以菱镁石为原料真空金属热还原法炼镁实验研究
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摘要
镁作为一种有色金属,具有低密度、高比强度、良好的阻尼减震性、可循环利用和环境友好等优良性能,被称为21世纪“绿色”工程材料,成为继钢铁、铝之后的第三大金属工程材料,其制备主要方法有熔盐电解法和Pidgeon法。Pidgeon法采用白云石为原料,由于投资成本低、技术简单等优势在我国被广泛应用,但同时也带来能耗大、资源浪费严重、对环境有较大污染等弊端。我国辽南菱镁石资源丰富,矿石品位高,本文以我国辽南菱镁石为原料,采用真空热还原法对金属镁冶炼进行了工艺研究。
论文应用热力学基本原理,计算出常压下硅铁还原氧化镁化学反应自由能和临界反应温度,结果表明在还原过程中添加活性CaO,生成产物Ca2Si04可促使临界还原温度由3846K降低到2820K,并避免反应生成Mg2Si04产物,减小还原过程中Mg的损失。还原过程中真空条件对还原温度有着重要的影响,计算结果表明当还原系统真空度为10.13Pa时,以FeSi(Si,75%)作为还原剂还原金属Mg临界反应温度1358K。
论文研究了我国辽南菱镁石的矿物特性与热分解性能,通过实验考察了菱镁石粒径为0.2mm、0.6mm、1.0mm、3.0mm、5.0mm、8.0mm,煅烧温度600-800℃(50℃间隔),煅烧时间30-70min(10min间隔)分解率、烧损率、水化活性度、活性度等工艺参数。确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。采用XRD和SEM技术分析产物,得出活性氧化镁形成机理即在菱镁石煅烧过程中包括碳酸镁大量吸热、亚稳氧化镁晶体结晶和再结晶的氧化镁烧结等三个阶段。论文采用Doyle和Coats-Redfern机理方程对菱镁石非等温热分解过程分析,得出菱镁石非等温分解过程机理符合Avrami Erofeev成核和核生长为控制步骤的A1模型,分解反应活化能E=225.06KJ·mo1-1,指前因子A=1.64×1012s-1,分解动力学方程：da/dt=1.64×1012/5exp(-225060/RT)(1-a),根据分解动力学方程对在不同煅烧温度下菱镁石热分解过程给予了预测。
通过对粒径1.0mm、3.0mm、5.0mm、8.0mm的石灰石在煅烧温度800～1100℃(50℃间隔),煅烧时间40-70min(10min间隔)分解率、灼减量、水化活性度和活性度等工艺参数考察,确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。对煅烧过程中添加少量的CaF2、NaCl试剂展开实验研究,得出分解率、活性度等工艺参数数值,并对CaF2、NaCl作用机理给予讨论。实验得出粒径8.0mm,1100℃煅烧60min分解率98.51%、灼减量43.35%、水化活性度30.81%,活性度84.7%,CaF2、NaCl添加量占总物料的3%～5%为宜。论文对石灰石非等温热分解动力学进行理论分析和实验研究,得出石灰石非等温分解过程机理符合二维相界反应的R2模型。分解反应活化能E=222.38KJ·mo1-1,指前因子A=3.34×109s-1,分解动力学方程da/t=3.34×109/5exp(-222380/RT)(1-a)1/2,根据分解动力学方程对在不同煅烧温度下石灰石热分解过程进行了预测。
论文研究了以菱镁石和石灰石为原料真空还原金属镁的工艺可行性,通过实验分别考察了还原温度、还原时间、硅铁还原剂加入量、制团压力、矿化剂加入量、不同还原剂、石灰石配比对镁还原率和硅利用率的影响,得出在1473K、10.13Pa真空度下还原1h,当CaO/MgO=1.4(mol)时,以75%硅铁作为还原剂,镁的还原率最大达94.42%,对反应产物金属Mg进行EDS分析,纯度98.36%,炉渣中主要为Ca2Si04和Si02,未检测出Mg2SiO4的存在。理论推导出以菱镁石为原料,硅铁还原过程反应机理方程D1三维扩散(Jander方程),表现形式：1-2/3a-(1-a)2/3=2.7×106exp(-313580/RT)t,表观活化能E=313.58KJ/mol,指前因子A=2.7×106s-1。
论文考察了白云石粒径为1.0mm、3.0mm、5.0mm、8.0mm,煅烧温度700-1100℃(50℃间隔),煅烧时间50-80min(10min间隔),烧损率、水化活性度等工艺参数。确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。结果表明粒径3.0mm,1050℃煅烧80min烧损率45.29%、水化活性度32.84%。以煅烧白云石为原料内热法真空下还原金属镁实验研究,分别考察还原温度、还原时间、硅铁还原剂加入量、制团压力、矿化剂加入量、不同还原剂、石灰石配比等对镁还原率和还原剂利用率的影响。实验结果表明1473K、10.13Pa真空度下还原1h,以75%硅铁作为还原剂,制团压力250Mpa,镁的还原率最大达93.70%。
论文通过以菱镁石、白云石为原料真空热还原法对金属镁实验研究对比,得出1200℃还原温度下,还原3h以菱镁石和石灰石为原料Mg的还原率及Si的利用率均高于以白云石为原料的Mg的还原率及Si的利用率。
实验设计了一台小型内电阻加热还原炉进行工业化实验,通过调整电流、电压及还原时间等工艺参数,得出最佳工艺条件,考察了该套装置连续还原工作时的稳定性,实验结果表明内电阻加热还原炉还原金属镁方案可行,在合理加热制度下,生产金属镁电耗9kWh/kg-Mg,Mg收率可达到90%,还原周期小于180min,热效率超过50%。
论文对我国现有炼镁方法Pidgeon法和本实验内电阻加热法进行生命周期评价,以1t镁锭作为功能单位,结果显示Pidgeon法炼镁过程能耗大,能耗1.48×105MJ/t,其中真空冶炼阶段和煅烧阶段能耗较多,分别占能耗总额的80.48%和15.21%。温室效应对环境负荷影响最大,所占比例49.65%。C02,SO2,NOx等废气的排放主要来源于煤的燃烧。内电阻加热法采用直接接触式加热反应物料,减小了热能的损失,提高了能量的利用率。
