低品位镍红土矿硫酸浸出及浸出渣综合利用理论及工艺研究
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摘要
随着我国经济的快速增长,近年来镍消费的增长率达到年均25%以上,并一跃成为世界第一大镍消费国,但镍资源的自给率不足30%,加快开发国际镍资源是解决我国镍资源不足问题的关键所在。同时,随着硫化镍资源的逐步枯竭,国际上已经将镍资源开发的重点转移到了占全球陆地镍资源约70%的镍红土矿。本论文针对东南亚某矿区镍红土矿床不同层位低品位镍红土矿矿物特性,选择采用新型湿法冶金工艺进行镍、钻、铁等有价金属综合提取的理论和工艺研究,为低品位镍红土矿的清洁高效处理提供了可靠的依据。
首先通过对不同层位低品位镍红土矿进行化学分析、物相组成分析以及镍钴赋存状态的试验研究,确定了矿石的主要成分及其物相组成,并在此基础上选择相应的湿法冶金处理工艺。研究结果表明低品位褐铁矿层镍红土矿的主要矿物物相为针铁矿,镍主要是以晶格取代的形式存在于针铁矿中,钻主要是以氧化物的形态存在于氧化锰颗粒中。该类矿石适宜于选择采用加压硫酸浸出工艺进行处理；而低品位过渡层镍红土矿的主要矿物物相为蛇纹石和部分针铁矿,矿物中的镍主要以非结晶或弱结晶以及类质同像的形态存在于硅酸盐矿物中,钴则主要存在于氧化锰颗粒中。该类矿石适宜于采用常压硫酸浸出工艺进行处理；低品位腐植土层镍红土矿的主要矿物物相为利蛇纹石、镍绿泥石和蒙脱石。镍主要以吸附状态或类质同像形态存在于镁或铁的硅酸盐矿物中,易于在常压状态下被酸溶液浸出,但是由于镁的含量很高,浸出过程中的酸耗将会很大,该类矿石适宜于作为中和剂用于浸出液中游离酸的中和。
对低品位过渡层镍红土矿常压硫酸浸出进行热力学计算分析,结果表明,常压条件下采用硫酸从过渡层镍红土矿中浸出镍是可行的。其浸出过程动力学实验研究表明,镍的浸出反应受固膜外扩散控制,而铁的浸出动力学符合液-固反应收缩未反应核模型,受内扩散控制。过渡层镍红土矿硫酸常压浸出试验研究表明,浸出温度、硫酸加入量、浸出时间、液固比以及矿石粒度对浸出效果有较大影响。在最佳浸出条件下,镍的浸出率可以达到86%以上,而铁的浸出率仅为28%左右,说明该浸出过程具有一定的选择性。采用腐植土中和-高温水解除铁新工艺对常压浸出液进行除杂研究,结果显示,常压浸出液中铁、铬、铝沉淀率分别为96.19%、93.32%和93.99%,镍的回收率达到96%以上,水解渣的主要成分为Fe2O3。
针对褐铁矿层镍红土矿高温高压酸浸过程进行了热力学计算与分析,结果表明,针铁矿水热生成赤铁矿的ΔGT值随温度升高而降低,说明提高浸出温度有利于铁的浸出率的降低和镍、钴浸出率的提高。褐铁矿层镍红土矿硫酸加压浸出试验表明,硫酸加入量和浸出温度对浸出效果的影响最大,温度越高浸出效果越好。最佳条件下镍和钴的浸出率可达95%以上,而铁的浸出率小于2%,浸出过程的选择性较高。探索了加压浸出液腐植土中和工艺,实验结果表明,在一定条件下,腐植土矿石中镍的浸出率可达65%以上,游离酸的中和率达到90%以上。
研究了石灰石中和除铁铝-C272离心萃取分离钴锰-低含量镍溶液直接旋流电积金属镍的新型浸出液处理工艺,结果表明该工艺具有流程简短、金属回收率高、能耗低、过程清洁等优点。通过石灰石中和除铁铝,得到的除杂后液中铁、铝、铬的含量均降低到0.02g/L以下,镍钴回收率均大于95%。中和后液采用新型萃取剂-C272通过高效离心萃取器进行镍钴萃取分离,得到的萃余液中Co2+、Mn2+的浓度均达到0.002g/L以下,而反萃液中Ni2+的浓度则小于0.05g/L,萃取分离效果良好。同时C272对钙的萃取率很低,从而避免了反萃过程中硫酸钙沉淀的产生。所采用的离心萃取器与传统的萃取设备相比,则具有通量大、级效率高、萃取速度快等优点。旋流选择电积技术是一种新型电解分离提取技术,能够直接从低浓度溶液中高效电解提取金属产品。低浓度镍萃余液旋流电积试验结果表明,得到的阴极镍产品质量符合国标GB/TNi9990的要求,其阴极电流效率达到93.8%,镍的直接回收率达到93.6%。说明旋流选择电积技术具有选择性高、能耗低的优点。
探索了浸出渣还原磁化焙烧-磁选铁精矿综合回收工艺,研究结果表明,含铁较高的水解渣和加压浸出渣通过该工艺处理后,可以实现铁资源的综合利用,磁选铁精矿中铁的含量达到64%以上,硫的含量达到0.2%以下,其化学成分完全达到炼铁行业对铁精矿化学成分的要求,铁精矿产率达到79.5%,铁的回收率达到87.6%。
通过本研究,确定了针对于低品位镍红土矿床不同层位的矿物分别采用硫酸常压浸出-高温水解除铁-石灰石中和除杂-C272高效离心萃取-旋流选择性电积镍,以及硫酸加压浸出-腐植土中和-石灰石中和深度除杂-C272高效离心萃取-旋流选择性电积镍的镍红土矿湿法冶金新工艺,该工艺对低品位镍红土矿具有较强的适应性,镍、钴的回收率较高,同时还可以综合回收铁。实验研究取得了大量的有价值的工艺参数和理论数据,对低品位镍红土矿的综合开发和利用具有指导意义。
As the rapid development of economy in China, the Chinese nickel consumption ranks first in the world with an average annual growth rate of 25% in recent years. However, its self-sufficiency rate is lower than 30%, and the key method to solve this problem is to develop the oversea nickel resources. At the same time, with the depletion of nickel sulfide resources, the exploration has been focused on nikcle laterite ones which account for 70% of the total nickel resources. In this study, novel hydrometallurgical processes have been chosen to recover nickel, cobalt and iron from nickel laterite based on the research on the mineralogical characterization of different layers of nickel laterite in southeast Asia area. This study provides reliable basis of clean and effective ways for low-grade nickel laterite processing.
