高铁硫化锌精矿和多金属复杂硫化矿加压浸出工艺及理论研究
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摘要
本论文对高铁硫化锌精矿及多金属复杂硫化矿的加压浸出工艺和理论进行了系统研究。
文中首先总结了我国有色冶金工业的成就与存在问题，介绍了加压湿法冶金的历史沿革，特别强调了加压湿法冶金的优越性及其在有色冶金中的重要作用。介绍了国内外加压湿法冶金的进展，叙述了国内外针对高铁硫化锌精矿及多金属复杂硫化矿采用加压浸出技术的研究成果和工业应用状况，从而明确提出了本论文的研究意义及主要研究内容。
论文研究内容主要分为两大部分：高铁硫化锌精矿氧压浸出的基础理论研究和多金属复杂硫化矿氧压浸出工艺研究。
在高铁硫化锌精矿氧压浸出基础理论研究部分：(1)分析了高铁硫化锌精矿氧压浸出过程的热力学规律，并绘制了298K下的(Zn_(0.75)Fe_(0.25)S—H_2O系φ-pH图，从热力学上说明了氧压浸出用于处理高铁硫化锌精矿的优越性；分析了氧压浸出时H_2S的生成并结合试验中所发现的现象阐明了H_2S生成对钛质釜体的腐蚀作用，提出了腐蚀机理，在此基础上提出了一条钛质加压釜安全操作的原则；计算了硫化锌精矿加压浸出的热平衡，计算结果表明，反应热不足以平衡物料升温到温度(150℃)所需的热量，需要从外部补充热量，提出了一个返回浸出的废电解液需要达到的预热温度的方法。(2)从工艺角度研究了矿样粒度、搅拌速度、温度、氧分压、酸度、时间、添加剂、精矿中铁含量和液固比等因素对锌、铁浸出率的影响。结果表明：温度、浸出时间、酸度对浸出影响最为显著。试验获得浸出合理的工艺条件为：矿样粒度-320目、温度140～150℃、总压力1.2～1.4MPa(即氧分压0.9～1.1 MPa)、始酸浓度H_2SO_4 150～170g／L、液固比5～6∶1、浸出时间2～2.5h、搅拌速度600～650r／min、添加剂用量为矿量的0.8～1.0％。在该给予条件下浸出，锌浸出率＞97％，铜浸出率＞90％，铁浸出率在30～35％之间，硫转化率在70～85％之间。(3)在确定的条件下，进行了高铁硫化锌精矿氧压浸出过程动力学研究，发展了原有的液-固反应“收缩核动力学模型”，使其能适用于一种固相物与多种水溶物种的反应，建立了高铁硫化锌精矿氧压浸出过程的动力学数学模型，并就浸出过程的反应机理进行了探讨分析，对硫化锌精矿加压浸出时铁的作用作出了解释。高铁硫化锌精矿氧压浸出过程动力学研究是本部分的重点研究内容，研究结果表明：高铁硫化锌精矿浸出过程中，对于Zn而言，浸出过程由表面化学反应所控制，遵循“未反应核减缩型”的表面化学反应控制的动力学规律，其反应活化能为55.04kJ／mol，酸度对Zn浸出反应的表观反应级数为-0.3182；对于Fe而言，浸出过程在浸出初期浸出速率受表面化学反应控制，遵循“未反应核减缩型”表面化学反应控制的动力学规律，其化学反应活化能为26.63 kJ／mol。
建立高铁硫化锌精矿氧压浸出Zn浸出率动力学数学模型为：
α％=100×{1-[1-exp(2.1704-6606.005×1／T+0.7791nP-0.3121n[C]+142.425[Fe]+27.941[Fe~(2+)])t／r_0]~3}
在多金属复杂硫化矿氧压浸出工艺研究部分：(1)从理论上分析了多金属复杂硫化矿加压浸出的热力学规律和各种硫化物相对稳定的程度及其溶解顺序。(2)从工艺生产的角度研究了矿样粒度、搅拌速度、温度、氧分压、酸度、时间、添加剂和液固比等因素对多金属复杂硫化矿精矿中各种金属浸出率的影响。试验获得合理的浸出工艺条件为：矿样粒度-320目、温度145～150℃、总压力1.5MPa(即氧分压1.1 MPa)、始酸浓度H_2SO_4 150g／L、液固比8∶1、浸出时间2h、搅拌速度600～650r／min、添加剂用量为矿量的0.5～1.0％。在该条件下浸出，多金属复杂硫化矿精矿中Zn浸出率在99％以上，Cu浸出率在91％以上，浸出渣中含Cu＜0.5％，Fe则95％以上进入溶液，金属Pb、金属Ag则98％以上进入浸出渣中，单质硫转化率为70％左右。(3)对低品位多金属复杂混合精矿和多金属复杂硫化矿(原矿)进行了加压浸出研究，从而也确定了该两种矿物的合理浸出工艺条件。(4)进行了多金属复杂硫化矿综合利用回收有价金属的新工艺流程研究。氧压浸出液经预中和除铁后与锌冶炼厂现有的中性浸出工序衔接，浸出渣则与熔池熔炼火法炼铅工序衔接，从而实现多金属复杂硫化矿中Cu、Zn、Pb、Ag、In、Cd、S等的综合回收利用。这一工艺路线比多金属复杂硫化矿分选分冶工艺有选冶总回收率高，投资省，对环境污染小等优越性，查新表明，该工艺路线有新颖性。
In this dissertation the technology and fundamentals of pressure leaching of high iron-zinc sulphide concentrate and polymetallic sulphide ore are studied systematically.
