锌电积用铅基多孔节能阳极的制备、表征与工程化试验
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摘要
湿法炼锌工业中,高浓度H_2SO_4电解液体系使得Zn电积过程一直采用铅基合金阳极。但铅基合金阳极析氧过电位高(约860mV),增加无用电耗近1000kWh/t-Zn(约占Zn电积总能耗的30%),同时存在抗蠕变性能差以及Pb被腐蚀进入电解液并降低电Zn品质等问题。针对上述问题的Ti基电催化涂层阳极尽管可有效降低阳极过电位,但较短寿命与高昂成本使其难以取代铅基合金阳极。因此,开发新型节能阳极仍是湿法炼Zn领域的重要课题。
在大量文献调研的基础上,作者率先提出铅基多孔节能阳极的概念,通过增大阳极导电面积,降低阳极电流密度,从而在保持Pb-Ag阳极优势的同时,降低阳极过电位,减少阳极腐蚀并提高Zn品质。论文研究开发了铅基多孔材料的反重力渗流铸造设备及工艺,系统评价了Pb-Ag(0.8%)(质量百分数,下同)多孔阳极的电化学性能,深入研究了表观电流密度对Pb-Ag(0.8%)平板阳极电化学行为的影响,开展了Pb-Ag(0.8%)多孔阳极的工程化电解试验;在此基础上,进一步研究了电催化活性金属元素掺杂的铅基多孔节能阳极。论文主要研究结果如下:
(1)设计并开发了Pb基多孔合金的反重力渗流铸造设备与工艺。铅基熔体在可控压力下充型和结晶,可有效避免渗流不足和渗流过度,解决了铅基熔体和填料粒子的润湿性与补缩问题,建立了孔径可控、结构均匀的铅基多孔合金的制备技术,制备了尺寸为250.0mm×160.0mm×30.0mm的Pb-Ag(0.8%)多孔材料。
(2)系统研究了不同孔径Pb-Ag(0.8%)多孔合金阳极的电化学行为,揭示了多孔阳极的电化学行为与特征。结果表明,不同孔径多孔阳极的相对稳定的析氧电位(以下简称析氧电位)、腐蚀速率均明显低于平板阳极,当阳极孔径为1.60～2.00mm时,其阳极析氧电位比Pb-Ag(0.8%)平板阳极降低了100mV左右,相对腐蚀速率减少50%左右,阴极产品含铅量显著降低,且多孔阳极减少了Mn~(2+)的贫化,有利于减少阳极泥的生成,而电流效率与平板阳极相当,均介于91%—92%之间。
(3)以阐明Pb-Ag(0.8%)多孔阳极的电化学行为与特征为目的,系统研究了不同电流密度下Pb基合金阳极电化学行为,揭示了电流密度对Pb-Ag(0.8%)平板阳极析氧电位、腐蚀速率、氧化膜的物相组成与微观结构、电流效率、阳极泥生成量及阴极Zn品质的影响规律。在纯ZnSO_4-H_2SO_4体系中,当电流密度分别由500A/m~2降低到100A/m~2时,其相对稳定的阳极电位(简称稳定电位)由1.835V(相对饱和甘汞电极,以下同)降低到1.742V,腐蚀速率由1.620g/m~2·h降低到0.652g/m~2·h;在ZnSO_4-MnSO4-H_2SO_4体系中,阳极析氧电位与腐蚀速率随电流密度降低的规律不变,100A/m~2和500A/m~2电流密度下的稳定电位则分别为1.704V和1.792V。
(4)Pb-Ag(0.8%)多孔阳极的工程化电解试验取得了良好效果。采用尺寸为200.0mm×100.0mm×6.0mm的Pb-Ag(0.8%)多孔阳极在工业电解条件下进行了为期24天的工程化电解试验。结果表明,与现行Pb-Ag(0.8%)平板阳极比较,多孔阳极析氧过电位降低约100mV,腐蚀率降低80%;使得吨Zn能耗降低78kWh,阳极泥减少80%,阴极锌产品中Pb含量降低60%。
(5)将Pb蓄电池电极中的有害杂质Bi作为合金元素引入锌电积用Pb-Ag(0.8%)阳极。揭示了Bi添加对Pb-Ag(0.8%)阳极析氧电位、腐蚀速率、合金及其氧化膜组织结构的影响规律,确定Bi的最佳添加量为0.8～1.0%,开发出具有电催化活性金属元素掺杂的电催化多孔节能阳极。
The anode of lead-based alloy is always used in industrial production of zinc owing to high concentration of H_2SO_4 in the electrolyte.However,there are several problems on the lead-based anode such as high oxygen evolution overpotential(about 860mV) which can increase the energy consumption about 1000 kWh/t-Zn(about 30%of the total energy consumption),low corrosion resistance and decrease of zinc quality due to lead dissolution in the electrolyte.Although titanium-based electro-catalytic coating anode can effectively reduce the oxygen evolution potential,it still cannot replace the lead-based anode due to its short life and high cost.Therefore,it still is an important subject to develop new energy-saving anode in the zinc hydrometallurgy.