The corresponding hydrometallurgical processes were chosen based on the analysis of chemical composition, mineral phase and modes of occurrence of nickel and cobalt of different layers of nickel laterite. The results show that the main mineral in nickel laterite with high iron content is goethite while nickel exists in the form of lattice substituted in goethite and cobalt exists in the oxide form associated with manganese oxides. This kind of ore is usually treated by pressure sulfuric acid leaching process. The main minerals in transition layer are serpentine and goethite while nickel exists in the form of non-crystallization or weak crystallization or isomorphism in silicate, and cobalt exists in the manganese oxides. This kind of ore is usually treated by atmosphere sulfuric acid leaching process. The main minerals in saprolitic are serpentine, chlorite and montmorillonite. In these minerals, nickel exists in the form of adsorption or isomorphism in magnesium or iron silicate, which is easily dissolved in acid solution at atmospheric condition. However, this kind of ore is of high magnesium content and usually used as neutralizer for acid leach instead of being processed with acid.
The thermodynamic study on atmosphere leaching of transition layer of nickel laterite was conducted and the results show that this method is feasible. The dynamic results in leaching process show that nickel extraction rate is controlled by diffusion through water film and iron dissolution rate is controlled by intraparticle diffusion which follows the liquid/solid shrinking core model. The experimental results show that the leaching temperature, sulfuric acid addition, leaching time, S/L ratio and mineral particles have significant effects on leaching efficiency. Under optimum conditions, the nickel extraction is more than 86% and the iron dissolution is only about 28%, which indicates the process is selective with nickel against iron. The leaching solution was neutralized by saprolitic followed by high-temperature hydrolysis of iron. The removal of iron, chromium and aluminum from leaching solution are 96.19%, 93.32% and 93.99%, respectively. The hydrolysis residue is mainly Fe2O3.
The thermodynamic study on pressure leaching of limonite was conducted and the results show that theΔGT value of goethite to hematite decreases with the increase of temperature, which indicates that the increase of temperature is helpful to reduce the iron dissolution and improve the nickel and cobalt extraction. The leaching experimental results show that the sulfuric acid addition and leaching temperature are the most effective factors. The higher the temperature, the better extraction results could be obtained. Both the extractions of nickel and cobalt are more than 95% and the iron dissolution is less than 2% under optimum conditions. The neutralization of pressure leaching solution by saprolitic was investigated and the results show that the nickel extraction from saprolitic is more than 65% and more than 90% acid is neutralized in this process.