As a kind of nonferrous metal, magnesium is referred to as the most promising green engineering material. It has such unique properties as light, tough, good heat conductivity, easily processed and recycled and a good recycling characteristics. Magnesium will be the largest engineering materials after iron and steel, aluminum. To extract metallic magnesium, two different technologies are commercially used:Pidgeon method in calcined dolomite and molten-salt electrolysis. An advantage of Pidgeon method is that low investment and simple techniques, so it is widely applied in China, but it still brings energy and resource wasting serious and more environmental pollution, etc. In the South China Liaoning province, there are plenty of magnesite stones and more grade higher. The research on smelting metallic magnesium process use a new method-internal resistance vacuum thermal reduction technology with South China Liaoning province magnesite stones as raw material.
By applying the basic principle of thermodynamics, the Gibbs free energy and critical temperature of deoxidization of MgO with ferrosilicon are calculated. Added active CaO during the whole reduction process can obtain Ca2SiO4, make critical temperature decrease from3846K to2820K, avoid the reaction Mg2SiO4product and decrease the loss of magnesium under latm. Vacuum degree has a significant impact on reduction temperature. The calculation results show critical temperature is1358K when the vacuum degree of the reduction system is10.13Pa.
The magnesite characteristics and thermal analysis properties are studied. By experiments examine the decomposition rate, burning rate, hydration activity degree and active degree of magnesite calcined process parameters under the condition of magnesite particle size range from0.2mm to8.0mm, calcining temperature range from600℃to800℃and time range from30min to70min, the optimal temperature and time of different size magnesite are determined. Formation mechanism of active magnesium oxide, including three stages of magnesium carbonate absorbing a large number heat, metastable magnesium oxide crystallizing and re-crystallization magnesium oxide sintering, is getting by analysis technology such as XRD and SEM, etc. The kinetic parameters and mechanism functions on magnesite non-isothermal decomposition process is obtained by using Coats-Redfern and Doyle equations. Magnesite decomposition process is in line with Avrami-Erofeev nucleation and nuclear growth as the control of steps Al model and kinetic equitation are expressed as da/dt=1.64×1012/5exp(-225060/RT)(1-α), with an apparent activation energy, E=225.06KJ·mol-1frequency factor, A=1.64×1012s-1. Magnesite thermal decomposition process gives a prediction at different calcination temperature on the decomposition kinetic equaition.
