铁帽矿石的锌铁分离与回收研究
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摘要
铁帽是各种金属硫化物矿床在经受比较彻底的氧化、风化淋蚀作用之后,形成以铁、锰等为主的氧化物、次生硫酸盐、各种矾类及粘土质混合物的堆积体,广泛分布于硫化矿床上部或附近。铁帽矿石富含铁及其他有价金属元素,属于特殊类型的氧化矿石,具有重要的潜在开发价值。为开发利用铁帽矿石资源,本论文以广西某大型硫化矿锌矿床铁帽矿石为研究对象,围绕矿石锌铁分离和综合回收问题,借助XRD、SEM.EDS.AAS.ICP等现代仪器分析方法,运用元素地球化学、冶金原理、实验设计、热力学、动力学等理论,研究了铁帽矿石的矿物学性质,通过采用常规选矿、常规碱浸出、机械活化浸出、硫酸浸出、常规焙烧以及深度还原焙烧等工艺和技术处理矿石,系统研究了铁帽矿石的选冶加工特性、产品特征以及过程中因素影响规律和过程机理。研究结果表明：
(1)铁帽矿石的主要矿物来源和性质与大多数氧化矿石不同,是导致铁帽矿石难选难冶的根本原因。所研究铁帽矿石中的铁主要赋存在菱铁矿和褐铁矿两种矿物中,其中菱铁矿为硫化矿床早期形成时沉积原生菱铁矿；褐铁矿为铁帽形成过程中硫化矿床的黄铁矿氧化和风化淋蚀的产物。铁帽中的锌主要赋存在菱铁矿、褐铁矿与菱锌矿三种矿物中,其中,在原生沉积菱铁矿形成过程,锌以类质同象方式进入菱铁矿中；在黄铁矿氧化和风化淋蚀为褐铁矿过程中,褐铁矿吸附拦截迁移中的硫酸锌,导致铁帽中大量的锌以吸附态形式赋存在褐铁矿中。
(2)由于研究铁帽矿石中独立锌矿物少,锌主要以类质同象形式存在于菱铁矿中和以被吸附状态存在于褐铁矿中,因此,采用常规选矿方法处理该铁帽矿石,不仅粗精矿的品位指标与铁帽矿石原矿接近,而且回收率低,证实了该铁帽矿石为难选氧化矿石,物理选矿无法实现锌铁的有效分离。
(3)由于研究铁帽矿石中的锌主要以类质同象形式存在于菱铁矿中和以被吸附状态存在于褐铁矿中,少量锌存在于菱锌矿中,而这三种矿物在碱性溶液的溶解特性不同,菱锌矿易溶,菱铁矿和褐铁矿难溶,因此,碱性浸出的实质是菱锌矿被溶解破坏释放锌,褐铁矿所吸附的锌被解吸进入溶液,菱铁矿不溶解性和褐铁矿中锌解吸的非自发性和非彻底性是导致铁帽矿石常规碱浸出工艺提锌难的根本原因。采用碱性浸出方法处理该铁帽矿石,单次浸出的锌浸出率低,均低于50%,采用多次碱浸和机械活化碱浸可适当提高锌的浸出率,最高达63%。
(4)由于硫酸易于溶解破坏菱锌矿和从褐铁矿中解吸吸附锌,并且在较高浓度和较长作用时间条件下可破坏菱铁矿,因此,采用硫酸浸出比碱性浸出更容易浸出铁帽矿石中的锌,锌浸出率可达到90%以上,但铁也进入溶液,铁浸出率大于50%,将导致后续溶液锌铁分离难度大。
(5)由于研究铁帽矿石中的锌铁紧密复杂共生,在常规焙烧过程中容易生成稳定难溶和无磁性的铁酸锌,因此,采用常规焙烧预处理该铁帽矿石,致使焙烧产品的碱性浸锌或磁选选铁效果均不理想。
(6)由于在高温、强还原气氛中铁矿物容易较彻底地转化为易于磁选回收的金属铁颗粒,而矿石中的锌被转化为低熔点的金属锌,再挥发转化为氧化锌进入气相,因此,深度还原—磁选工艺是处理锌铁以类质同象和吸附关系共存的该类型铁帽矿石最适宜的工艺,可实现锌铁的高效分离和综合回收。采用深度还原预处理该铁帽矿石时,金属化率达到92%以上,锌挥发率达到97%以上,对深度还原产品进行磁选分离,所得铁精矿铁品位与铁回收率均在90%以上
(7)采用响应面法分析浸出试验数据,易于确定各因素的影响主次及交叉作用规律,并获得形式简洁和预测可靠性高的二次回归方程。在碱性浸出中,各因素影响的主次顺序是：浸出时间>浸出剂浓度>浸出温度,浸出时间和浸出剂浓度两因素的交互作用影响明显大于其他两因素组合的交互作用影响。在硫酸浸出中,各因素影响的主次顺序是：硫酸浓度>浸出时间>浸出温度,与硫酸浓度配合的两因素组合交互作用影响大小接近,且明显大于无硫酸浓度参与的其他两因素组合的交互作用影响。