The concept of porous lead-based anode was firstly put forward by the author based on numerous literature investigation.By increasing the anode conductive area to reduce the anodic current density,the porous lead-based anode can reduce the anodic overvoltage,lower the anode corrosion rate and improve the product quality while maintaining the advantages of Pb-Ag alloy anode.In this paper,the equipment and technics of counter-gravity infiltration was developed,the electrochemical properties of porous Pb-Ag(0.8%) anode was evaluated systematically,the effect of current density on the electrochemical behavior of traditional flat anodes was studied thoroughly and a pilot scale electrolysis experiment of porous Pb-Ag(0.8%) was carried out. Based on that,the porous lead-based anode doping metal of electro-catalytic activity was further studied.The main conclusions and results are summarized as follows:
(1) The equipment and technics of counter-gravity infiltration for the fabrication of porous lead-based alloy are designed and developed.Filling and crystallization under controllable pressure can effectively avoid the lack and excess of infiltration and solve the problem of wettability and feeding between the lead-based melt and filler particles.The technics for the preparation of porous lead-based anode with controllable pore size and uniform pore structure is set up and the porous materials of Pb-Ag (0.8%) with dimension of 250.0mm×160.0mm×30.0mm are prepared.
(2) The electrochemical behavior of porous Pb-Ag(0.8%) anode with different pore diameter is studied systematically and the electrochemical behavior and characteristics of porous anode are revealed. Results show that the oxygen evolution overvoltage and corrosion rate of porous anode are obviously lower than that of flat anode.When the pore diameter is 1.60-2.00mm,its anodic potential is 100mV lower than flat anode and its corrosion rate is about 50%of the flat anode.The lead content of cathode Zn is decreased remarkably by using porous anode. The current efficiency for porous anode is almost same as that for flat anode which is 91%-92%while the porous anode is beneficial for reducing anode slime because the phenomenon of Mn~(2+) dilution is less obvious.
(3) In order to illustrate electrochemical behavior and characteristics of porous anode.The electrochemical behavior of lead-based anode is studied systematically under different current densities and the effect of current density on the anodic potential,the corrosion rate,the composition and microstructure of anodic oxidized layer,the current efficiency,the quantity of anode slime and the quality of cathode zinc is analyzed.In electrolyte of pure ZnSO_4-H_2SO_4,when current density is decreased from 500 A/m~2 to 100 A/m~2,the anodic potential(VS SCE) decreases from 1.835V to 1.742V and the corrosion rate decreases from 1.620g/m~2·h to 0.652g/m~2·h.In the electrolyte of ZnSO_4-MnSO_4-H_2SO_4, the anodic potential and corrosion rate also decrease with the decrease of current density,the stabilized anodic potential is 1.704V and 1.792V at the current density of 100 A/m~2 and 500 A/m~2 respectively.
(4) The porous Pb-Ag(0.8%) anode with dimension of 200.0mm×100.0mm×6.0mm is tested in pilot scale experiment for 24 days and the anode is found to perform well in industrial electrolysis conditions.The results show that compared with the flat anode,the anodic potential is decreased about 100mV,the corrosion rate is reduced by 80%,the energy consumption is lowered 78kWh/t-Zn,the quantity of anode slime is reduced by 80%and the lead content of cathode Zn is 60%.