A novel treatment process was studied including iron and aluminum removal by limestone neutralization, nickel separation from cobalt and manganese by C272 centrifugation extraction and recovery of nickel from low nickel concentration solution by direct cyclone electrowinning. The results show that this method has the advantages of short route, high metal recovery, low energy consumption and clean production. The iron, aluminum and chromium concentration in purified solution are all lower than 0.02g/L after limestone neutralization, and the recovery of both nickel and cobalt are more than 95%. Then, the cobalt and manganese were separated from nickel by C272 centrifugation extraction. Both cobalt and manganese concentration in raffinate are lower than 0.002g/L, and the nickel concentration in stripping solution is lower than 0.05g/L. Meanwhile, the calcium extraction by C272 is quite low which avoids the calcium carbonate precipitation in stripping process. Compared to traditional extraction device, the centrifugation extractor shows the advantages including big flux, high stage efficiency and quick extraction speed. Selective cyclone electrowinning is a novel separation technology, which can be used for direct electrowinning of metals from low concentration solution. The experimental results of cyclone electrowinning of nickel show that the cathode nickel meets the requirement of national standard GB/TNi9990. The current efficiency is 93.8%, and the direct recovery of nickel is 93.6%. It indicates the cyclone electrowinning method shows advantages of high selectivity and low energy consumption.
The iron in leaching residue was recovered as concentrate by reduction-roasting magnetic separation method. The results show that the iron resources from hydrolysis and pressure leaching processes are comprehensively utilized by this method. The iron content in concentrate is above 64%, and the sulfur content is lower than 0.2%, which totally meet the chemical component requirements of iron concentrate to iron-making industry. The weight percentage of iron concentrate is 79.5% and the iron recovery is 87.6%.
In this study, based on the mineral differences of different layers of nickel laterite, two novel hydrometallurgical processes were investigated: atmosphere sulfuric acid leaching-iron removal by hydrolysis-neutralization by limestone-nickel separation by C272 centrifugation extraction-nickel recovery by direct cyclone electrowinning, and pressure sulfuric acid leaching-acid neutralization by saprolitic-neutralization by limestone-nickel separation by C272 centrifugation extraction-nickel recovery by direct cyclone electrowinning. These processes are quite feasible to treat the low-grade nickel laterite with high recovery of nickel and cobalt, and comprehensive utilization of iron. This study obtained large amounts of valuable process parameters and theoretic data, which are of great significance for comprehensive explosion and utilization of low-grade nickel laterite.
