts with CaO in dolomite to form 2CaO * Si0 2 compound at high temperature. Therefore, in this case, the molar ratio of CaO in the raw material mixture should be appropriately increased in the ratio of the two raw materials after calcination, or the amount of MgO blended should be appropriately reduced.
  • the above two kinds of calcined materials are prepared in the above ratio, they are placed in a ball mill for grinding, and the above two kinds of calcined materials may be separately ground and then the above ingredients are uniformly mixed.
  • the above-mentioned uniformly mixed milled material is blended into aluminum powder according to the ratio of the raw material and the reducing agent in the chemical reaction formula (1), and the aluminum powder is added in an amount of 3-10% more than the theoretical blending amount.
  • the actual amount of blending is more than the theoretical blending amount because the reducing agent aluminum powder also reduces some of the metal impurities in the reaction material during the reduction reaction to cause additional consumption of the reducing agent aluminum powder.
  • the reduction reaction material and the reducing agent aluminum powder are thoroughly mixed, they are pressed into a mass or a block of other shapes, and then the agglomerates mixed with the reducing agent aluminum powder are placed in a high temperature vacuum reactor with a magnesium crystallizer. Inside, at a vacuum pressure of less than 20 Pa and a temperature of 900-125 CTC, the gaseous magnesium metal formed by the reaction of CaO, MgO and A1 in the material.
  • Magnesia and magnesite ore are used as raw materials, and aluminum powder is used as a reducing agent to reduce magnesium metal in a vacuum.
  • the dolomite with CaCO 3 and MgCO 3 molar ratio of 1:1 is calcined at a temperature of 1000-120 CTC to obtain a material having a CaO and MgO molar ratio of 1:1, and the magnesite ore (main component is MgCO 3 ) at 800 Calcination is carried out at a temperature of -1000 ° C to obtain a magnesium oxide material.
  • the dolomite calcined product CaO*MgO is mixed with the magnesite ore calcined product MgO, so that the molar ratio of CaO and MgO in the mixture of calcined dolomite and calcined magnesite is 1: 3, when some other metals and non-metallic impurities are contained in the two minerals, the influence of the impurities on the reactants should be considered, and the above ingredients should be appropriately modified, such as the presence of SiO 2 impurities in the raw materials.
  • the molar ratio of CaO in the raw material mixture should be appropriately increased in the ratio of the two calcined raw materials. Or appropriately reduce the amount of MgO blended.
  • the above two kinds of calcined materials are prepared in the above ratio, they are placed in a ball mill for grinding, and the above two kinds of calcined materials may be separately ground and then the above ingredients are uniformly mixed.
  • the above-mentioned uniformly mixed fine powder is blended into aluminum powder according to the ratio of the raw material and the reducing agent in the chemical reaction formula (1), and the aluminum powder is added in an amount of 3 to 10% more than the theoretical blending amount.
  • the actual amount of blending is more than the theoretical blending amount because the reducing agent aluminum powder also reduces some of the metal impurities in the reaction material during the reduction reaction to cause additional consumption of the reducing agent aluminum powder.
  • the reducing reaction material and the reducing agent aluminum powder are thoroughly mixed, they are pressed into a mass or other shaped block material, and then These agglomerates mixed with reducing agent aluminum powder are placed in a high-temperature vacuum reactor with a magnesium crystallizer. Under vacuum conditions of less than 20 Pa and temperatures of 900-125 CTC, CaO, MgO and A1 in the material.
  • the reaction yields two products, one is gaseous magnesium metal formed by the reaction, the gaseous magnesium metal is condensed and crystallized on the magnesium crystallizer to form crystalline magnesium, and the other reaction product has a main chemical composition of CaO ⁇ A1 2 0 3 .
  • the raw material is the same as in the seventh embodiment, and the reducing agent is made of aluminum-magnesium alloy powder.
  • the ratio of the raw materials is the same as that of the embodiment 7.
  • the reducing agent is metered in the same manner as in the embodiment 7.
  • the reaction method is the same as that in the embodiment 7.
  • the magnesium in the reducing agent finally forms crystalline magnesium metal.