(8)铁帽矿石的浸出过程动力学可以用收缩未反应芯扩散控制模型描述,模型参数与反应条件密切相关,且浸出过程的活化能较低,均小于30kJ／mol。其中,碱性浸出动力学宜采用分段收缩未反应芯扩散控制模型描述,且10～120min时段的活化能低于120～360min时段的活化能。根据模型拟合结果和活化能的分段特征,可以推断在碱性浸出中,菱锌矿溶解反应活化能低,属于快反应过程,而褐铁矿中锌的解吸脱附活化能高,属于慢反应过程,因此,碱性浸出的关键是褐铁矿中锌的解吸脱附。硫酸浸出动力学可采用整段收缩未反应芯扩散控制模型描述,且锌浸出的活化能低于铁浸出的活化能。根据模型拟合结果和活化能的特征,可以推断在硫酸浸出中,菱锌矿与菱铁矿的溶解反应活化能低,属于快反应过程,而褐铁矿中锌的解吸脱附与褐铁矿溶解的活化能高,属于慢反应过程,因此,硫酸浸出过程中锌浸出的关键仍然是褐铁矿中锌的解吸脱附。
总之,本论文结合地质学、选矿学、冶金学等学科理论,通过试验研究和现代分析测试相结合的方法,揭示了铁帽形成机制与其矿石矿物形成和主要元素赋存状态的内在关系,探清了采用常规选冶技术处理该类型矿石存在的问题以及难于选冶分离和回收的原因,指出了该类型矿石矿物分离和综合利用的新方向。论文研究成果具有重要的学术价值,对铁帽矿石的实际开发利用具有重要的指导意义。
Gossan is the name given to a large mass formed by sulfide ore deposits after oxidation and weathering and distributed widely above or near sulfide ore deposits. Its composition is dominated by neoformed minerals bearing iron and manganese, mainly oxidate, secondary sulfate, vitriol and clay. Gossan is a special oxide ore with high contents of iron and other valuable metals and has greatly potential developing value. In order to effectively utilize it, the object of this thesis is the gossan ore derived from zinc sulfate ore deposits in Guangxi Zhuang Autonomous Region of China. It was focused on the problem of separation and recovery of zinc and iron. Mineralogy properties of the gossan ore were studied by means of modern analysis methods such as XRD, SEM, EDS, AAS and ICP and combined with the theories of element geochemistry, metallurgical principle, experiment design, thermodynamics and kinetics. Moreover, the conventional mineral processing methods, the conventional alkaline leaching, mechanical activation leaching, sulfuric acid leaching, the conventional roasting and deep reduction were used to study the feasibility and characteristics, product features, effects of operating factors and process mechanism in mineral processing and metallurgy. The results are shown in followings.