(5) Bi which is harmful for the electrode of lead-acid battery is introduced to Pb-Ag(0.8%) anode of zinc electrowinning and its effect on anodic potential,corrosion rate and the structure and composition of anodic oxidized layer is analyzed.The optimum content of Bi is found to be 0.8-1.0%.The porous lead-based anode doping metal of electro-catalytic activity is developed.
在大量文献调研的基础上,作者率先提出铅基多孔节能阳极的概念,通过增大阳极导电面积,降低阳极电流密度,从而在保持Pb-Ag阳极优势的同时,降低阳极过电位,减少阳极腐蚀并提高Zn品质。论文研究开发了铅基多孔材料的反重力渗流铸造设备及工艺,系统评价了Pb-Ag(0.8%)(质量百分数,下同)多孔阳极的电化学性能,深入研究了表观电流密度对Pb-Ag(0.8%)平板阳极电化学行为的影响,开展了Pb-Ag(0.8%)多孔阳极的工程化电解试验;在此基础上,进一步研究了电催化活性金属元素掺杂的铅基多孔节能阳极。论文主要研究结果如下:
(1)设计并开发了Pb基多孔合金的反重力渗流铸造设备与工艺。铅基熔体在可控压力下充型和结晶,可有效避免渗流不足和渗流过度,解决了铅基熔体和填料粒子的润湿性与补缩问题,建立了孔径可控、结构均匀的铅基多孔合金的制备技术,制备了尺寸为250.0mm×160.0mm×30.0mm的Pb-Ag(0.8%)多孔材料。
(2)系统研究了不同孔径Pb-Ag(0.8%)多孔合金阳极的电化学行为,揭示了多孔阳极的电化学行为与特征。结果表明,不同孔径多孔阳极的相对稳定的析氧电位(以下简称析氧电位)、腐蚀速率均明显低于平板阳极,当阳极孔径为1.60～2.00mm时,其阳极析氧电位比Pb-Ag(0.8%)平板阳极降低了100mV左右,相对腐蚀速率减少50%左右,阴极产品含铅量显著降低,且多孔阳极减少了Mn~(2+)的贫化,有利于减少阳极泥的生成,而电流效率与平板阳极相当,均介于91%—92%之间。
(3)以阐明Pb-Ag(0.8%)多孔阳极的电化学行为与特征为目的,系统研究了不同电流密度下Pb基合金阳极电化学行为,揭示了电流密度对Pb-Ag(0.8%)平板阳极析氧电位、腐蚀速率、氧化膜的物相组成与微观结构、电流效率、阳极泥生成量及阴极Zn品质的影响规律。在纯ZnSO_4-H_2SO_4体系中,当电流密度分别由500A/m~2降低到100A/m~2时,其相对稳定的阳极电位(简称稳定电位)由1.835V(相对饱和甘汞电极,以下同)降低到1.742V,腐蚀速率由1.620g/m~2·h降低到0.652g/m~2·h;在ZnSO_4-MnSO4-H_2SO_4体系中,阳极析氧电位与腐蚀速率随电流密度降低的规律不变,100A/m~2和500A/m~2电流密度下的稳定电位则分别为1.704V和1.792V。
(4)Pb-Ag(0.8%)多孔阳极的工程化电解试验取得了良好效果。采用尺寸为200.0mm×100.0mm×6.0mm的Pb-Ag(0.8%)多孔阳极在工业电解条件下进行了为期24天的工程化电解试验。结果表明,与现行Pb-Ag(0.8%)平板阳极比较,多孔阳极析氧过电位降低约100mV,腐蚀率降低80%;使得吨Zn能耗降低78kWh,阳极泥减少80%,阴极锌产品中Pb含量降低60%。
(5)将Pb蓄电池电极中的有害杂质Bi作为合金元素引入锌电积用Pb-Ag(0.8%)阳极。揭示了Bi添加对Pb-Ag(0.8%)阳极析氧电位、腐蚀速率、合金及其氧化膜组织结构的影响规律,确定Bi的最佳添加量为0.8～1.0%,开发出具有电催化活性金属元素掺杂的电催化多孔节能阳极。
The anode of lead-based alloy is always used in industrial production of zinc owing to high concentration of H_2SO_4 in the electrolyte.However,there are several problems on the lead-based anode such as high oxygen evolution overpotential(about 860mV) which can increase the energy consumption about 1000 kWh/t-Zn(about 30%of the total energy consumption),low corrosion resistance and decrease of zinc quality due to lead dissolution in the electrolyte.Although titanium-based electro-catalytic coating anode can effectively reduce the oxygen evolution potential,it still cannot replace the lead-based anode due to its short life and high cost.Therefore,it still is an important subject to develop new energy-saving anode in the zinc hydrometallurgy.
