铅、锑还原造铳熔炼新方法研究
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摘要
在我国铅、锑、铋冶炼生产中，产生大量低浓度二氧化硫烟气，难以制酸，造成严重的环境污染。作者用富含氧化铁的黄铁矿烧渣作固硫剂，提出了一种无二氧化硫排放的铅、锑、铋硫化矿精矿的还原造锍熔炼新方法，对还原造锍熔炼的原理、硫化铅精矿及脆硫锑铅矿精矿的还原造锍熔炼工艺及铁锍的处理进行了较系统的深入研究，得出了有意义的结论。
首次对以氧化铁作固硫剂的还原造锍反应进行了热力学分析，确定硫化铅、脆硫铅锑矿、硫化锑及硫化铋的还原造锍反应是可以自发进行的。根据捷姆金(JIEMUJIN)模型，得出了杂质金属在铁锍及金属之间的分配比例的计算公式：D=r_M~OKP_S_2~(0.5y)/1，按此公式的计算结果与实验情况相符合。另外，测定了1373K及1473K温度下铅在FeS-Na_2S系中溶解度，这对控制铁锍含铅量具有重要意义。
首次用富含氧化铁的黄铁矿烧渣替代纯氧化铁作固硫剂进行铅、锑硫化矿的无二氧化硫一步熔炼---还原造锍熔炼试验，试验包括硫化铅精矿和脆硫锑铅矿精矿的实验室试验和半工业性试验。这对解决迫在眉睫的大量低浓度二氧化硫和黄铁矿烧渣的污染问题以及含金黄铁矿烧渣黄金资源的开发利用具有重要意义。同时大大降低了还原造锍熔炼的成本，使其应用于工业生产成为可能。
在硫化铅精矿的还原造锍熔炼试验研究中，熔炼时间、添加剂及烧渣加入量、熔炼温度等因素对还原造锍熔炼的影响较大。实验室试验表明在最佳条件下的结果为：铅和银的直收率分别＞8％及70％，固硫率≥96％。硫化铅精矿1m~2反射炉矿还原造锍熔炼半工业试验结果说明，在熔炼规模放大1200倍后，铅直收率87.13％，总回收率96.44％，固硫率≥96％和烟气中二氧化硫含量全部达标；另外，粗铅质量好，含铅≥98％，含铜、锌≤0.05％，并在熔炼过程中完成配锑。因此，粗铅可直接电解精炼。但反射炉传热传质效果差，热效率低，生产效率低，不适于还原造锍熔炼。
在脆硫铅锑矿的还原造锍熔炼中，首次采用锑酸钠渣及含砷碱渣作为含钠添加剂，以代替苏打和无水芒硝，不仅可以降低生产成本，而且对粗铅和粗锑在碱性精炼过程中产生的精炼渣的无污染处理具有重要意义。在用苏打和无水硫酸钠作添加剂的小型试验中，铅和锑的直收率可分别达到68.50％和83.26％，银的直收率为70％，金属总回收率＞95％，固硫率≥96％。在锑酸钠渣与脆硫铅锑矿精矿混合熔炼
的小型试验中，铅和锑的直收率分别达到了78.24%和90.43%。在砷
碱渣与脆硫铅锑矿精矿混合熔炼的小型试验中，砷与大量的锑、铅和
铁形成黄渣，造成金属直收率大幅降低。烧渣加入量为理论量的70%
时，金属直收率最高:Sb 6 1 .42%，Pb52.93%O
首次用短回转窑(。1.4、2.0m)作为脆硫铅锑精矿和碱渣、锑酸钠
渣还原造硫熔练半工业试验的设备，与反射炉比较，短回转窑具有热效
率高，熔炼强度大的优点。短回转窑熔炼试验取得了较好结果:熔炼
能力为反射炉的6倍以上，铅和锑的直收率分别)63.50%及88.02%，
固硫率在95%以上。但铅和银在铁毓中分配比例较高，铅约占总铅的
巧%，银为30%，铁梳中的铅和银必须经济有效地回收。
提出了湿氧化法和焙烧制酸法两种处理铁硫的方法。湿法氧化过
程动力学分析表明，铁梳的氧化受反应物通过产物硫膜层的扩散过程
控制。因此，元素硫的转化率最高也只有79.14%。在800℃及2h的
条件下氧化焙烧，铁梳完全氧化成氧化铁和二氧化硫，而铅、锑的挥
发率低，银不挥发，都留于氧化铁渣中，便于返回利用。因此，焙烧制
酸法是有希望用于工业生产的铁毓处理方法。
本文提出和研究开发的铅、锑、锡的还原造梳熔炼新方法处理这
些金属硫化矿精矿时不产生低浓度二氧化硫烟气，同时又能顺便处理
硫酸工业产生的黄铁矿烧渣及铅锑碱性精炼过程产生的锑酸钠渣和
碱渣，这对环境污染的治理以及烧渣中黄金和碱性精炼渣中铅锑的回
收具有重要意义。这种冶炼方法己申请了国家发明专利(申请
号:001 1 3284.9)，并与三家单位开展了共同开发该专利(申请)技术的合
作。
In our country, the low concentration of sulfur dioxide smoke, which produced in the smelting of lead and antimony sulfides concentrates, is hard to make acid, and it caused serious environment pollution. In the thesis, a new smelting process of lead, antimony ,and bismuth sulfides concentrates with free sulfur dioxide- reducing-matting smelting by use of pyrite cinder as a fixed sulfur agent has been proposed. In the process, the matting reactions should occur in strong reducing atmosphere. The principle and technics of this process for smelting lead sulfide and Jamesonite concentrates and the treating ferrous matte has been researched, and some valuable conclusions is obtained.
The thermodynamic calculation of reducing-matting reactions with ferric oxide as a fixed sulfur agent has been done. It is firstly found that the reducing-matting reactions of lead sulfide, antimony sulfide, Jamesonite, and bismuth sulfide are feasible, but is infeasible for zinc sulfide. To be based on JIEMUJIN model the formula for calculating distribution coefficients of impurity elements between metals phase and