(1) Compared with other oxide ores, the difference of origins and properties of gossan ore minerals lead to the difficulty in mineral processing and metallurgy. In this work, the occurrences of iron and zinc in gossan ores were investigated. The results show that iron occurs predominantly in forms of siderite and limonite, and zinc in forms of siderite, limonite and smithsonite. Siderite belongs to primary deposit born in the early stage of sulfide deposit formation, in which zinc exists in the form of isomorphism. Limonite is the product of pyrite oxidation and weathering in the process of gossan formation, and zinc sulfate is intercepted and absorbed by limonite in the course of migration.
(2) The grade of rough concentrate is near to that of the raw ore and metal recovery is low in the conventional mineral processing. The results indicate that the methods do not realize the effective separation of zinc and iron and the gossan ore is a refractory oxide ores because independent zinc minerals content is low and zinc is the form of isomorphism and adsorption in siderite and limonite, respectively.
(3) In alkaline leaching, the zinc leaching rate of single leaching was less than50%, and that of multi-leaching and mechanical activation leaching could be improved to a certain extent, up to63%maximumly. The results show that zinc in smithsonite could be dissolved in leaching solution, zinc on limonite could be partly desorbed under the action of external forces and zinc in siderite could not be recovered due to its solubility in leaching agent. Therefore, it could be concluded that the alkaline leaching is difficult to recover zinc from the gossan ore for the reasons above mentioned.
(4) In sulfuric acid leaching, the zinc leaching rate is greater than90%because smithsonite is dissolved and zinc in limonite is desorbed easily at high concentration and long leaching time. However, iron is also leached with zinc leaching and the leaching rate of iron is more than50%, which results in the following separation of zinc and iron becomes more difficult.
(5) The results of alkaline leaching and magnetic separation are not ideal because zinc ferrite which is indissoluble and nonmagnetic generated easily for complex associations between zinc and iron in the conventional roasting.
(6) The results show that the process of deep reduction-magnetic separation is most suitable to treat this type of gossan ore which zinc is the form of isomorphism and adsorption. The effective separation and recovery of zinc and iron could be realized because iron minerals could be thoroughly changed into iron particle recovered with magnetic separation easily and zinc could be volatilized into gaseous phase under the atmosphere of strongly reduction and high temperature. The metallization rate, zinc volatile rate, iron grade and iron recovery is greater than92%,97%,90%and90%, respectively.
(7) The influence laws of factors and quadratic regression equation with a simple form and high prediction reliability can be obtained easily by analysis of response surface method. The influence sequence is leaching time> leaching agent concentration> leaching temperature, and the interactive effect of leaching time and leaching agent concentration is more obvious than others in alkaline leaching. The influence sequence is sulfuric acid concentration> leaching time> leaching temperature, and the interactive effect of sulfuric acid concentration and the other factors is more obvious than others without sulfuric acid concentration in sulfuric acid leaching.
(8) The leaching kinetics of gossan ores could be described with unreacted shrinking core diffusion control model, model parameters is closely related with reaction conditions, and activation energy is less than30kJ/mol. Kinetics of alkaline leaching can be described with unreacted shrinking core diffusion control model in two time scales, and the activation energy of10-120minutes was less than that of120-360minutes. According to the simulation results and the characteristics of sectional activation energy, it could be inferred that the activation energy for smithsonite dissolution was low and the leaching process belonged to fast reaction, while the activation energy of zinc desorption in limonite was high and the leaching process belonged to slow reaction, which was the key step for alkaline leaching. Kinetics of sulfuric acid leaching can be described with unreacted shrinking core diffusion control model in whole time scale, and the activation energy of zinc leaching was less than that of iron leaching. According to the simulation results and the characteristics of activation energy, it could be inferred the activation energy for smithsonite and siderite dissolution was low and the leaching process belonged to fast reaction, while the activation energy for zinc desorption and limonite dissolution was high and the leaching process belonged to slow reaction. So zinc desorption in limonite was still the key step in sulfuric acid leaching.