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Description

一种真空还原制取金属镁的方法
技术领域- 本发明涉及一种金属镁的制备方法， 特别涉及一种以铝或铝合金为还原剂以 MgO/CaO 摩尔比大于 1的物料为原料真空还原制取金属镁的方法。
背景技术：
目前工业上纯镁的冶炼方法有两种， 一种是熔盐电解法， 另一种是真空金属热还原法。 前一种方法使用以石墨作为阳极的电解槽电解氯化镁， 其电解反应为在阳极生成 Cl2， 在阴极 生成金属镁， 由于电解法使用氯化物电解质体系， 且阳极上产生氯气， 所以容易造成环境污 染， 处理废气废渣的环保费用的投资大， 且电解的能耗高。 相比之下， 真空金属热还原法由 于没有像电解法那样的环境污染， 设备腐蚀小， 且该方法投资小， 工艺简单， 生产成本低， 因此该方法在我国被广泛地采用， 但是该方法也有其缺点， 这些缺点就是能耗很大， 生产率 很低。 目前在真空金属热还原法生产镁时， 大都是以 75%Si的硅铁作还原剂， 通常称为硅热 法。 硅热法炼镁能耗大和生产率低的原因是还原物料与产出的镁之比， 即通常所说的料 /镁比 非常大。 在工业生产上料 /镁比约为 6： 1， 也就是说生产一吨金属镁需要 6吨的还原物料， 造成料镁比如此之低的一个主要原因是目前的金属热还原炼镁均使用白云石为原料， 白云石 的分子式为 MgC03 · CaC03， 即白云石由一个分子的 MgC03和一个分子的 CaC03组成， 其煅 烧后变为一个分子的 MgO和一个分子的 CaO组成的化合物， 即目前金属热还原法所用的还原 物料为 MgO/CaO摩尔比为 1 的还原反应物料。 其与硅铁中的硅按反应式 （1 ) 进行配料， 在 真空条件和高于 120CTC的温度下还原生成金属镁。
2CaO + 2MgO + Si (Fe) = 2Mg + 2CaO · Si02
这就是目前国内外广泛使用的硅热法真空热还原炼镁技术。 因为这一技术是由加拿大人 Pidgeon (皮江） 发明的， 因此也称之为 Pidgeon法 （皮江法） 炼镁技术。 从上述分析可以看 出， 如果要让金属热还原法炼镁技术的能耗大幅度地降低， 则必须要从源头上， 即从原料配 料和还原剂上进行重大的改革， 使金属热还原反应的物料中的 MgO的量大大提高， CaO的 量大大减少， 这样才能使料 /镁比大大地降低， 从而达到使生产率大大提高， 能耗大大降低的 目的。 在金属热还原法炼镁的研究工作中， 也有用硅铝合金作还原剂的， 但其所使用的原料 仍然为白云石， 因此并不能使还原物料中的 MgO/CaO摩尔比发生改变， 料 /镁比也不能降低， 因此也就不能使金属热还原炼镁生产率得到提高， 能耗得以降低， 这样硅铝合金作为还原剂 的炼镁技术也未能在工业生得以实验。 发明内容：
针对目前工业硅热真空还原法炼镁所存在的问题， 本发明提供一种以铝或铝合金为还原 剂以 MgO/CaO摩尔比大于 1的物料为原料真空还原制取金属镁的方法， 目的在于减少原料 消耗， 大幅提高镁的生产率和大幅降低炼镁的能量消耗， 从而可以大大地提高镁厂的经济效πϊ-。
实现本发明的具体方案包括以下步骤：
1、 原料的准备：
以白云石、 菱镁矿石、 水镁石和石灰石为原料， 分别进行煅烧， 其中白云石的煅烧温度 为 1000~1200°C， 煅烧后获得含 CaO · MgO物料； 菱镁矿石的煅烧温度为 800~1000°C， 煅烧 后获得含 MgO物料； 水镁石的煅烧温度为 800~1000°C， 煅烧后获得含 MgO物料； 石灰石的 煅烧温度为 1000~1200°C， 煅烧后获得含 CaO物料； 将上述四种物料中的两种或两种以上混 合， 配制成 MgO/CaO摩尔比大于 1的原料。