The achievements and existing problems of non-ferrous metallurgical industry in our country are summarized and historical evolution of pressure hydrometallurgy is presented with an emphasis on its advantages and important role in non-ferrous metallurgy. The advances in pressure hydrometallurgy and the research achievements and industrial application status of pressure leaching of high iron-zinc sulphide concentrate and polymetallic sulphide ore at home and abroad are briefed, thereby significance and main contents of this research are put forward explicitly.
This dissertation can be divided up into two parts: investigation into the fundamentals of oxygen pressure leaching of high iron- zinc sulphide concentrate and research on the technology of oxygen pressure leaching of polymetallic sulphide ore.
In the first part, (1)the thermodynamic laws of oxygen pressure leaching of high iron-zinc sulphide concentrate are analysed, theφ-pH diagram of (Zn_(0.75)Fe_(0.25) )S-H_2O system at 298K is constructed, and the superiority of oxygen pressure leaching of high iron-zinc sulphide concentrate is shown from the standpoint of the thermodynamics. The formation of H_2S in the oxygen pressure leaching process is also analysed, the chemical attack of H_2S on titanium-base autoclave is observed and the corrosion mechanism is proposed, and the safe working rules are recommended. And the heat balance of pressure leaching of zinc sulphide concentrate is calculated. The results indicate that reactive heat quantity is not balanced with heat quantity for heating up the slurry to 150°C and require supply exteriorly. The method of preheating temperature of reture spent electrolyte for leaching is proposed. (2)the effects of particle size, agitation rate, temperature, oxygen partial pressure, initial acid concentration, leaching time, additive, iron content in the concentrate and liquid-to-solid ratio on the leaching rates of zinc ,copper and iron are examined from the technological angle. The results show that the effects of temperature, leaching time and acidity are predominant. The reasonable technological conditions obtained by experiment are: the particle size of the sample is -320 mesh, the temperature 140℃to 150℃, the leaching time 2 hours to 2.5 hours, the initial acid concentration 150g/L to 170g/L, the overall pressure 1.2MPa to 1.4MPa, or the oxygen partial pressure 0.9MPa to 1.1Mpa, the liquid-to-solid ratio 5:1 to 6:1, the agitation rate 600r/min to 650 r/min, and the amount of additive 0.8% to 1.0% of the sample amount. Under these experiment conditions, the leaching rate of zinc is greater than 97%, the leaching rate of copper greater than 90%, the leaching rate of iron 30% to 35%, and the output rate of sulphur is 70% to 85%. (3)Under the determined kinetic conditions, the kinetics of oxygen pressure leaching of high iron-zinc sulphide concentrate is studied, the original "kinetic model of shrinking core" for liquid-solid reaction is developed andapplied to the reaction of a solid species with two or more water-soluble species, a mathematical model for this leaching process is obtained, and the reaction mechanism of this leaching process is discussed and analysed. The role of iron in the process of pressure leaching of zinc sulphide concentrate is explained. The kinetic study of oxygen pressure leaching of high iron-zinc sulphide concentrate is emphasis of this part, and the results show that as to zinc the leaching process is controlled by the surface chemical reaction and follows the kinetic law of "shrinking of unreacted core", the reaction activation energy is 55.04kJ/mol, the apparent reaction order with respect to the initial acid concentration is -0.3182; and as to iron, at the initial stage the leaching process is controlled by the chemical reactions and follows the surface chemical reaction-controlled kinetic law of "shrinking of unreacted core", and the reaction activation energy is 26.63kJ/mol.