In summary, in this thesis, the relations between gossan formation mechanism and mineral composition were revealed by modern analysis methods combined with the theories involved geology, mineral processing and metallurgy. The main reasons why gossan ores were difficult to be treated with conventional process were found out, and the new process for utilization of this type ores was suggested. The research results in this thesis deserve important academic value and is instructive for gossan resources exploitation and utilization.
(1)铁帽矿石的主要矿物来源和性质与大多数氧化矿石不同,是导致铁帽矿石难选难冶的根本原因。所研究铁帽矿石中的铁主要赋存在菱铁矿和褐铁矿两种矿物中,其中菱铁矿为硫化矿床早期形成时沉积原生菱铁矿；褐铁矿为铁帽形成过程中硫化矿床的黄铁矿氧化和风化淋蚀的产物。铁帽中的锌主要赋存在菱铁矿、褐铁矿与菱锌矿三种矿物中,其中,在原生沉积菱铁矿形成过程,锌以类质同象方式进入菱铁矿中；在黄铁矿氧化和风化淋蚀为褐铁矿过程中,褐铁矿吸附拦截迁移中的硫酸锌,导致铁帽中大量的锌以吸附态形式赋存在褐铁矿中。
(2)由于研究铁帽矿石中独立锌矿物少,锌主要以类质同象形式存在于菱铁矿中和以被吸附状态存在于褐铁矿中,因此,采用常规选矿方法处理该铁帽矿石,不仅粗精矿的品位指标与铁帽矿石原矿接近,而且回收率低,证实了该铁帽矿石为难选氧化矿石,物理选矿无法实现锌铁的有效分离。
(3)由于研究铁帽矿石中的锌主要以类质同象形式存在于菱铁矿中和以被吸附状态存在于褐铁矿中,少量锌存在于菱锌矿中,而这三种矿物在碱性溶液的溶解特性不同,菱锌矿易溶,菱铁矿和褐铁矿难溶,因此,碱性浸出的实质是菱锌矿被溶解破坏释放锌,褐铁矿所吸附的锌被解吸进入溶液,菱铁矿不溶解性和褐铁矿中锌解吸的非自发性和非彻底性是导致铁帽矿石常规碱浸出工艺提锌难的根本原因。采用碱性浸出方法处理该铁帽矿石,单次浸出的锌浸出率低,均低于50%,采用多次碱浸和机械活化碱浸可适当提高锌的浸出率,最高达63%。
(4)由于硫酸易于溶解破坏菱锌矿和从褐铁矿中解吸吸附锌,并且在较高浓度和较长作用时间条件下可破坏菱铁矿,因此,采用硫酸浸出比碱性浸出更容易浸出铁帽矿石中的锌,锌浸出率可达到90%以上,但铁也进入溶液,铁浸出率大于50%,将导致后续溶液锌铁分离难度大。
(5)由于研究铁帽矿石中的锌铁紧密复杂共生,在常规焙烧过程中容易生成稳定难溶和无磁性的铁酸锌,因此,采用常规焙烧预处理该铁帽矿石,致使焙烧产品的碱性浸锌或磁选选铁效果均不理想。
(6)由于在高温、强还原气氛中铁矿物容易较彻底地转化为易于磁选回收的金属铁颗粒,而矿石中的锌被转化为低熔点的金属锌,再挥发转化为氧化锌进入气相,因此,深度还原—磁选工艺是处理锌铁以类质同象和吸附关系共存的该类型铁帽矿石最适宜的工艺,可实现锌铁的高效分离和综合回收。采用深度还原预处理该铁帽矿石时,金属化率达到92%以上,锌挥发率达到97%以上,对深度还原产品进行磁选分离,所得铁精矿铁品位与铁回收率均在90%以上
(7)采用响应面法分析浸出试验数据,易于确定各因素的影响主次及交叉作用规律,并获得形式简洁和预测可靠性高的二次回归方程。在碱性浸出中,各因素影响的主次顺序是：浸出时间>浸出剂浓度>浸出温度,浸出时间和浸出剂浓度两因素的交互作用影响明显大于其他两因素组合的交互作用影响。在硫酸浸出中,各因素影响的主次顺序是：硫酸浓度>浸出时间>浸出温度,与硫酸浓度配合的两因素组合交互作用影响大小接近,且明显大于无硫酸浓度参与的其他两因素组合的交互作用影响。
(8)铁帽矿石的浸出过程动力学可以用收缩未反应芯扩散控制模型描述,模型参数与反应条件密切相关,且浸出过程的活化能较低,均小于30kJ／mol。其中,碱性浸出动力学宜采用分段收缩未反应芯扩散控制模型描述,且10～120min时段的活化能低于120～360min时段的活化能。根据模型拟合结果和活化能的分段特征,可以推断在碱性浸出中,菱锌矿溶解反应活化能低,属于快反应过程,而褐铁矿中锌的解吸脱附活化能高,属于慢反应过程,因此,碱性浸出的关键是褐铁矿中锌的解吸脱附。硫酸浸出动力学可采用整段收缩未反应芯扩散控制模型描述,且锌浸出的活化能低于铁浸出的活化能。根据模型拟合结果和活化能的特征,可以推断在硫酸浸出中,菱锌矿与菱铁矿的溶解反应活化能低,属于快反应过程,而褐铁矿中锌的解吸脱附与褐铁矿溶解的活化能高,属于慢反应过程,因此,硫酸浸出过程中锌浸出的关键仍然是褐铁矿中锌的解吸脱附。