2、 将上述配制的原料在球磨机中磨细至 100目以下并混合均匀， 获得待还原粉料。
3、 在待还原粉料中加入粒度在 1mm以下的还原剂铝粉或铝合金粉， 制成反应物料， 还 原剂的加入量为反应理论所需用量的 1.03~1.1倍，其中铝合金粉为铝硅合金粉或铝镁合金粉， 反应理论所根据的反应方程式为：
3MgO + 2A1= 3Mg +A1203 ( 1 )
3MgO + 2Si= 3Mg + Si203 ( 2 )
所述的还原剂为工业铝粉、 工业铝硅合金粉和工业铝镁合金粉， 或回收的铝、 铝硅合金 或铝镁合金制备的粉料。
4、 将反应物料压制成团状或块状。
5、 将团状或块状反应物料置于带有镁结晶器的高温真空还原反应炉内进行真空还原反 应， 反应炉内压力小于 30Pa， 反应温度 900~1250°C， 反应生成气态金属镁在镁结晶器上冷凝 结晶成金属镁， 并生成渣块， 渣块的成分包括 CaO · 2A1203、 CaO · A1203、 CaO · 6A1203和 12CaO · 7Al20
上述方法中的铝的还原反应分别按以下反应式进行：
CaO + 6MgO + 4A1 = 6Mg + CaO · 2A1203 (3)
CaO + 18MgO + 12A1 = 18Mg + CaO · 6A1203 (4)
12CaO + 21MgO + 14A1 = 21Mg + 12CaO · 7A1203 (5) CaO + 3MgO + 2A1 = 3Mg + CaO · A1203 (6)
当还原剂使用铝硅合金粉时， 配料中 CaO和 MgO的配比还应考虑到还原剂中硅的组分 含量在还原过程中所起的还原作用， 其与配料中 CaO和 MgO的反应满足如下反应方程式对 CaO和 MgO量的要求。
硅的还原反应按以下反应式进行：
2CaO + 2MgO + Si = 2Mg + 2CaO · Si02 (7)
上述方法中当原料中存在 3102杂质时， 煅烧后配制原料时相应提高 CaO的加入量， 或降低 MgO的加入量， 通过计算 3102与。&0反应后剩余的 CaO符合步骤 1 的配比要求； Si02与 CaO反应的方程式为：
2CaO + Si02=2CaO · Si02
上述的 MgO/CaO摩尔比大于 1， 其摩尔比可选择 1.5~18。
本发明采用还原反应物料中 MgO/CaO摩尔比为 1.5~18， 通过金属热还原技术制备金属 镁， 如还原反应物料中 MgO/CaO摩尔比为 6， 且以工业废铝为还原剂时， 可使本方法的料 / 镁比达到 3.0左右， 这样就可以使金属热还原法炼镁的能耗降低 40%以上， 生产率提高 40% 以上， 使镁厂的经济效益大大提高。
具体实施方式
本发明实施例中采用的还原剂铝粉、铝硅合金粉和铝镁合金粉的粒度在 1mm以下； 还原 剂为工业铝粉、 工业铝硅合金粉或工业铝镁合金粉， 或回收的铝、 铝硅合金或铝镁合金制备 的粉料。
本发明实施例中煅烧后的原料配料后在球磨机中磨细至 100目以下并混合均匀。
实施例 1
以白云石和菱镁矿石为原料， 以粒度 1.0mm以下的铝粉为还原剂的真空铝热还原制取金 属镁。
将 CaC03与 MgC03摩尔比为 1： 1的白云石在 1000~1200°C的温度下煅烧制得 CaO和 MgO摩 尔比为 1： 1的物料， 将菱镁矿石 （主要成分为 MgC03) 在 800~1000°C的温度条件下进行煅 烧， 制得氧化镁物料。 将白云石煅后产物 CaO * MgO与菱镁矿石的煅后产物 MgO进行配料， 其煅后白云石与煅后菱镁石混合物中 MgO/CaO摩尔比为 6。
当两种矿物中含有某些其它的金属和非金属杂质时， 应考虑杂质对反应物的影响， 对上 述配料进行适当的修正， 如原料中存在着 Si02杂质含量时， 应考虑 Si02在高温反应时会与白 云石中的 CaO反应生成 2CaO * Si02化合物， 因此在这种情况下， 两种煅烧后的原料的配比中 应适当提高原料配料中 CaO的摩尔量， 或适当减少 MgO的配入量。
