高硅白云石熔融还原炼镁新技术研究
摘要
中国是全球第一大产镁国，采用的是皮江法热还原炼镁技术。随着科技的不断进步和人类环境的日益恶化，技术落后的皮江法成为了国家限制发展项目。本文结合重庆万盛地区拥有丰富的高硅白云石资源，提出了高生产率、低能耗、低污染的硅浴熔融还原炼镁新技术。对熔融还原炼镁工艺的一些基本现象和规律进行了研究，以期为重庆高硅白云石资源的有效利用提供参考。本文通过试验获得了以下结论：
①该白云石中Ca和Mg元素分别占矿物总质量的21.06%和12.66%，且n(CaO):n(MgO)为1.00。杂质Si含量偏高，含SiO_2为1.6%，且分布不均匀。成分分析表明万盛白云石是典型的高硅白云石。该白云石的主要物相是CaMg(CO_3)_2复盐，并含有少量的SiO_2相。白云石在受热分解过程中，杂质相SiO_2会与分解产生的CaO结合形成Ca_2SiO_4相。万盛白云石受热分解大约从740℃开始，到880℃结束，失重率为46.4%。
②为了获得高质量煅白（煅烧白云石），根据万盛白云石矿的热分析结果进行了白云石煅烧实验，考察了煅烧温度、煅烧时间和白云石粒度三个因素对煅白质量的影响。通过正交实验得出各因素对煅白质量的影响顺序为：煅烧温度、白云石粒度、煅烧时间。经优化的最佳工艺为：煅烧温度为1050℃，白云石粒度范围为6~13mm，煅烧时间为60min。该工艺下白云石的分解率为98.41%，煅白的水化活性为32.07%。是满足炼镁工业生产用的高质量煅白。
③煅白中CaO和MgO均为碱性氧化物，熔点很高。通过往煅白中加入Al_2O_3和SiO_2造渣，能够获得完全熔融的液态。使用热力学软件Factsage模拟了在1600℃下往理想煅白中加入不同量Al_2O_3和SiO_2时炉渣的熔融性，结果表明随着炉渣中Al_2O_3和SiO_2加入量增加，未熔化的固体逐渐减少，直至消失，且CaO较MgO先溶入炉渣中。结合CaO-MgO-Al_2O_3-SiO_2四元相图，通过炉渣熔融性模拟和验证实验得出：加入Al_2O_3和SiO_2造渣时，含有大约55%煅白和45%的造渣剂的炉渣能在1600℃下获得完全熔融的液态。
④对硅浴熔融还原MgO的热力学进行了分析。在不考虑反应物和生成物在液态中活度的理想状态下，反应在常压下所需要的初始温度高达1925℃，当系统压强降低为1×10~4Pa时，反应能够在1550℃进行；而在实际熔融还原过程中，物质的活度对熔融还原影响较大，而且在还原过程中物质的活度也会随着反应的进行而不断变化。为了使后期的熔融还原反应顺利进行，可以采用更低的系统压力。
⑤在真空下进行了硅浴熔融还原MgO实验，考察了渣系成分、CaF_2添加量、反应温度、反应时间和75%硅铁合金添加量对渣中MgO还原率的影响。渣系成分对MgO的还原影响很大，渣中SiO_2量较多的情况下，会增大渣中SiO_2的活性，抑制反应的进行。增大造渣剂中Al_2O_3/SiO_2比值，渣中MgO的还原率提高显著，实验获得的较为理想的炉渣成分为：55%CaO·MgO-35%Al_2O_3-10%SiO_2。对该成分炉渣进行了正交实验，结果表明其他四个因素对MgO还原率的影响顺序为：反应温度、还原剂添加量、反应时间、CaF_2添加量。该成分炉渣在反应温度为1600℃，还原剂添加量n(Si)/n(2MgO)为1.2，反应时间为120min，CaF_2添加量为3%的工艺条件下，渣中MgO的还原率高达97.3%。
⑥结合实验数据，对硅浴熔融还原MgO进行了动力学分析。结果表明硅浴熔融还原反应是二级化学反应。提高Al_2O_3/SiO_2比值、反应温度和CaF_2加入量等都能不同程度的提高还原反应速率。在反应温度1550~1600℃间表观反应活化能为586kJ/mol。熔融还原反应由于在高温下进行，界面化学反应迅速，氧化物在炉渣中的传质成为了整个熔融还原过程的限制环节。
⑦通过分别对镁的饱和蒸气压和高温熔融还原形成的蒸气压进行热力学计算发现，在进行MgO熔融还原时，反应的温度越高，所对应的露点温度就越高。反应温度为1600℃时，对应的露点为870℃，高出纯镁的熔点(651℃)将近200℃。该反应温度下形成的镁蒸气在冷凝时绝大部分会先形成液态金属镁。如果冷凝温度控制在651℃时，会有96%的镁蒸气形成液态，剩余的部分则需要继续降温直接冷凝成固态。
⑧自行设计了一台实验室用500g级小型硅钼棒真空炉，加热功率为4kW，在全功率下可以在1h之内使炉膛温度升高到1600℃。与万盛博奥镁业金属有效公司共同研制了一台10kg级可连续加料的试验真空熔融还原炉，加热元件采用高温石墨，加热功率为30kW，最高使用温度为1800℃。
China is the largest primary magnesium producer in the world, and the primarymagnesium mainly produced by Pidgeon process. With the growing advancement ofscience and technology and the continuous deterioration of hunan environment, thetechnological backwardness Pidgeon process has became one of national limiteddevelopment projects in China. Combining with rich high-silica dolomite resources inWansheng of Chongqing, this paper developed a new technology of magnesiumproduction by smelting reduction, which has high productivity, low energy consumptionand low pollution. In order to provide references for effective utilization of high-silicadolomite in Chongqing area, some of the basic phenomena and laws of smeltingreduction in silica bath were studed in this paper and the results are as follows:
①The chemical composition of Ca, Mg and Si in Wansheng dolomite were21.06%,12.66%and1.6%, respectively, which has the n(CaO)/n(MgO)ratio of1.00. Theimpurity of Si was distributed unevenly with higher chemical composition level indolomite. The analysis of chemical composition indicated that Wansheng dolomite wasa typical high-silica dolomite. Detected by XRD, the mian phase of Wansheng dolomitewas CaMg(CO_3)_2, and the impurity phase was SiO_2. When Wansheng dolomite wasdecomposed by heating, the phase of CaMg(CO_3)_2decomposed into two phases of CaOand MgO. Then, thecombination reaction between CaO and SiO_2was occurred and newimpurity phase of Ca_2SiO_4was formed. The decomposition of Wansheng dolomite wasfrom740℃to880℃end with the weight loss rate of46.4%.
②The order of impacts of various process factors on quality of calcined dolomitewas: calcining temperature, dolomite particle seize and calcining time. When thedolomite of particle seize between6and13mm was calcined at1050℃for60min, thecalcined dolomite with high quality was obtained, which the decomposition rate anddegree of activity were98.41%and32.07%, respectively.
③CaO and MgO in calcined dolomite are alkaline earth oxides and have veryhigh melting temperatures. In order to get molten slag under the experimentalconditions, it was required to mix appropriate Al_2O_3and SiO_2with calcined dolomite.Through software simulation, thermodynamic analysis and experimental verification,it’s found that the unmelted solid reduced gradually with the addition amount of Al_2O_3and SiO_2increasing and CaO dissolved in the slag before MgO. It’s could got molten slag which contained about55%calcined dolomite and45%slagging agent at1600℃.
④The smelting reduction was thermodynamically analyzed. Under the idealstate without considering the activity of the reactants and products in the liquid, thestarting temperature of silicothermic reduction of MgO in molten slag achieved1925℃under atmosphere. When the system pressure reduced to1×10~4Pa, the reductionreaction could be conducted in1550℃. In actual smelting reduction process, theactivity of substance had important impact on reduction reaction and could continuouschange as reduction proceeding. It’s could use lower system pressure to assure that thelatter stage of smelting reduction could be carried out smoothly.