总之,本论文结合地质学、选矿学、冶金学等学科理论,通过试验研究和现代分析测试相结合的方法,揭示了铁帽形成机制与其矿石矿物形成和主要元素赋存状态的内在关系,探清了采用常规选冶技术处理该类型矿石存在的问题以及难于选冶分离和回收的原因,指出了该类型矿石矿物分离和综合利用的新方向。论文研究成果具有重要的学术价值,对铁帽矿石的实际开发利用具有重要的指导意义。
Gossan is the name given to a large mass formed by sulfide ore deposits after oxidation and weathering and distributed widely above or near sulfide ore deposits. Its composition is dominated by neoformed minerals bearing iron and manganese, mainly oxidate, secondary sulfate, vitriol and clay. Gossan is a special oxide ore with high contents of iron and other valuable metals and has greatly potential developing value. In order to effectively utilize it, the object of this thesis is the gossan ore derived from zinc sulfate ore deposits in Guangxi Zhuang Autonomous Region of China. It was focused on the problem of separation and recovery of zinc and iron. Mineralogy properties of the gossan ore were studied by means of modern analysis methods such as XRD, SEM, EDS, AAS and ICP and combined with the theories of element geochemistry, metallurgical principle, experiment design, thermodynamics and kinetics. Moreover, the conventional mineral processing methods, the conventional alkaline leaching, mechanical activation leaching, sulfuric acid leaching, the conventional roasting and deep reduction were used to study the feasibility and characteristics, product features, effects of operating factors and process mechanism in mineral processing and metallurgy. The results are shown in followings.
(1) Compared with other oxide ores, the difference of origins and properties of gossan ore minerals lead to the difficulty in mineral processing and metallurgy. In this work, the occurrences of iron and zinc in gossan ores were investigated. The results show that iron occurs predominantly in forms of siderite and limonite, and zinc in forms of siderite, limonite and smithsonite. Siderite belongs to primary deposit born in the early stage of sulfide deposit formation, in which zinc exists in the form of isomorphism. Limonite is the product of pyrite oxidation and weathering in the process of gossan formation, and zinc sulfate is intercepted and absorbed by limonite in the course of migration.