The Limestone characteristics and thermal analysis properties are studied. By experiments examining the decomposition rate, burning rate, hydration activity degree and active degree of Limestone calcined process parameters under the condition of Limestone particle size range from0.2mm to8.0mm, calcining temperature range from600℃to800℃and time range from30min to70min, the optimal temperature and time of different size Limestone are determined. Decomposition rate, activity degree process parameters are getting under a condition of additive a small amount of CaF2、NaCl reagent to limestone and the elaborate mechanism of CaF2、NaCl is analyed, too. It derived limestone' decomposition rate was98.51%, loss rate43.35%, hydration activity30.81%, active degree84.7%and CaF2、 NaCl added3%～5%of total materials when particle size is8.0mm and calcined60min under1100℃. Limestone decomposition process is in line with two-dimensional phase boundary reaction R2model and kinetic equitation is expressed as da/dt=3.34×109/5exp(-222380/RT)(1-α)1/2, with an apparent activation energy, E=222.38KJ· mol-1, frequency factor, A=3.34X109s-1. Lime stone thermal decomposition process gives a prediction at different calcination temperature on the decomposition kinetic equation.
Discussion the feasibility on a vacuum process to smelt magnesium with magnesite and limestone as raw material in the paper and investigation factors on the impact of Mg reduction ratio and Si utilization ratio which including reduction temperature and time, FeSi added mount, briquetting pressure, mineralizer added, different reductants, added limestone. The result showed Mg reduction ratio could reach up to94.42%under reduction temperature1473K, vacuum degree10.13Pa, FeSi(Si,75%) as reducing agent, CaO/MgO mole rate1.4,1hour to reduce reaction. Mg product purity is98.36%. Slag mainly include Ca2SiO4和SiO2 which do not detect Mg2SiO4. Reduction process is in line with three-dimensional phase boundary reaction D3model and kinetic equitation are expressed as1-2/3a-(1-a)2/3=2.7×106exp(-313580/RT)t, with an apparent activation energy, E=313.58KJ/mol, frequency factor, A=2.7x106s-1
The dolomite characteristics and thermal analysis properties are studied. By experiments examining burning rate, hydration activity degree of dolomite calcined process parameters under the condition of dolomite particle size range from1.0mm to8.0mm, calcining temperature range from700℃to1100℃and time range from50min to80min, the optimal temperature and time of different size dolomite are determined. Smelting metallic magnesium experimental factors on the impact of Mg reduction ratio and Si utilization ratio which including reduction temperature and time, FeSi added to mount, briquetting pressure, mineralizer added, different reductants, added limestone are investigated under vacuum thermal reduction with dolomite as raw material factors. The result showed the Mg reduction rate could reach up to93.70%under reduction temperature1473K, vacuum degree10.13Pa, FeSi(Si,75%) as reducing agent, CaO/MgO mole rate1.4,1hour to reduce reaction.
Smelting metallic magnesium experiment is carried out with magnesite and limestone as raw material. It obtained that Mg reduction ratio and Si utilization ratio are more when magnesite is selected as raw material than dolomite as raw material.
Some industrialization experiments for the production of magnesium from calcined magnesites and limestones were done on a novel vacuum furnace by using internal heating method. The optimum process parameters are obtained by adjusting the current, voltage and reduction time. The results show that its magnesium yield exceed90%with the working cycle of180min, that its power consumption is below9kWh/kg and thermal efficiency can reach up to50%.
The life cycle assessment method was used to investigate the energy consumption and environmental loading of It magnesium production with internal resistance vacuum thermal reduction technology and Pidgeon technology. As a consequence, the consumption of the abundance energy with Pidgeon magnesium production process is1.48×105MJ/t-Mg ingot and greenhouse effect is the biggest one to the environment loading, accounts for the total amount49.65×. The most energy consuming stage is vacuum refining stage and calcination stage, and it occupies80.48%and15.21%for total energy consuming respectively. CO2， SO2, NOX and other exhaust emissions mainly come from coal combustion. Internal resistance vacuum thermal reduction technology use direct-contact heat reaction mass, reduce the heat loss and improve energy efficiency.