⑤The experiments of silicothermic smelting reduction were carried out undervacuum and the influence of various process factors on reduction extent of MgO in slagwere studied. The chemical composition of slag had important impact on smeltingreduction. Under condition of slag containing more SiO_2, the reduction reaction couldbe restrained because of activity of SiO_2increasing. Reduction rate of MgO couldimprove as the ratio of Al_2O_3/SiO_2increasing. By orthogonal experiment, it’s could gotthat the order of impacts of other various process factors on reduction extent of MgOwas: reaction temperature, the addditon amount of75%ferrosilicon alloy, reaction timeand the addition amount of CaF_2.The experimental results showed that the idealcomposition of slag was55%CaO·MgO-35%Al_2O_3-10%SiO_2and reduction extent ofMgO in this slag was achieved up to97.3%under such optional condition of reactiontemperature of1600℃, n(Si)/n(2MgO)ratio of1.2, reduction time of120min and addingCaF_2of3%, reduction extent of MgO was achieved up to97.3%.
⑥The kinetics of silicothermic smelting reduction were studied and the resultsindicated that silicothermic smelting reduction was second order chemical reation andthe reduction extent of MgO inceased by increasing either one of the following factors:the initial mass ratio of Al_2O_3/SiO_2, the addition of CaF_2, the initial molar ratio ofSi/2MgO, and reaction temperature. The overall smelting reduction was controlled bymass transfer in slag with an apparent activation energy586kJ/mol.
⑦In silicothermic smelting reduction, the dew point temperature ofmagnesium vapor increased as reaction temperature increasing. When reduction processwas carried at1600℃, the corresponding dew point temperature of magnesium vaporwas870℃, which higher than magnesium melting point(651℃) nearly200℃.If thecoolling temperature of magnesium vapor was controlled at651℃, magnesium vapor of96%converted into liquid, the other vapor could condensated directly to solid by decearing coolling temperature below651℃.
⑧A500g-calss and a10kg-class furnace for vacuum smelting reduction weredeveloped. The500g-calss laboratory small furnace had4kW power heated by siliconmolybdenum rod and the furnace temperature was increased to1600℃at full power in1h. The10kg-class furnace which had continuous feeding charge had30kW powerheated by graphite heater and could achieved to the maximum temperature of1800℃.
①该白云石中Ca和Mg元素分别占矿物总质量的21.06%和12.66%，且n(CaO):n(MgO)为1.00。杂质Si含量偏高，含SiO_2为1.6%，且分布不均匀。成分分析表明万盛白云石是典型的高硅白云石。该白云石的主要物相是CaMg(CO_3)_2复盐，并含有少量的SiO_2相。白云石在受热分解过程中，杂质相SiO_2会与分解产生的CaO结合形成Ca_2SiO_4相。万盛白云石受热分解大约从740℃开始，到880℃结束，失重率为46.4%。
②为了获得高质量煅白（煅烧白云石），根据万盛白云石矿的热分析结果进行了白云石煅烧实验，考察了煅烧温度、煅烧时间和白云石粒度三个因素对煅白质量的影响。通过正交实验得出各因素对煅白质量的影响顺序为：煅烧温度、白云石粒度、煅烧时间。经优化的最佳工艺为：煅烧温度为1050℃，白云石粒度范围为6~13mm，煅烧时间为60min。该工艺下白云石的分解率为98.41%，煅白的水化活性为32.07%。是满足炼镁工业生产用的高质量煅白。