ferrous matte phase was got: D = and the calculated results are
met with experimental data. The solubility of lead in the system of FeS-Na2S was determined at temperature of 1373K and 1473K. It is important for controlling content of lead in the ferrous matte.
In the experiments of the new process smelting with lead and antimony sulfide concentrates without sulfur dioxide, pyrite cinder rich in ferric oxide was firstly used for a fixed sulfur agent in stead of purity ferric oxide, and which is important for solving problems on the pollution of low concentration of sulfur dioxide smoke and recovery of gold in the pyrite cinder containing gold and decreases the cost of the process, so that its industrial application becomes feasible.
In the experiment of the reducing-matting smelting of lead sulfide concentrates the influence of the technics conditions such as smelting time and temperature, the addition of pyrite cinder and additive on the reducing-matting smelting is notable. Under the optimum condition of the table experiments, the direct recovery of lead and silver is higher than 88% and 70%, respectively, and the ratio of sulfur fixed is higher than 96%. The pilot test of the new process was conducted in a reverberator furnace with area of 1m2. In the case of the smelting scale being enlarged 1200 factors the new process is also feasible. A good result of the experiment was abtained that the direct and sum recovery of lead is 87.13%and 96.44%,respectively, the ratio of sulfur fixed is more than 96% and the content of sulfur dioxide in dust smoke is lower than the
country standard. The content of copper and zinc in rude lead is lower than 0.05%, so the rude lead can be directly electrolyted for refining. But reverberator furnace has the disadvantage of lower heat efficiency and productivity and it is infeasible for this process.
In the experiments of the reducing-mattig smelting on Jamesonite concentrate, sodium antimonate slag or alkali slag containing arsenic was firstly used as additive instead of soda and sodium sulfate, that is not only decreased the cost of the process, but also has great significance for treating alkali slag produced in alkali refining of rude lead ,rude antimony and their alloy. In the table experiment using soda and sodium sulfate as additive, the direct recovery of lead, antimony ,and silver is 68.50%,83.26%,and70%, respectively, and the sum recovery of metals and the ratio of sulfur fixed is more than 95% and 96%, respectively. In the experiment using sodium antimonite slag as additive, the direct recovery ratio of lead and antimony is 78.24%and 90.43%, respectively.