论文应用热力学基本原理,计算出常压下硅铁还原氧化镁化学反应自由能和临界反应温度,结果表明在还原过程中添加活性CaO,生成产物Ca2Si04可促使临界还原温度由3846K降低到2820K,并避免反应生成Mg2Si04产物,减小还原过程中Mg的损失。还原过程中真空条件对还原温度有着重要的影响,计算结果表明当还原系统真空度为10.13Pa时,以FeSi(Si,75%)作为还原剂还原金属Mg临界反应温度1358K。
论文研究了我国辽南菱镁石的矿物特性与热分解性能,通过实验考察了菱镁石粒径为0.2mm、0.6mm、1.0mm、3.0mm、5.0mm、8.0mm,煅烧温度600-800℃(50℃间隔),煅烧时间30-70min(10min间隔)分解率、烧损率、水化活性度、活性度等工艺参数。确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。采用XRD和SEM技术分析产物,得出活性氧化镁形成机理即在菱镁石煅烧过程中包括碳酸镁大量吸热、亚稳氧化镁晶体结晶和再结晶的氧化镁烧结等三个阶段。论文采用Doyle和Coats-Redfern机理方程对菱镁石非等温热分解过程分析,得出菱镁石非等温分解过程机理符合Avrami Erofeev成核和核生长为控制步骤的A1模型,分解反应活化能E=225.06KJ·mo1-1,指前因子A=1.64×1012s-1,分解动力学方程：da/dt=1.64×1012/5exp(-225060/RT)(1-a),根据分解动力学方程对在不同煅烧温度下菱镁石热分解过程给予了预测。
通过对粒径1.0mm、3.0mm、5.0mm、8.0mm的石灰石在煅烧温度800～1100℃(50℃间隔),煅烧时间40-70min(10min间隔)分解率、灼减量、水化活性度和活性度等工艺参数考察,确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。对煅烧过程中添加少量的CaF2、NaCl试剂展开实验研究,得出分解率、活性度等工艺参数数值,并对CaF2、NaCl作用机理给予讨论。实验得出粒径8.0mm,1100℃煅烧60min分解率98.51%、灼减量43.35%、水化活性度30.81%,活性度84.7%,CaF2、NaCl添加量占总物料的3%～5%为宜。论文对石灰石非等温热分解动力学进行理论分析和实验研究,得出石灰石非等温分解过程机理符合二维相界反应的R2模型。分解反应活化能E=222.38KJ·mo1-1,指前因子A=3.34×109s-1,分解动力学方程da/t=3.34×109/5exp(-222380/RT)(1-a)1/2,根据分解动力学方程对在不同煅烧温度下石灰石热分解过程进行了预测。
论文研究了以菱镁石和石灰石为原料真空还原金属镁的工艺可行性,通过实验分别考察了还原温度、还原时间、硅铁还原剂加入量、制团压力、矿化剂加入量、不同还原剂、石灰石配比对镁还原率和硅利用率的影响,得出在1473K、10.13Pa真空度下还原1h,当CaO/MgO=1.4(mol)时,以75%硅铁作为还原剂,镁的还原率最大达94.42%,对反应产物金属Mg进行EDS分析,纯度98.36%,炉渣中主要为Ca2Si04和Si02,未检测出Mg2SiO4的存在。理论推导出以菱镁石为原料,硅铁还原过程反应机理方程D1三维扩散(Jander方程),表现形式：1-2/3a-(1-a)2/3=2.7×106exp(-313580/RT)t,表观活化能E=313.58KJ/mol,指前因子A=2.7×106s-1。
论文考察了白云石粒径为1.0mm、3.0mm、5.0mm、8.0mm,煅烧温度700-1100℃(50℃间隔),煅烧时间50-80min(10min间隔),烧损率、水化活性度等工艺参数。确定了各个不同粒径最佳活性度下煅烧温度与煅烧时间。结果表明粒径3.0mm,1050℃煅烧80min烧损率45.29%、水化活性度32.84%。以煅烧白云石为原料内热法真空下还原金属镁实验研究,分别考察还原温度、还原时间、硅铁还原剂加入量、制团压力、矿化剂加入量、不同还原剂、石灰石配比等对镁还原率和还原剂利用率的影响。实验结果表明1473K、10.13Pa真空度下还原1h,以75%硅铁作为还原剂,制团压力250Mpa,镁的还原率最大达93.70%。
论文通过以菱镁石、白云石为原料真空热还原法对金属镁实验研究对比,得出1200℃还原温度下,还原3h以菱镁石和石灰石为原料Mg的还原率及Si的利用率均高于以白云石为原料的Mg的还原率及Si的利用率。
实验设计了一台小型内电阻加热还原炉进行工业化实验,通过调整电流、电压及还原时间等工艺参数,得出最佳工艺条件,考察了该套装置连续还原工作时的稳定性,实验结果表明内电阻加热还原炉还原金属镁方案可行,在合理加热制度下,生产金属镁电耗9kWh/kg-Mg,Mg收率可达到90%,还原周期小于180min,热效率超过50%。
论文对我国现有炼镁方法Pidgeon法和本实验内电阻加热法进行生命周期评价,以1t镁锭作为功能单位,结果显示Pidgeon法炼镁过程能耗大,能耗1.48×105MJ/t,其中真空冶炼阶段和煅烧阶段能耗较多,分别占能耗总额的80.48%和15.21%。温室效应对环境负荷影响最大,所占比例49.65%。C02,SO2,NOx等废气的排放主要来源于煤的燃烧。内电阻加热法采用直接接触式加热反应物料,减小了热能的损失,提高了能量的利用率。