③煅白中CaO和MgO均为碱性氧化物，熔点很高。通过往煅白中加入Al_2O_3和SiO_2造渣，能够获得完全熔融的液态。使用热力学软件Factsage模拟了在1600℃下往理想煅白中加入不同量Al_2O_3和SiO_2时炉渣的熔融性，结果表明随着炉渣中Al_2O_3和SiO_2加入量增加，未熔化的固体逐渐减少，直至消失，且CaO较MgO先溶入炉渣中。结合CaO-MgO-Al_2O_3-SiO_2四元相图，通过炉渣熔融性模拟和验证实验得出：加入Al_2O_3和SiO_2造渣时，含有大约55%煅白和45%的造渣剂的炉渣能在1600℃下获得完全熔融的液态。
④对硅浴熔融还原MgO的热力学进行了分析。在不考虑反应物和生成物在液态中活度的理想状态下，反应在常压下所需要的初始温度高达1925℃，当系统压强降低为1×10~4Pa时，反应能够在1550℃进行；而在实际熔融还原过程中，物质的活度对熔融还原影响较大，而且在还原过程中物质的活度也会随着反应的进行而不断变化。为了使后期的熔融还原反应顺利进行，可以采用更低的系统压力。
⑤在真空下进行了硅浴熔融还原MgO实验，考察了渣系成分、CaF_2添加量、反应温度、反应时间和75%硅铁合金添加量对渣中MgO还原率的影响。渣系成分对MgO的还原影响很大，渣中SiO_2量较多的情况下，会增大渣中SiO_2的活性，抑制反应的进行。增大造渣剂中Al_2O_3/SiO_2比值，渣中MgO的还原率提高显著，实验获得的较为理想的炉渣成分为：55%CaO·MgO-35%Al_2O_3-10%SiO_2。对该成分炉渣进行了正交实验，结果表明其他四个因素对MgO还原率的影响顺序为：反应温度、还原剂添加量、反应时间、CaF_2添加量。该成分炉渣在反应温度为1600℃，还原剂添加量n(Si)/n(2MgO)为1.2，反应时间为120min，CaF_2添加量为3%的工艺条件下，渣中MgO的还原率高达97.3%。
⑥结合实验数据，对硅浴熔融还原MgO进行了动力学分析。结果表明硅浴熔融还原反应是二级化学反应。提高Al_2O_3/SiO_2比值、反应温度和CaF_2加入量等都能不同程度的提高还原反应速率。在反应温度1550~1600℃间表观反应活化能为586kJ/mol。熔融还原反应由于在高温下进行，界面化学反应迅速，氧化物在炉渣中的传质成为了整个熔融还原过程的限制环节。
⑦通过分别对镁的饱和蒸气压和高温熔融还原形成的蒸气压进行热力学计算发现，在进行MgO熔融还原时，反应的温度越高，所对应的露点温度就越高。反应温度为1600℃时，对应的露点为870℃，高出纯镁的熔点(651℃)将近200℃。该反应温度下形成的镁蒸气在冷凝时绝大部分会先形成液态金属镁。如果冷凝温度控制在651℃时，会有96%的镁蒸气形成液态，剩余的部分则需要继续降温直接冷凝成固态。
⑧自行设计了一台实验室用500g级小型硅钼棒真空炉，加热功率为4kW，在全功率下可以在1h之内使炉膛温度升高到1600℃。与万盛博奥镁业金属有效公司共同研制了一台10kg级可连续加料的试验真空熔融还原炉，加热元件采用高温石墨，加热功率为30kW，最高使用温度为1800℃。
China is the largest primary magnesium producer in the world, and the primarymagnesium mainly produced by Pidgeon process. With the growing advancement ofscience and technology and the continuous deterioration of hunan environment, thetechnological backwardness Pidgeon process has became one of national limiteddevelopment projects in China. Combining with rich high-silica dolomite resources inWansheng of Chongqing, this paper developed a new technology of magnesiumproduction by smelting reduction, which has high productivity, low energy consumptionand low pollution. In order to provide references for effective utilization of high-silicadolomite in Chongqing area, some of the basic phenomena and laws of smeltingreduction in silica bath were studed in this paper and the results are as follows:
①The chemical composition of Ca, Mg and Si in Wansheng dolomite were21.06%,12.66%and1.6%, respectively, which has the n(CaO)/n(MgO)ratio of1.00. Theimpurity of Si was distributed unevenly with higher chemical composition level indolomite. The analysis of chemical composition indicated that Wansheng dolomite wasa typical high-silica dolomite. Detected by XRD, the mian phase of Wansheng dolomitewas CaMg(CO_3)_2, and the impurity phase was SiO_2. When Wansheng dolomite wasdecomposed by heating, the phase of CaMg(CO_3)_2decomposed into two phases of CaOand MgO. Then, thecombination reaction between CaO and SiO_2was occurred and newimpurity phase of Ca_2SiO_4was formed. The decomposition of Wansheng dolomite wasfrom740℃to880℃end with the weight loss rate of46.4%.