The kinetic mathematical model for leaching process is :α%=100×{1-[1-exp(2.1704-6606.005×1/T+0.779lnP-0.312ln[C] + 142.425[Fe]+27.941[Fe~(2+)])t/r_0]~3}
In the second part, (l)the thermodynamic laws of oxygen pressure leaching of polymetallic sulphide ore, and the relative stability and dissolution order of various sulphides are analysed theoretically. (2)The effects of particle size, agitation rate, temperature, oxygen partial pressure, initial acid concentration, leaching time, additive, and liquid-to-solid ratio on the leaching rates of various metals in the samples are examined from the technological angle. The reasonable technological conditions obtained by experiment are: the particle size of the sample is -320 mesh, the temperature 145℃to 150℃, the overall pressure 1.5MPa, or the oxygen partial pressure 1.1MPa, the initial acid concentration 150g/L, the liquid-to-solid ratio 8:1, the leaching time 2 hours, the agitation rate 600r/min to 650 r/min, and the amount of additive 0.5% to 1.0% of the sample amount. Under these experiment conditions, the leaching rate of zinc is greater than 99%, the leaching rate of copper greater than 91%(the Cu content in the residue is less than 0.5%), the leaching rate of iron greater than 95%, more than 98% of lead and silver are left in the residue, and the output rate of sulphur is about 70%. (3)Reserch on oxygen pressure leaching of low-grade mixed polymetallic sulphide concentrate and polymetallic run-of-mine sulphide ore is conducted, and the reasonable technological conditions are determined. (4)A new technological process of comprehensive utilization of polymetallic sulphide ore and concentrate and recovery of valuable metals is suggested. The leaching liquor is pre-neutralized to precipitate iron and then sent to the neutral leaching section in an existing zinc production plant. The residue is sent to the lead bath smelting section. Thus Zn, Cu, Pb, Ag, In, Cd, and S in the polymetallic sulphide ore can be recovered comprehensively. By comparison with traditional process selective of flotation followed by separate metallurgical treatments, the advantages of the new process are as follows: the overall recovery is higher, the capital costs are lower, and the levels of environmental pollution are abated. The results of up-to-date back-check of literature indicate that the new process is novel one.
文中首先总结了我国有色冶金工业的成就与存在问题，介绍了加压湿法冶金的历史沿革，特别强调了加压湿法冶金的优越性及其在有色冶金中的重要作用。介绍了国内外加压湿法冶金的进展，叙述了国内外针对高铁硫化锌精矿及多金属复杂硫化矿采用加压浸出技术的研究成果和工业应用状况，从而明确提出了本论文的研究意义及主要研究内容。
论文研究内容主要分为两大部分：高铁硫化锌精矿氧压浸出的基础理论研究和多金属复杂硫化矿氧压浸出工艺研究。