In the experiment using alkali slag containing arsenic as additive, arsenic reacted with antimony and iron to produce a great amount of slag containing As, Fe , Sb and Pb,thereby, the recovery of metals decreased greatly. In the case of addition pyrite cinder being 70% of the theory amount the most high direct recovery of lead a
首次对以氧化铁作固硫剂的还原造锍反应进行了热力学分析，确定硫化铅、脆硫铅锑矿、硫化锑及硫化铋的还原造锍反应是可以自发进行的。根据捷姆金(JIEMUJIN)模型，得出了杂质金属在铁锍及金属之间的分配比例的计算公式：D=r_M~OKP_S_2~(0.5y)/1，按此公式的计算结果与实验情况相符合。另外，测定了1373K及1473K温度下铅在FeS-Na_2S系中溶解度，这对控制铁锍含铅量具有重要意义。
首次用富含氧化铁的黄铁矿烧渣替代纯氧化铁作固硫剂进行铅、锑硫化矿的无二氧化硫一步熔炼---还原造锍熔炼试验，试验包括硫化铅精矿和脆硫锑铅矿精矿的实验室试验和半工业性试验。这对解决迫在眉睫的大量低浓度二氧化硫和黄铁矿烧渣的污染问题以及含金黄铁矿烧渣黄金资源的开发利用具有重要意义。同时大大降低了还原造锍熔炼的成本，使其应用于工业生产成为可能。
在硫化铅精矿的还原造锍熔炼试验研究中，熔炼时间、添加剂及烧渣加入量、熔炼温度等因素对还原造锍熔炼的影响较大。实验室试验表明在最佳条件下的结果为：铅和银的直收率分别＞8％及70％，固硫率≥96％。硫化铅精矿1m~2反射炉矿还原造锍熔炼半工业试验结果说明，在熔炼规模放大1200倍后，铅直收率87.13％，总回收率96.44％，固硫率≥96％和烟气中二氧化硫含量全部达标；另外，粗铅质量好，含铅≥98％，含铜、锌≤0.05％，并在熔炼过程中完成配锑。因此，粗铅可直接电解精炼。但反射炉传热传质效果差，热效率低，生产效率低，不适于还原造锍熔炼。
在脆硫铅锑矿的还原造锍熔炼中，首次采用锑酸钠渣及含砷碱渣作为含钠添加剂，以代替苏打和无水芒硝，不仅可以降低生产成本，而且对粗铅和粗锑在碱性精炼过程中产生的精炼渣的无污染处理具有重要意义。在用苏打和无水硫酸钠作添加剂的小型试验中，铅和锑的直收率可分别达到68.50％和83.26％，银的直收率为70％，金属总回收率＞95％，固硫率≥96％。在锑酸钠渣与脆硫铅锑矿精矿混合熔炼
的小型试验中，铅和锑的直收率分别达到了78.24%和90.43%。在砷
碱渣与脆硫铅锑矿精矿混合熔炼的小型试验中，砷与大量的锑、铅和
铁形成黄渣，造成金属直收率大幅降低。烧渣加入量为理论量的70%
时，金属直收率最高:Sb 6 1 .42%，Pb52.93%O
首次用短回转窑(。1.4、2.0m)作为脆硫铅锑精矿和碱渣、锑酸钠
渣还原造硫熔练半工业试验的设备，与反射炉比较，短回转窑具有热效
率高，熔炼强度大的优点。短回转窑熔炼试验取得了较好结果:熔炼
能力为反射炉的6倍以上，铅和锑的直收率分别)63.50%及88.02%，
固硫率在95%以上。但铅和银在铁毓中分配比例较高，铅约占总铅的
巧%，银为30%，铁梳中的铅和银必须经济有效地回收。
提出了湿氧化法和焙烧制酸法两种处理铁硫的方法。湿法氧化过
程动力学分析表明，铁梳的氧化受反应物通过产物硫膜层的扩散过程
控制。因此，元素硫的转化率最高也只有79.14%。在800℃及2h的
条件下氧化焙烧，铁梳完全氧化成氧化铁和二氧化硫，而铅、锑的挥
发率低，银不挥发，都留于氧化铁渣中，便于返回利用。因此，焙烧制
酸法是有希望用于工业生产的铁毓处理方法。
本文提出和研究开发的铅、锑、锡的还原造梳熔炼新方法处理这
些金属硫化矿精矿时不产生低浓度二氧化硫烟气，同时又能顺便处理
硫酸工业产生的黄铁矿烧渣及铅锑碱性精炼过程产生的锑酸钠渣和
碱渣，这对环境污染的治理以及烧渣中黄金和碱性精炼渣中铅锑的回
收具有重要意义。这种冶炼方法己申请了国家发明专利(申请
号:001 1 3284.9)，并与三家单位开展了共同开发该专利(申请)技术的合
作。
In our country, the low concentration of sulfur dioxide smoke, which produced in the smelting of lead and antimony sulfides concentrates, is hard to make acid, and it caused serious environment pollution. In the thesis, a new smelting process of lead, antimony ,and bismuth sulfides concentrates with free sulfur dioxide- reducing-matting smelting by use of pyrite cinder as a fixed sulfur agent has been proposed. In the process, the matting reactions should occur in strong reducing atmosphere. The principle and technics of this process for smelting lead sulfide and Jamesonite concentrates and the treating ferrous matte has been researched, and some valuable conclusions is obtained.
The thermodynamic calculation of reducing-matting reactions with ferric oxide as a fixed sulfur agent has been done. It is firstly found that the reducing-matting reactions of lead sulfide, antimony sulfide, Jamesonite, and bismuth sulfide are feasible, but is infeasible for zinc sulfide. To be based on JIEMUJIN model the formula for calculating distribution coefficients of impurity elements between metals phase and