首先通过对不同层位低品位镍红土矿进行化学分析、物相组成分析以及镍钴赋存状态的试验研究,确定了矿石的主要成分及其物相组成,并在此基础上选择相应的湿法冶金处理工艺。研究结果表明低品位褐铁矿层镍红土矿的主要矿物物相为针铁矿,镍主要是以晶格取代的形式存在于针铁矿中,钻主要是以氧化物的形态存在于氧化锰颗粒中。该类矿石适宜于选择采用加压硫酸浸出工艺进行处理；而低品位过渡层镍红土矿的主要矿物物相为蛇纹石和部分针铁矿,矿物中的镍主要以非结晶或弱结晶以及类质同像的形态存在于硅酸盐矿物中,钴则主要存在于氧化锰颗粒中。该类矿石适宜于采用常压硫酸浸出工艺进行处理；低品位腐植土层镍红土矿的主要矿物物相为利蛇纹石、镍绿泥石和蒙脱石。镍主要以吸附状态或类质同像形态存在于镁或铁的硅酸盐矿物中,易于在常压状态下被酸溶液浸出,但是由于镁的含量很高,浸出过程中的酸耗将会很大,该类矿石适宜于作为中和剂用于浸出液中游离酸的中和。
对低品位过渡层镍红土矿常压硫酸浸出进行热力学计算分析,结果表明,常压条件下采用硫酸从过渡层镍红土矿中浸出镍是可行的。其浸出过程动力学实验研究表明,镍的浸出反应受固膜外扩散控制,而铁的浸出动力学符合液-固反应收缩未反应核模型,受内扩散控制。过渡层镍红土矿硫酸常压浸出试验研究表明,浸出温度、硫酸加入量、浸出时间、液固比以及矿石粒度对浸出效果有较大影响。在最佳浸出条件下,镍的浸出率可以达到86%以上,而铁的浸出率仅为28%左右,说明该浸出过程具有一定的选择性。采用腐植土中和-高温水解除铁新工艺对常压浸出液进行除杂研究,结果显示,常压浸出液中铁、铬、铝沉淀率分别为96.19%、93.32%和93.99%,镍的回收率达到96%以上,水解渣的主要成分为Fe2O3。
针对褐铁矿层镍红土矿高温高压酸浸过程进行了热力学计算与分析,结果表明,针铁矿水热生成赤铁矿的ΔGT值随温度升高而降低,说明提高浸出温度有利于铁的浸出率的降低和镍、钴浸出率的提高。褐铁矿层镍红土矿硫酸加压浸出试验表明,硫酸加入量和浸出温度对浸出效果的影响最大,温度越高浸出效果越好。最佳条件下镍和钴的浸出率可达95%以上,而铁的浸出率小于2%,浸出过程的选择性较高。探索了加压浸出液腐植土中和工艺,实验结果表明,在一定条件下,腐植土矿石中镍的浸出率可达65%以上,游离酸的中和率达到90%以上。
研究了石灰石中和除铁铝-C272离心萃取分离钴锰-低含量镍溶液直接旋流电积金属镍的新型浸出液处理工艺,结果表明该工艺具有流程简短、金属回收率高、能耗低、过程清洁等优点。通过石灰石中和除铁铝,得到的除杂后液中铁、铝、铬的含量均降低到0.02g/L以下,镍钴回收率均大于95%。中和后液采用新型萃取剂-C272通过高效离心萃取器进行镍钴萃取分离,得到的萃余液中Co2+、Mn2+的浓度均达到0.002g/L以下,而反萃液中Ni2+的浓度则小于0.05g/L,萃取分离效果良好。同时C272对钙的萃取率很低,从而避免了反萃过程中硫酸钙沉淀的产生。所采用的离心萃取器与传统的萃取设备相比,则具有通量大、级效率高、萃取速度快等优点。旋流选择电积技术是一种新型电解分离提取技术,能够直接从低浓度溶液中高效电解提取金属产品。低浓度镍萃余液旋流电积试验结果表明,得到的阴极镍产品质量符合国标GB/TNi9990的要求,其阴极电流效率达到93.8%,镍的直接回收率达到93.6%。说明旋流选择电积技术具有选择性高、能耗低的优点。
探索了浸出渣还原磁化焙烧-磁选铁精矿综合回收工艺,研究结果表明,含铁较高的水解渣和加压浸出渣通过该工艺处理后,可以实现铁资源的综合利用,磁选铁精矿中铁的含量达到64%以上,硫的含量达到0.2%以下,其化学成分完全达到炼铁行业对铁精矿化学成分的要求,铁精矿产率达到79.5%,铁的回收率达到87.6%。
通过本研究,确定了针对于低品位镍红土矿床不同层位的矿物分别采用硫酸常压浸出-高温水解除铁-石灰石中和除杂-C272高效离心萃取-旋流选择性电积镍,以及硫酸加压浸出-腐植土中和-石灰石中和深度除杂-C272高效离心萃取-旋流选择性电积镍的镍红土矿湿法冶金新工艺,该工艺对低品位镍红土矿具有较强的适应性,镍、钴的回收率较高,同时还可以综合回收铁。实验研究取得了大量的有价值的工艺参数和理论数据,对低品位镍红土矿的综合开发和利用具有指导意义。
As the rapid development of economy in China, the Chinese nickel consumption ranks first in the world with an average annual growth rate of 25% in recent years. However, its self-sufficiency rate is lower than 30%, and the key method to solve this problem is to develop the oversea nickel resources. At the same time, with the depletion of nickel sulfide resources, the exploration has been focused on nikcle laterite ones which account for 70% of the total nickel resources. In this study, novel hydrometallurgical processes have been chosen to recover nickel, cobalt and iron from nickel laterite based on the research on the mineralogical characterization of different layers of nickel laterite in southeast Asia area. This study provides reliable basis of clean and effective ways for low-grade nickel laterite processing.