在高铁硫化锌精矿氧压浸出基础理论研究部分：(1)分析了高铁硫化锌精矿氧压浸出过程的热力学规律，并绘制了298K下的(Zn_(0.75)Fe_(0.25)S—H_2O系φ-pH图，从热力学上说明了氧压浸出用于处理高铁硫化锌精矿的优越性；分析了氧压浸出时H_2S的生成并结合试验中所发现的现象阐明了H_2S生成对钛质釜体的腐蚀作用，提出了腐蚀机理，在此基础上提出了一条钛质加压釜安全操作的原则；计算了硫化锌精矿加压浸出的热平衡，计算结果表明，反应热不足以平衡物料升温到温度(150℃)所需的热量，需要从外部补充热量，提出了一个返回浸出的废电解液需要达到的预热温度的方法。(2)从工艺角度研究了矿样粒度、搅拌速度、温度、氧分压、酸度、时间、添加剂、精矿中铁含量和液固比等因素对锌、铁浸出率的影响。结果表明：温度、浸出时间、酸度对浸出影响最为显著。试验获得浸出合理的工艺条件为：矿样粒度-320目、温度140～150℃、总压力1.2～1.4MPa(即氧分压0.9～1.1 MPa)、始酸浓度H_2SO_4 150～170g／L、液固比5～6∶1、浸出时间2～2.5h、搅拌速度600～650r／min、添加剂用量为矿量的0.8～1.0％。在该给予条件下浸出，锌浸出率＞97％，铜浸出率＞90％，铁浸出率在30～35％之间，硫转化率在70～85％之间。(3)在确定的条件下，进行了高铁硫化锌精矿氧压浸出过程动力学研究，发展了原有的液-固反应“收缩核动力学模型”，使其能适用于一种固相物与多种水溶物种的反应，建立了高铁硫化锌精矿氧压浸出过程的动力学数学模型，并就浸出过程的反应机理进行了探讨分析，对硫化锌精矿加压浸出时铁的作用作出了解释。高铁硫化锌精矿氧压浸出过程动力学研究是本部分的重点研究内容，研究结果表明：高铁硫化锌精矿浸出过程中，对于Zn而言，浸出过程由表面化学反应所控制，遵循“未反应核减缩型”的表面化学反应控制的动力学规律，其反应活化能为55.04kJ／mol，酸度对Zn浸出反应的表观反应级数为-0.3182；对于Fe而言，浸出过程在浸出初期浸出速率受表面化学反应控制，遵循“未反应核减缩型”表面化学反应控制的动力学规律，其化学反应活化能为26.63 kJ／mol。
建立高铁硫化锌精矿氧压浸出Zn浸出率动力学数学模型为：
α％=100×{1-[1-exp(2.1704-6606.005×1／T+0.7791nP-0.3121n[C]+142.425[Fe]+27.941[Fe~(2+)])t／r_0]~3}
在多金属复杂硫化矿氧压浸出工艺研究部分：(1)从理论上分析了多金属复杂硫化矿加压浸出的热力学规律和各种硫化物相对稳定的程度及其溶解顺序。(2)从工艺生产的角度研究了矿样粒度、搅拌速度、温度、氧分压、酸度、时间、添加剂和液固比等因素对多金属复杂硫化矿精矿中各种金属浸出率的影响。试验获得合理的浸出工艺条件为：矿样粒度-320目、温度145～150℃、总压力1.5MPa(即氧分压1.1 MPa)、始酸浓度H_2SO_4 150g／L、液固比8∶1、浸出时间2h、搅拌速度600～650r／min、添加剂用量为矿量的0.5～1.0％。在该条件下浸出，多金属复杂硫化矿精矿中Zn浸出率在99％以上，Cu浸出率在91％以上，浸出渣中含Cu＜0.5％，Fe则95％以上进入溶液，金属Pb、金属Ag则98％以上进入浸出渣中，单质硫转化率为70％左右。(3)对低品位多金属复杂混合精矿和多金属复杂硫化矿(原矿)进行了加压浸出研究，从而也确定了该两种矿物的合理浸出工艺条件。(4)进行了多金属复杂硫化矿综合利用回收有价金属的新工艺流程研究。氧压浸出液经预中和除铁后与锌冶炼厂现有的中性浸出工序衔接，浸出渣则与熔池熔炼火法炼铅工序衔接，从而实现多金属复杂硫化矿中Cu、Zn、Pb、Ag、In、Cd、S等的综合回收利用。这一工艺路线比多金属复杂硫化矿分选分冶工艺有选冶总回收率高，投资省，对环境污染小等优越性，查新表明，该工艺路线有新颖性。
In this dissertation the technology and fundamentals of pressure leaching of high iron-zinc sulphide concentrate and polymetallic sulphide ore are studied systematically.
The achievements and existing problems of non-ferrous metallurgical industry in our country are summarized and historical evolution of pressure hydrometallurgy is presented with an emphasis on its advantages and important role in non-ferrous metallurgy. The advances in pressure hydrometallurgy and the research achievements and industrial application status of pressure leaching of high iron-zinc sulphide concentrate and polymetallic sulphide ore at home and abroad are briefed, thereby significance and main contents of this research are put forward explicitly.
This dissertation can be divided up into two parts: investigation into the fundamentals of oxygen pressure leaching of high iron- zinc sulphide concentrate and research on the technology of oxygen pressure leaching of polymetallic sulphide ore.