The concept of porous lead-based anode was firstly put forward by the author based on numerous literature investigation.By increasing the anode conductive area to reduce the anodic current density,the porous lead-based anode can reduce the anodic overvoltage,lower the anode corrosion rate and improve the product quality while maintaining the advantages of Pb-Ag alloy anode.In this paper,the equipment and technics of counter-gravity infiltration was developed,the electrochemical properties of porous Pb-Ag(0.8%) anode was evaluated systematically,the effect of current density on the electrochemical behavior of traditional flat anodes was studied thoroughly and a pilot scale electrolysis experiment of porous Pb-Ag(0.8%) was carried out. Based on that,the porous lead-based anode doping metal of electro-catalytic activity was further studied.The main conclusions and results are summarized as follows:
(1) The equipment and technics of counter-gravity infiltration for the fabrication of porous lead-based alloy are designed and developed.Filling and crystallization under controllable pressure can effectively avoid the lack and excess of infiltration and solve the problem of wettability and feeding between the lead-based melt and filler particles.The technics for the preparation of porous lead-based anode with controllable pore size and uniform pore structure is set up and the porous materials of Pb-Ag (0.8%) with dimension of 250.0mm×160.0mm×30.0mm are prepared.
(2) The electrochemical behavior of porous Pb-Ag(0.8%) anode with different pore diameter is studied systematically and the electrochemical behavior and characteristics of porous anode are revealed. Results show that the oxygen evolution overvoltage and corrosion rate of porous anode are obviously lower than that of flat anode.When the pore diameter is 1.60-2.00mm,its anodic potential is 100mV lower than flat anode and its corrosion rate is about 50%of the flat anode.The lead content of cathode Zn is decreased remarkably by using porous anode. The current efficiency for porous anode is almost same as that for flat anode which is 91%-92%while the porous anode is beneficial for reducing anode slime because the phenomenon of Mn~(2+) dilution is less obvious.
(3) In order to illustrate electrochemical behavior and characteristics of porous anode.The electrochemical behavior of lead-based anode is studied systematically under different current densities and the effect of current density on the anodic potential,the corrosion rate,the composition and microstructure of anodic oxidized layer,the current efficiency,the quantity of anode slime and the quality of cathode zinc is analyzed.In electrolyte of pure ZnSO_4-H_2SO_4,when current density is decreased from 500 A/m~2 to 100 A/m~2,the anodic potential(VS SCE) decreases from 1.835V to 1.742V and the corrosion rate decreases from 1.620g/m~2·h to 0.652g/m~2·h.In the electrolyte of ZnSO_4-MnSO_4-H_2SO_4, the anodic potential and corrosion rate also decrease with the decrease of current density,the stabilized anodic potential is 1.704V and 1.792V at the current density of 100 A/m~2 and 500 A/m~2 respectively.
(4) The porous Pb-Ag(0.8%) anode with dimension of 200.0mm×100.0mm×6.0mm is tested in pilot scale experiment for 24 days and the anode is found to perform well in industrial electrolysis conditions.The results show that compared with the flat anode,the anodic potential is decreased about 100mV,the corrosion rate is reduced by 80%,the energy consumption is lowered 78kWh/t-Zn,the quantity of anode slime is reduced by 80%and the lead content of cathode Zn is 60%.
(5) Bi which is harmful for the electrode of lead-acid battery is introduced to Pb-Ag(0.8%) anode of zinc electrowinning and its effect on anodic potential,corrosion rate and the structure and composition of anodic oxidized layer is analyzed.The optimum content of Bi is found to be 0.8-1.0%.The porous lead-based anode doping metal of electro-catalytic activity is developed.
引文
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