The corresponding hydrometallurgical processes were chosen based on the analysis of chemical composition, mineral phase and modes of occurrence of nickel and cobalt of different layers of nickel laterite. The results show that the main mineral in nickel laterite with high iron content is goethite while nickel exists in the form of lattice substituted in goethite and cobalt exists in the oxide form associated with manganese oxides. This kind of ore is usually treated by pressure sulfuric acid leaching process. The main minerals in transition layer are serpentine and goethite while nickel exists in the form of non-crystallization or weak crystallization or isomorphism in silicate, and cobalt exists in the manganese oxides. This kind of ore is usually treated by atmosphere sulfuric acid leaching process. The main minerals in saprolitic are serpentine, chlorite and montmorillonite. In these minerals, nickel exists in the form of adsorption or isomorphism in magnesium or iron silicate, which is easily dissolved in acid solution at atmospheric condition. However, this kind of ore is of high magnesium content and usually used as neutralizer for acid leach instead of being processed with acid.
The thermodynamic study on atmosphere leaching of transition layer of nickel laterite was conducted and the results show that this method is feasible. The dynamic results in leaching process show that nickel extraction rate is controlled by diffusion through water film and iron dissolution rate is controlled by intraparticle diffusion which follows the liquid/solid shrinking core model. The experimental results show that the leaching temperature, sulfuric acid addition, leaching time, S/L ratio and mineral particles have significant effects on leaching efficiency. Under optimum conditions, the nickel extraction is more than 86% and the iron dissolution is only about 28%, which indicates the process is selective with nickel against iron. The leaching solution was neutralized by saprolitic followed by high-temperature hydrolysis of iron. The removal of iron, chromium and aluminum from leaching solution are 96.19%, 93.32% and 93.99%, respectively. The hydrolysis residue is mainly Fe2O3.
The thermodynamic study on pressure leaching of limonite was conducted and the results show that theΔGT value of goethite to hematite decreases with the increase of temperature, which indicates that the increase of temperature is helpful to reduce the iron dissolution and improve the nickel and cobalt extraction. The leaching experimental results show that the sulfuric acid addition and leaching temperature are the most effective factors. The higher the temperature, the better extraction results could be obtained. Both the extractions of nickel and cobalt are more than 95% and the iron dissolution is less than 2% under optimum conditions. The neutralization of pressure leaching solution by saprolitic was investigated and the results show that the nickel extraction from saprolitic is more than 65% and more than 90% acid is neutralized in this process.
A novel treatment process was studied including iron and aluminum removal by limestone neutralization, nickel separation from cobalt and manganese by C272 centrifugation extraction and recovery of nickel from low nickel concentration solution by direct cyclone electrowinning. The results show that this method has the advantages of short route, high metal recovery, low energy consumption and clean production. The iron, aluminum and chromium concentration in purified solution are all lower than 0.02g/L after limestone neutralization, and the recovery of both nickel and cobalt are more than 95%. Then, the cobalt and manganese were separated from nickel by C272 centrifugation extraction. Both cobalt and manganese concentration in raffinate are lower than 0.002g/L, and the nickel concentration in stripping solution is lower than 0.05g/L. Meanwhile, the calcium extraction by C272 is quite low which avoids the calcium carbonate precipitation in stripping process. Compared to traditional extraction device, the centrifugation extractor shows the advantages including big flux, high stage efficiency and quick extraction speed. Selective cyclone electrowinning is a novel separation technology, which can be used for direct electrowinning of metals from low concentration solution. The experimental results of cyclone electrowinning of nickel show that the cathode nickel meets the requirement of national standard GB/TNi9990. The current efficiency is 93.8%, and the direct recovery of nickel is 93.6%. It indicates the cyclone electrowinning method shows advantages of high selectivity and low energy consumption.
The iron in leaching residue was recovered as concentrate by reduction-roasting magnetic separation method. The results show that the iron resources from hydrolysis and pressure leaching processes are comprehensively utilized by this method. The iron content in concentrate is above 64%, and the sulfur content is lower than 0.2%, which totally meet the chemical component requirements of iron concentrate to iron-making industry. The weight percentage of iron concentrate is 79.5% and the iron recovery is 87.6%.
In this study, based on the mineral differences of different layers of nickel laterite, two novel hydrometallurgical processes were investigated: atmosphere sulfuric acid leaching-iron removal by hydrolysis-neutralization by limestone-nickel separation by C272 centrifugation extraction-nickel recovery by direct cyclone electrowinning, and pressure sulfuric acid leaching-acid neutralization by saprolitic-neutralization by limestone-nickel separation by C272 centrifugation extraction-nickel recovery by direct cyclone electrowinning. These processes are quite feasible to treat the low-grade nickel laterite with high recovery of nickel and cobalt, and comprehensive utilization of iron. This study obtained large amounts of valuable process parameters and theoretic data, which are of great significance for comprehensive explosion and utilization of low-grade nickel laterite.
引文
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