As a kind of nonferrous metal, magnesium is referred to as the most promising green engineering material. It has such unique properties as light, tough, good heat conductivity, easily processed and recycled and a good recycling characteristics. Magnesium will be the largest engineering materials after iron and steel, aluminum. To extract metallic magnesium, two different technologies are commercially used:Pidgeon method in calcined dolomite and molten-salt electrolysis. An advantage of Pidgeon method is that low investment and simple techniques, so it is widely applied in China, but it still brings energy and resource wasting serious and more environmental pollution, etc. In the South China Liaoning province, there are plenty of magnesite stones and more grade higher. The research on smelting metallic magnesium process use a new method-internal resistance vacuum thermal reduction technology with South China Liaoning province magnesite stones as raw material.
By applying the basic principle of thermodynamics, the Gibbs free energy and critical temperature of deoxidization of MgO with ferrosilicon are calculated. Added active CaO during the whole reduction process can obtain Ca2SiO4, make critical temperature decrease from3846K to2820K, avoid the reaction Mg2SiO4product and decrease the loss of magnesium under latm. Vacuum degree has a significant impact on reduction temperature. The calculation results show critical temperature is1358K when the vacuum degree of the reduction system is10.13Pa.
The magnesite characteristics and thermal analysis properties are studied. By experiments examine the decomposition rate, burning rate, hydration activity degree and active degree of magnesite calcined process parameters under the condition of magnesite particle size range from0.2mm to8.0mm, calcining temperature range from600℃to800℃and time range from30min to70min, the optimal temperature and time of different size magnesite are determined. Formation mechanism of active magnesium oxide, including three stages of magnesium carbonate absorbing a large number heat, metastable magnesium oxide crystallizing and re-crystallization magnesium oxide sintering, is getting by analysis technology such as XRD and SEM, etc. The kinetic parameters and mechanism functions on magnesite non-isothermal decomposition process is obtained by using Coats-Redfern and Doyle equations. Magnesite decomposition process is in line with Avrami-Erofeev nucleation and nuclear growth as the control of steps Al model and kinetic equitation are expressed as da/dt=1.64×1012/5exp(-225060/RT)(1-α), with an apparent activation energy, E=225.06KJ·mol-1frequency factor, A=1.64×1012s-1. Magnesite thermal decomposition process gives a prediction at different calcination temperature on the decomposition kinetic equaition.