②The order of impacts of various process factors on quality of calcined dolomitewas: calcining temperature, dolomite particle seize and calcining time. When thedolomite of particle seize between6and13mm was calcined at1050℃for60min, thecalcined dolomite with high quality was obtained, which the decomposition rate anddegree of activity were98.41%and32.07%, respectively.
③CaO and MgO in calcined dolomite are alkaline earth oxides and have veryhigh melting temperatures. In order to get molten slag under the experimentalconditions, it was required to mix appropriate Al_2O_3and SiO_2with calcined dolomite.Through software simulation, thermodynamic analysis and experimental verification,it’s found that the unmelted solid reduced gradually with the addition amount of Al_2O_3and SiO_2increasing and CaO dissolved in the slag before MgO. It’s could got molten slag which contained about55%calcined dolomite and45%slagging agent at1600℃.
④The smelting reduction was thermodynamically analyzed. Under the idealstate without considering the activity of the reactants and products in the liquid, thestarting temperature of silicothermic reduction of MgO in molten slag achieved1925℃under atmosphere. When the system pressure reduced to1×10~4Pa, the reductionreaction could be conducted in1550℃. In actual smelting reduction process, theactivity of substance had important impact on reduction reaction and could continuouschange as reduction proceeding. It’s could use lower system pressure to assure that thelatter stage of smelting reduction could be carried out smoothly.
⑤The experiments of silicothermic smelting reduction were carried out undervacuum and the influence of various process factors on reduction extent of MgO in slagwere studied. The chemical composition of slag had important impact on smeltingreduction. Under condition of slag containing more SiO_2, the reduction reaction couldbe restrained because of activity of SiO_2increasing. Reduction rate of MgO couldimprove as the ratio of Al_2O_3/SiO_2increasing. By orthogonal experiment, it’s could gotthat the order of impacts of other various process factors on reduction extent of MgOwas: reaction temperature, the addditon amount of75%ferrosilicon alloy, reaction timeand the addition amount of CaF_2.The experimental results showed that the idealcomposition of slag was55%CaO·MgO-35%Al_2O_3-10%SiO_2and reduction extent ofMgO in this slag was achieved up to97.3%under such optional condition of reactiontemperature of1600℃, n(Si)/n(2MgO)ratio of1.2, reduction time of120min and addingCaF_2of3%, reduction extent of MgO was achieved up to97.3%.
⑥The kinetics of silicothermic smelting reduction were studied and the resultsindicated that silicothermic smelting reduction was second order chemical reation andthe reduction extent of MgO inceased by increasing either one of the following factors:the initial mass ratio of Al_2O_3/SiO_2, the addition of CaF_2, the initial molar ratio ofSi/2MgO, and reaction temperature. The overall smelting reduction was controlled bymass transfer in slag with an apparent activation energy586kJ/mol.
⑦In silicothermic smelting reduction, the dew point temperature ofmagnesium vapor increased as reaction temperature increasing. When reduction processwas carried at1600℃, the corresponding dew point temperature of magnesium vaporwas870℃, which higher than magnesium melting point(651℃) nearly200℃.If thecoolling temperature of magnesium vapor was controlled at651℃, magnesium vapor of96%converted into liquid, the other vapor could condensated directly to solid by decearing coolling temperature below651℃.
⑧A500g-calss and a10kg-class furnace for vacuum smelting reduction weredeveloped. The500g-calss laboratory small furnace had4kW power heated by siliconmolybdenum rod and the furnace temperature was increased to1600℃at full power in1h. The10kg-class furnace which had continuous feeding charge had30kW powerheated by graphite heater and could achieved to the maximum temperature of1800℃.
引文
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