将上述两种煅后料按上述比例配好后， 放入球磨机中进行磨细， 也可以将上述两种煅后 料分别进行磨细然后再将上述配料混合均匀。
将上述均匀混合后的磨细料， 按化学反应式（1 ) 中原料与还原剂的配比配入铝粉， 铝粉 的配入量应比理论配入量多 3~10%。 实际配入量之所以要比理论配入量多是因为铝粉中常含 有一些被氧化的氧化铝， 氧化铝不起还原作用， 但会消耗原料中的 CaO组分。 除此之外， 还 原剂铝粉在还原反应中还会还原反应物料中的某些金属杂质而使还原剂铝粉产生额外的消 耗。
将还原反应物料和还原剂铝粉进行充分混合后， 压制成团或其它形状的块状料， 然后将 这些混有还原剂铝粉的团块料放入带有镁结晶器的高温真空还原反应炉内， 在小于 20 Pa以 下的真空压力和 900~1250°C的温度条件下， 物料中的 CaO， MgO和 A1反应生成的气态金属 镁， 气态的金属镁在镁结晶器上冷凝结晶成结晶镁。
实施例 2
以镁化白云石和菱镁石为原料， 以铝粉为还原剂， 高温真空还原制取金属镁。 中国辽宁 省南部有一种矿物， 其主要的化学组成为 CaC03和 MgC03， 煅烧后其主要化学组成为 CaO和 MgO , 其质量比为 27 : 73。 分别将镁化白云石在 1000-115CTC的温度条件下和菱镁石在 800-100CTC的温度条件下煅烧， 并分别制取含 MgO为 73%左右, 含 CaO为 27%左右的镁化白 云石和含主要成分为 MgO的菱镁石两种矿石的煅后料。
将两种煅后料按比例进行配料， 两种物料的配料比例按其混合后的 CaO与 MgO的摩尔比为 1： 6， 如果原矿物原料中还有其他杂质， 如 Si02， 要按 Si02在高温反应中与 CaO反应生成 2CaOSi(V 耗原料中的 CaO， 对两种煅后料的原料配比进行修正。
将上述两种煅后料按上述配料配好后在球磨机上进行混合和磨细成细粉后， 按比化学反 应式（1 ) 的理论配入量多 3~10%的量配入铝粉， 然后混合均匀， 压制成团， 然后将此团块置 于带有镁结晶器的高温真空还原反应炉内，在小于 20Pa和 900~1250°C温度的条件下，使反应 物料进行反应， 反应得到两种产物， 一种是气态的金属镁， 气态的金属镁在结晶器上冷凝结 晶成金属镁， 另一种反应产物其主要化学组成为 CaO · 2A1203， 以及少量的 CaO * A1203。。 实施例 3
以石灰石和菱镁石为原料， 以铝粉为还原剂， 高温真空还原制取金属镁。 假定两种原料的主要化学成分分别为 CaC03和 MgC03， 其中的杂质含量很少， 可忽略不 计。
将上述两种矿物原料分别在 1000-120CTC (石灰石） 和 800-1000°C的温度下煅烧成 CaO 禾口 MgO。
煅烧成的 CaO和 MgO按摩尔比 1： 6进行配料， 然后进行混合磨细， 如原料中存在有其 它化学杂质， 在高温条件下与原料中的 CaO和 MgO反应造成配料中的 CaO和 MgO部分消 耗时， 可适当地对两种煅烧后的矿物配料的配比进行调整和修正。
将磨细后的上述两种煅烧后的矿物配料与超过按反应方程式 （1 ) 的理论量过量 3~10% 的铝粉还原剂混合均匀后压制成团块，然后将此团块置入带有镁结晶器的高温真空反应炉内， 在小于 20Pa和 900-125CTC温度的条件下，使反应物料进行反应，反应是生成的气态的金属镁， 在结晶器上冷凝结晶成金属镁。
实施例 4
以白云石和菱镁矿为原料， 以 Al-Si合金为还原剂高温真空还原制取金属镁。
在此实施例中的 Al-Si合金主要是回收的含硅的铸造 Al-Si合金。假定这种铸造用的铝硅 合金为共晶铝硅合金， 合金中硅的含量为 12%。