The Limestone characteristics and thermal analysis properties are studied. By experiments examining the decomposition rate, burning rate, hydration activity degree and active degree of Limestone calcined process parameters under the condition of Limestone particle size range from0.2mm to8.0mm, calcining temperature range from600℃to800℃and time range from30min to70min, the optimal temperature and time of different size Limestone are determined. Decomposition rate, activity degree process parameters are getting under a condition of additive a small amount of CaF2、NaCl reagent to limestone and the elaborate mechanism of CaF2、NaCl is analyed, too. It derived limestone' decomposition rate was98.51%, loss rate43.35%, hydration activity30.81%, active degree84.7%and CaF2、 NaCl added3%～5%of total materials when particle size is8.0mm and calcined60min under1100℃. Limestone decomposition process is in line with two-dimensional phase boundary reaction R2model and kinetic equitation is expressed as da/dt=3.34×109/5exp(-222380/RT)(1-α)1/2, with an apparent activation energy, E=222.38KJ· mol-1, frequency factor, A=3.34X109s-1. Lime stone thermal decomposition process gives a prediction at different calcination temperature on the decomposition kinetic equation.
Discussion the feasibility on a vacuum process to smelt magnesium with magnesite and limestone as raw material in the paper and investigation factors on the impact of Mg reduction ratio and Si utilization ratio which including reduction temperature and time, FeSi added mount, briquetting pressure, mineralizer added, different reductants, added limestone. The result showed Mg reduction ratio could reach up to94.42%under reduction temperature1473K, vacuum degree10.13Pa, FeSi(Si,75%) as reducing agent, CaO/MgO mole rate1.4,1hour to reduce reaction. Mg product purity is98.36%. Slag mainly include Ca2SiO4和SiO2 which do not detect Mg2SiO4. Reduction process is in line with three-dimensional phase boundary reaction D3model and kinetic equitation are expressed as1-2/3a-(1-a)2/3=2.7×106exp(-313580/RT)t, with an apparent activation energy, E=313.58KJ/mol, frequency factor, A=2.7x106s-1
The dolomite characteristics and thermal analysis properties are studied. By experiments examining burning rate, hydration activity degree of dolomite calcined process parameters under the condition of dolomite particle size range from1.0mm to8.0mm, calcining temperature range from700℃to1100℃and time range from50min to80min, the optimal temperature and time of different size dolomite are determined. Smelting metallic magnesium experimental factors on the impact of Mg reduction ratio and Si utilization ratio which including reduction temperature and time, FeSi added to mount, briquetting pressure, mineralizer added, different reductants, added limestone are investigated under vacuum thermal reduction with dolomite as raw material factors. The result showed the Mg reduction rate could reach up to93.70%under reduction temperature1473K, vacuum degree10.13Pa, FeSi(Si,75%) as reducing agent, CaO/MgO mole rate1.4,1hour to reduce reaction.
Smelting metallic magnesium experiment is carried out with magnesite and limestone as raw material. It obtained that Mg reduction ratio and Si utilization ratio are more when magnesite is selected as raw material than dolomite as raw material.
Some industrialization experiments for the production of magnesium from calcined magnesites and limestones were done on a novel vacuum furnace by using internal heating method. The optimum process parameters are obtained by adjusting the current, voltage and reduction time. The results show that its magnesium yield exceed90%with the working cycle of180min, that its power consumption is below9kWh/kg and thermal efficiency can reach up to50%.
The life cycle assessment method was used to investigate the energy consumption and environmental loading of It magnesium production with internal resistance vacuum thermal reduction technology and Pidgeon technology. As a consequence, the consumption of the abundance energy with Pidgeon magnesium production process is1.48×105MJ/t-Mg ingot and greenhouse effect is the biggest one to the environment loading, accounts for the total amount49.65×. The most energy consuming stage is vacuum refining stage and calcination stage, and it occupies80.48%and15.21%for total energy consuming respectively. CO2， SO2, NOX and other exhaust emissions mainly come from coal combustion. Internal resistance vacuum thermal reduction technology use direct-contact heat reaction mass, reduce the heat loss and improve energy efficiency.
引文
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