(2) The grade of rough concentrate is near to that of the raw ore and metal recovery is low in the conventional mineral processing. The results indicate that the methods do not realize the effective separation of zinc and iron and the gossan ore is a refractory oxide ores because independent zinc minerals content is low and zinc is the form of isomorphism and adsorption in siderite and limonite, respectively.
(3) In alkaline leaching, the zinc leaching rate of single leaching was less than50%, and that of multi-leaching and mechanical activation leaching could be improved to a certain extent, up to63%maximumly. The results show that zinc in smithsonite could be dissolved in leaching solution, zinc on limonite could be partly desorbed under the action of external forces and zinc in siderite could not be recovered due to its solubility in leaching agent. Therefore, it could be concluded that the alkaline leaching is difficult to recover zinc from the gossan ore for the reasons above mentioned.
(4) In sulfuric acid leaching, the zinc leaching rate is greater than90%because smithsonite is dissolved and zinc in limonite is desorbed easily at high concentration and long leaching time. However, iron is also leached with zinc leaching and the leaching rate of iron is more than50%, which results in the following separation of zinc and iron becomes more difficult.
(5) The results of alkaline leaching and magnetic separation are not ideal because zinc ferrite which is indissoluble and nonmagnetic generated easily for complex associations between zinc and iron in the conventional roasting.
(6) The results show that the process of deep reduction-magnetic separation is most suitable to treat this type of gossan ore which zinc is the form of isomorphism and adsorption. The effective separation and recovery of zinc and iron could be realized because iron minerals could be thoroughly changed into iron particle recovered with magnetic separation easily and zinc could be volatilized into gaseous phase under the atmosphere of strongly reduction and high temperature. The metallization rate, zinc volatile rate, iron grade and iron recovery is greater than92%,97%,90%and90%, respectively.
(7) The influence laws of factors and quadratic regression equation with a simple form and high prediction reliability can be obtained easily by analysis of response surface method. The influence sequence is leaching time> leaching agent concentration> leaching temperature, and the interactive effect of leaching time and leaching agent concentration is more obvious than others in alkaline leaching. The influence sequence is sulfuric acid concentration> leaching time> leaching temperature, and the interactive effect of sulfuric acid concentration and the other factors is more obvious than others without sulfuric acid concentration in sulfuric acid leaching.
(8) The leaching kinetics of gossan ores could be described with unreacted shrinking core diffusion control model, model parameters is closely related with reaction conditions, and activation energy is less than30kJ/mol. Kinetics of alkaline leaching can be described with unreacted shrinking core diffusion control model in two time scales, and the activation energy of10-120minutes was less than that of120-360minutes. According to the simulation results and the characteristics of sectional activation energy, it could be inferred that the activation energy for smithsonite dissolution was low and the leaching process belonged to fast reaction, while the activation energy of zinc desorption in limonite was high and the leaching process belonged to slow reaction, which was the key step for alkaline leaching. Kinetics of sulfuric acid leaching can be described with unreacted shrinking core diffusion control model in whole time scale, and the activation energy of zinc leaching was less than that of iron leaching. According to the simulation results and the characteristics of activation energy, it could be inferred the activation energy for smithsonite and siderite dissolution was low and the leaching process belonged to fast reaction, while the activation energy for zinc desorption and limonite dissolution was high and the leaching process belonged to slow reaction. So zinc desorption in limonite was still the key step in sulfuric acid leaching.
In summary, in this thesis, the relations between gossan formation mechanism and mineral composition were revealed by modern analysis methods combined with the theories involved geology, mineral processing and metallurgy. The main reasons why gossan ores were difficult to be treated with conventional process were found out, and the new process for utilization of this type ores was suggested. The research results in this thesis deserve important academic value and is instructive for gossan resources exploitation and utilization.
引文
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