ferrous matte phase was got: D = and the calculated results are
met with experimental data. The solubility of lead in the system of FeS-Na2S was determined at temperature of 1373K and 1473K. It is important for controlling content of lead in the ferrous matte.
In the experiments of the new process smelting with lead and antimony sulfide concentrates without sulfur dioxide, pyrite cinder rich in ferric oxide was firstly used for a fixed sulfur agent in stead of purity ferric oxide, and which is important for solving problems on the pollution of low concentration of sulfur dioxide smoke and recovery of gold in the pyrite cinder containing gold and decreases the cost of the process, so that its industrial application becomes feasible.
In the experiment of the reducing-matting smelting of lead sulfide concentrates the influence of the technics conditions such as smelting time and temperature, the addition of pyrite cinder and additive on the reducing-matting smelting is notable. Under the optimum condition of the table experiments, the direct recovery of lead and silver is higher than 88% and 70%, respectively, and the ratio of sulfur fixed is higher than 96%. The pilot test of the new process was conducted in a reverberator furnace with area of 1m2. In the case of the smelting scale being enlarged 1200 factors the new process is also feasible. A good result of the experiment was abtained that the direct and sum recovery of lead is 87.13%and 96.44%,respectively, the ratio of sulfur fixed is more than 96% and the content of sulfur dioxide in dust smoke is lower than the
country standard. The content of copper and zinc in rude lead is lower than 0.05%, so the rude lead can be directly electrolyted for refining. But reverberator furnace has the disadvantage of lower heat efficiency and productivity and it is infeasible for this process.
In the experiments of the reducing-mattig smelting on Jamesonite concentrate, sodium antimonate slag or alkali slag containing arsenic was firstly used as additive instead of soda and sodium sulfate, that is not only decreased the cost of the process, but also has great significance for treating alkali slag produced in alkali refining of rude lead ,rude antimony and their alloy. In the table experiment using soda and sodium sulfate as additive, the direct recovery of lead, antimony ,and silver is 68.50%,83.26%,and70%, respectively, and the sum recovery of metals and the ratio of sulfur fixed is more than 95% and 96%, respectively. In the experiment using sodium antimonite slag as additive, the direct recovery ratio of lead and antimony is 78.24%and 90.43%, respectively.
In the experiment using alkali slag containing arsenic as additive, arsenic reacted with antimony and iron to produce a great amount of slag containing As, Fe , Sb and Pb,thereby, the recovery of metals decreased greatly. In the case of addition pyrite cinder being 70% of the theory amount the most high direct recovery of lead a
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