首先将上述两种矿物原料分别在 1000~1200°C (白云石） 和 800~1000°C (菱镁石） 的温 度下进行煅烧， 白云石煅烧后产物为 CaO * MgO， 菱镁石煅烧产物为 MgO。
用磨细后的煅后白云石与煅后菱镁石进行配料， 然后配入还原剂 Al-Si合金粉。 由于使用 的还原剂为含 12%Si的共晶铝硅合金的还原剂， 因此煅后白云石和煅后菱镁石的配料量分别 按照还原剂中的 A1和 Si在高温还原反应中所参与的反应进行配料， 其中合金中 A1的还原反应 对原料的配料要求， 按所配得的混合物料中 CaO和 MgO的摩尔比 1： 6; 而合金中 Si的还原反 应剂的配入量按混合料中 CaO与 MgO的摩尔比为 1： 1进行配料。由于两种矿物原料中的主要 杂质为 Si02， 因此在配料中要考虑到在高温反应过程中 Si02与白云石煅烧后料中的 CaO反应 会生成 2CaOSi02的化合物造成原料配比中的 CaO的损失， 因此配料中要对 Si02而造成的 CaO 损失加以修正。
在此实施例中， 还原剂使用回收的铸造铝硅合金， 合金中 A1和 Si都是还原剂， 其中的 A1在高温真空反应炉中按化学反应式 （1 ) 参与对物料的还原反应， 而合金中的 Si按化学反 应式 （2)参与物料的还原反应， 同时按铝硅合金中的成分按反应式 （1 )和 （2)计算共同配 料， 考虑到还原剂合金中可能存在氧化物杂质以及原料中的某些金属氧化物杂质在高温还原 反应中参与和铝和硅的反应而造成还原剂的损失， 因此， 还原剂的配料量需大于按反应式计 算的理论配料量 3~10%。 按上述配料量配出的白云石煅后料和菱镁石煅后料放入球磨机内进 行混合和磨细， 之后再配入还原剂 （还原剂以细粉的方式加入到物料中） 混合均匀， 然后压 制成团块，将团块放入带有镁结晶器的高温真空反应炉内，在小于 20Pa和 900-125CTC温度的 条件下， 使反应物料进行反应， 反应生成的气态的金属镁， 在结晶器上冷凝结晶成金属镁。 实施例 5
以白云石和菱镁矿石为原料， 以铝粉为还原剂真空还原金属镁。
将 CaC03与 MgC03摩尔比为 1： 1的白云石在 1000-120CTC的温度下煅烧制得 CaO和 MgO摩 尔比为 1： 1的物料， 将菱镁矿石 （主要成分为 MgC03 ) 在 800~1000°C的温度条件下进行煅 烧， 制得氧化镁物料。 然后按化学反应方程式 （1 )， 将白云石煅后产物 CaO * MgO与菱镁矿 石的煅后产物 MgO进行配料， 使煅后白云石与煅后菱镁石混合物中 CaO和 MgO的摩尔比为 1： 18， 当两种矿物中含有某些其它的金属和非金属杂质时， 应考虑杂质对反应物的影响， 对 上述配料进行适当的修正， 如原料中存在着 Si02杂质含量时， 应考虑 Si02在高温反应时会与 白云石中的 CaO反应生成 2CaO * Si02化合物， 因此在这种情况下， 两种煅烧后的原料的配比 中应适当提高原料配料中 CaO的摩尔量， 或适当减少 MgO的配入量。
将上述两种煅后料按上述比例配好后， 放入球磨机中进行磨细， 也可以将上述两种煅后 料分别进行磨细然后再将上述配料混合均匀。
将上述均匀混合后的磨细料， 按化学反应式（1 ) 中原料与还原剂的配比配入铝粉， 铝粉 的配入量应比理论配入量多 3-10%。 实际配入量之所以要比理论配入量多是因为还原剂铝粉 在还原反应中还会还原反应物料中的某些金属杂质而使还原剂铝粉产生额外的消耗。
将还原反应物料和还原剂铝粉进行充分混合后， 压制成团或其它形状的块状料， 然后将 这些混有还原剂铝粉的团块料放入带有镁结晶器的高温真空反应炉内， 在小于 20 Pa以下的 真空压力和 1150-135CTC的温度条件下， 物料中的 CaO， MgO和 A1反应生成的气态金属镁， 在镁结晶器上冷凝结晶成结晶镁。