In the first part, (1)the thermodynamic laws of oxygen pressure leaching of high iron-zinc sulphide concentrate are analysed, theφ-pH diagram of (Zn_(0.75)Fe_(0.25) )S-H_2O system at 298K is constructed, and the superiority of oxygen pressure leaching of high iron-zinc sulphide concentrate is shown from the standpoint of the thermodynamics. The formation of H_2S in the oxygen pressure leaching process is also analysed, the chemical attack of H_2S on titanium-base autoclave is observed and the corrosion mechanism is proposed, and the safe working rules are recommended. And the heat balance of pressure leaching of zinc sulphide concentrate is calculated. The results indicate that reactive heat quantity is not balanced with heat quantity for heating up the slurry to 150°C and require supply exteriorly. The method of preheating temperature of reture spent electrolyte for leaching is proposed. (2)the effects of particle size, agitation rate, temperature, oxygen partial pressure, initial acid concentration, leaching time, additive, iron content in the concentrate and liquid-to-solid ratio on the leaching rates of zinc ,copper and iron are examined from the technological angle. The results show that the effects of temperature, leaching time and acidity are predominant. The reasonable technological conditions obtained by experiment are: the particle size of the sample is -320 mesh, the temperature 140℃to 150℃, the leaching time 2 hours to 2.5 hours, the initial acid concentration 150g/L to 170g/L, the overall pressure 1.2MPa to 1.4MPa, or the oxygen partial pressure 0.9MPa to 1.1Mpa, the liquid-to-solid ratio 5:1 to 6:1, the agitation rate 600r/min to 650 r/min, and the amount of additive 0.8% to 1.0% of the sample amount. Under these experiment conditions, the leaching rate of zinc is greater than 97%, the leaching rate of copper greater than 90%, the leaching rate of iron 30% to 35%, and the output rate of sulphur is 70% to 85%. (3)Under the determined kinetic conditions, the kinetics of oxygen pressure leaching of high iron-zinc sulphide concentrate is studied, the original "kinetic model of shrinking core" for liquid-solid reaction is developed andapplied to the reaction of a solid species with two or more water-soluble species, a mathematical model for this leaching process is obtained, and the reaction mechanism of this leaching process is discussed and analysed. The role of iron in the process of pressure leaching of zinc sulphide concentrate is explained. The kinetic study of oxygen pressure leaching of high iron-zinc sulphide concentrate is emphasis of this part, and the results show that as to zinc the leaching process is controlled by the surface chemical reaction and follows the kinetic law of "shrinking of unreacted core", the reaction activation energy is 55.04kJ/mol, the apparent reaction order with respect to the initial acid concentration is -0.3182; and as to iron, at the initial stage the leaching process is controlled by the chemical reactions and follows the surface chemical reaction-controlled kinetic law of "shrinking of unreacted core", and the reaction activation energy is 26.63kJ/mol.
The kinetic mathematical model for leaching process is :α%=100×{1-[1-exp(2.1704-6606.005×1/T+0.779lnP-0.312ln[C] + 142.425[Fe]+27.941[Fe~(2+)])t/r_0]~3}
In the second part, (l)the thermodynamic laws of oxygen pressure leaching of polymetallic sulphide ore, and the relative stability and dissolution order of various sulphides are analysed theoretically. (2)The effects of particle size, agitation rate, temperature, oxygen partial pressure, initial acid concentration, leaching time, additive, and liquid-to-solid ratio on the leaching rates of various metals in the samples are examined from the technological angle. The reasonable technological conditions obtained by experiment are: the particle size of the sample is -320 mesh, the temperature 145℃to 150℃, the overall pressure 1.5MPa, or the oxygen partial pressure 1.1MPa, the initial acid concentration 150g/L, the liquid-to-solid ratio 8:1, the leaching time 2 hours, the agitation rate 600r/min to 650 r/min, and the amount of additive 0.5% to 1.0% of the sample amount. Under these experiment conditions, the leaching rate of zinc is greater than 99%, the leaching rate of copper greater than 91%(the Cu content in the residue is less than 0.5%), the leaching rate of iron greater than 95%, more than 98% of lead and silver are left in the residue, and the output rate of sulphur is about 70%. (3)Reserch on oxygen pressure leaching of low-grade mixed polymetallic sulphide concentrate and polymetallic run-of-mine sulphide ore is conducted, and the reasonable technological conditions are determined. (4)A new technological process of comprehensive utilization of polymetallic sulphide ore and concentrate and recovery of valuable metals is suggested. The leaching liquor is pre-neutralized to precipitate iron and then sent to the neutral leaching section in an existing zinc production plant. The residue is sent to the lead bath smelting section. Thus Zn, Cu, Pb, Ag, In, Cd, and S in the polymetallic sulphide ore can be recovered comprehensively. By comparison with traditional process selective of flotation followed by separate metallurgical treatments, the advantages of the new process are as follows: the overall recovery is higher, the capital costs are lower, and the levels of environmental pollution are abated. The results of up-to-date back-check of literature indicate that the new process is novel one.
引文
[1] 陈家镛等．湿法冶金手册[M]．北京：冶金工业出版社，2005
[2] 柴成栋 摘译，夏德长 校．硫化锌精矿湿法与火法冶金工艺的发展与比较[J]．E&MJ，1990(5)：52-56
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