实施例 6
以白云石和菱镁矿石为原料， 以铝粉为还原剂真空还原金属镁。
将 CaC03与 MgC03摩尔比为 1： 1的白云石在 1000-120CTC的温度下煅烧制得 CaO和 MgO摩 尔比为 1： 1的物料， 将菱镁矿石 （主要成分为 MgC03 ) 在 800-1000°C的温度条件下进行煅 烧， 制得氧化镁物料。 然后按化学反应方程式 （1 )， 将白云石煅后产物 CaO * MgO与菱镁矿 石的煅后产物 MgO进行配料， 使煅后白云石与煅后菱镁石混合物中 CaO和 MgO的摩尔比为 12： 21 , 当两种矿物中含有某些其它的金属和非金属杂质时， 应考虑杂质对反应物的影响， 对上述配料进行适当的修正， 如原料中存在着 Si02杂质含量时， 应考虑 Si02在高温反应时会 与白云石中的 CaO反应生成 2CaO * Si02化合物， 因此在这种情况下， 两种煅烧后的原料的配 比中应适当提高原料配料中 CaO的摩尔量， 或适当减少 MgO的配入量。
将上述两种煅后料按上述比例配好后， 放入球磨机中进行磨细， 也可以将上述两种煅后 料分别进行磨细然后再将上述配料混合均匀。
将上述均匀混合后的磨细料， 按化学反应式（1 ) 中原料与还原剂的配比配入铝粉， 铝粉 的配入量应比理论配入量多 3-10%。 实际配入量之所以要比理论配入量多是因为还原剂铝粉 在还原反应中还会还原反应物料中的某些金属杂质而使还原剂铝粉产生额外的消耗。
将还原反应物料和还原剂铝粉进行充分混合后， 压制成团或其它形状的块状料， 然后将 这些混有还原剂铝粉的团块料放入带有镁结晶器的高温真空反应炉内， 在小于 20 Pa以下的 真空压力和 900-125CTC的温度条件下， 物料中的 CaO， MgO和 A1反应生成的气态金属镁。 实施例 7
以白云石和菱镁矿石为原料， 以铝粉为还原剂真空还原金属镁。
将 CaC03与 MgC03摩尔比为 1： 1的白云石在 1000-120CTC的温度下煅烧制得 CaO和 MgO摩 尔比为 1： 1的物料， 将菱镁矿石 （主要成分为 MgC03 ) 在 800-1000°C的温度条件下进行煅 烧， 制得氧化镁物料。 然后按化学反应方程式 （1 )， 将白云石煅后产物 CaO * MgO与菱镁矿 石的煅后产物 MgO进行配料， 使煅后白云石与煅后菱镁石混合物中 CaO和 MgO的摩尔比为 1： 3， 当两种矿物中含有某些其它的金属和非金属杂质时， 应考虑杂质对反应物的影响， 对 上述配料进行适当的修正， 如原料中存在着 Si02杂质含量时， 应考虑 Si02在高温反应时会与 白云石中的 CaO反应生成 2CaO * Si02化合物， 因此在这种情况下， 两种煅烧后的原料的配比 中应适当提高原料配料中 CaO的摩尔量， 或适当减少 MgO的配入量。
将上述两种煅后料按上述比例配好后， 放入球磨机中进行磨细， 也可以将上述两种煅后 料分别进行磨细然后再将上述配料混合均匀。
将上述均匀混合后的磨细料， 按化学反应式（1 ) 中原料与还原剂的配比配入铝粉， 铝粉 的配入量应比理论配入量多 3~10%。 实际配入量之所以要比理论配入量多是因为还原剂铝粉 在还原反应中还会还原反应物料中的某些金属杂质而使还原剂铝粉产生额外的消耗。
将还原反应物料和还原剂铝粉进行充分混合后， 压制成团或其它形状的块状料， 然后将 这些混有还原剂铝粉的团块料放入带有镁结晶器的高温真空反应炉内，在小于 20 Pa以下的真 空压力和 900-125CTC的温度条件下， 物料中的 CaO， MgO和 A1反应得到两种产物， 一种是反 应生成的气态金属镁， 气态的金属镁在镁结晶器上冷凝结晶成结晶镁， 另一种反应产物其主 要化学组成为 CaO · A1203。
实施例 8
原料同实施例 7， 还原剂采用铝镁合金粉， 原料配比方式同实施例 7， 还原剂计量方式同 实施例 7， 反应方式同实施例 7， 还原剂中的镁最终形成结晶金属镁。

Claims

杈 利 要 求 书
1、 一种以铝或铝合金为还原剂以 MgO/CaO摩尔比大于 1 的物料为原料真空还原制取 金属镁的方法， 其特征在于按以下步骤进行：
( 1 ) 以白云石、 菱镁矿石、 水镁石和石灰石为原料， 分别进行煅烧， 其中白云石的煅 烧温度为 1000~1200°C， 煅烧后获得含 CaO · MgO物料； 菱镁矿石的煅烧温度为 800~1000 。C， 煅烧后获得含 MgO物料； 水镁石的煅烧温度为 800~1000°C， 煅烧后获得含 MgO物料； 石灰石的煅烧温度为 1000~1200°C， 煅烧后获得含 CaO物料； 将上述四种物料中的两种或两 种以上混合， 配制成 MgO/CaO摩尔比大于 1的原料；
(2) 将上述配制的原料在球磨机中磨细至 100目以下并混合均匀， 获得待还原粉料；
( 3 )在待还原粉料中加入还原剂， 还原剂为粒度在 lmm以下的铝粉或铝合金粉， 制成 反应物料， 还原剂的加入量为反应理论所需用量的 1.03~1.1倍； 所述的铝合金粉为铝硅合金 粉或铝镁合金粉；
(4) 将反应物料压制成团状或块状；
( 5 ) 将团状或块状反应物料置于带有镁结晶器的高温真空还原反应炉内进行真空还原 反应， 反应炉内压力小于 30Pa， 反应温度 900~1250°C， 反应生成气态金属镁在镁结晶器上冷 凝结晶成金属镁。
2、 根据权利要求 1所述的以铝或铝合金为还原剂以 MgO/CaO摩尔比大于 1的物料 为原料真空还原制取金属镁的方法， 其特征在于所述的原料中存在 3102杂质或采用的还 原剂铝合金中存在硅组分时， 煅烧后配制原料时提高 CaO的加入量， 或降低 MgO的加入 量， 通过计算 Si02与 CaO反应后剩余的 CaO符合步骤 （1 ) 的配比要求； Si02与 CaO反应 的方程式为：
2CaO + Si02=2CaO · Si02
3、根据权利要求 1所述的以铝或铝合金为还原剂以 MgO/CaO摩尔比大于 1的物料 为原料真空还原制取金属镁的方法， 其特征在于所述的还原剂为工业铝粉、 工业铝硅合 金粉或工业铝镁合金粉， 或回收的铝、 铝硅合金或铝镁合金制备的粉料。
4、根据权利要求 1所述的以铝或铝合金为还原剂以 MgO/CaO摩尔比大于 1的物料 为原料真空还原制取金属镁的方法， 其特征在于所述的 MgO/CaO摩尔比大于 1， 其摩 尔比可选择 1.5~18。
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CN102560149B (zh) * 2012-03-08 2014-03-05 东北大学 一种以硅钙合金为还原剂真空炼镁的方法
CN102534254A (zh) * 2012-03-28 2012-07-04 瓮福（集团）有限责任公司 一种以高镁磷尾矿为原料制备金属镁的方法
CN102534253A (zh) * 2012-03-28 2012-07-04 瓮福（集团）有限责任公司 利用高镁磷尾矿熔融还原制备金属镁的方法
CN102808089A (zh) * 2012-07-23 2012-12-05 东北大学 一种以氧化镁为原料制备金属镁和镁铝尖晶石的方法
CN113789450A (zh) * 2021-08-27 2021-12-14 中国铝业股份有限公司 一种铝热生产金属镁的制备方法
CN116005007B (zh) * 2023-01-06 2024-10-01 濮阳濮耐高温材料（集团）股份有限公司 一种铝热还原制备金属镁和镁铝尖晶石的方法

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