Generation process of FeS and its inhibition mechanism on iron mineral reduction in selective direct reduction of laterite nickel ore

Numerous studies have demonstrated that Na₂SO₄ can significantly inhibit the reduction of iron oxide in the selective reduction process of laterite nickel ore. FeS generated in the process plays an important role in selective reduction, but the generation process of FeS and its inhibition mechanism on iron reduction are not clear. To figure this out, X-ray diffraction and scanning electron microscopy analyses were conducted to study the roasted ore. The results show that when Na₂SO₄ is added in the roasting, the FeO content in the roasted ore increases accompanied by the emergence of FeS phase. Further analysis indicates that Na₂S formed by the reaction of Na₂SO₄ with CO reacts with SiO₂ at the FeO surface to generate FeS and Na₂Si₂O₅. As a result, a thin film forms on the surface of FeO, hindering the contact between reducing gas and FeO. Therefore, the reduction of iron is depressed, and the FeO content in the roasted ore increases.     

Feasibility of co-reduction roasting of a saprolitic laterite ore and waste red mud

Large scale utilization is still an urgent problem for waste red mud with a high content of alkaline metal component in the future. Laterite ores especially the saprolitic laterite ore are one refractory nickel resource, the nickel and iron of which can be effectively recovered by direct reduction and magnetic separation. Alkaline metal salts were usually added to enhance reduction of laterite ores. The feasibility of co-reduction roasting of a saprolitic laterite ore and red mud was investigated. Results show that the red mud addition promoted the reduction of the saprolitic laterite ore and the iron ores in the red mud were co-reduced and recovered. By adding 35wt% red mud, the nickel grade and recovery were 4.90wt% and 95.25wt%, and the corresponding iron grade and total recovery were 71.00wt% and 93.77wt%, respectively. The X-ray diffraction (XRD), scanning electron microscopy, and energy dispersive spectroscopy (SEM-EDS) analysis results revealed that red mud addition was helpful to increase the liquid phase and ferronickel grain growth. The chemical compositions “CaO and Na₂O” in the red mud replaced FeO to react with SiO₂ and MgSiO₃ to form augite.     

Reaction condition optimization and kinetic investigation of roasting zinc oxide ore using (NH<Subscript>4</Subscript>)<Subscript>2</Subscript>SO<Subscript>4</Subscript>

An orthogonal test was used to optimize the reaction conditions of roasting zinc oxide ore using (NH₄)₂SO₄. The optimized reaction conditions are defined as an (NH₄)₂SO₄/zinc molar ratio of 1.4:1, a roasting temperature of 440°C, and a thermostatic time of 60 min. The molar ratio of (NH₄)₂SO₄/zinc is the most predominant factor and the roasting temperature is the second significant factor that governs the zinc extraction. Thermogravimetric–differential thermal analysis was used for (NH₄)₂SO₄ and zinc mixed in a molar ratio of 1.4:1 at the heating rates of 5, 10, 15, and 20 K·min-1. Two strong endothermic peaks indicate that the complex chemical reactions occur at approximately 290°C and 400°C. XRD analysis was employed to examine the transformations of mineral phases during roasting process. Kinetic parameters, including reaction apparent activation energy, reaction order, and frequency factor, were calculated by the Doyle–Ozawa and Kissinger methods. Corresponding to the two endothermic peaks, the kinetic equations were obtained.     

石油焦作还原剂对低品位红土镍矿与赤泥共还原制备镍铁的影响

石油焦作为工业固体废物,其堆积和储存对生态环境产生巨大的影响。本文对石油焦在低品位红土镍矿与赤泥共还原过程中用作还原剂的可行性及其机理进行了研究。通过研究石油焦用量、焙烧温度和焙烧时间等对红土镍矿与赤泥共还原过程的影响,确定最佳的工艺条件为石油焦用量20wt%、焙烧温度1250°C、焙烧时间60 min。在此条件下,可以获得镍品位1.96wt%、铁品位85.76wt%、镍回收率97.83wt%、铁回收率96.81wt%的镍铁产品。扫描电镜和能谱(SEM–EDS)分析结果表明,红土镍矿与赤泥共还原过程中镍和铁主要以镍铁颗粒的形式存在,镍铁颗粒分布均匀且纯度很高,粒径约30 μm。结果表明,石油焦作为还原剂用于红土镍矿和赤泥共还原是可行的,与无烟煤作还原剂相比,石油焦具有成本低的优点。研究结果不仅为石油焦的利用提供了一个新途径,同时也为缺煤地区红土镍矿与赤泥共还原工艺的利用提供了一种解决方案。     

Simultaneously catalytic removal of NO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> and particulate matter on diesel particulate filter

Diesel engines combine a high fuel economy with high durability and low maintenance costs and are, there-fore, used on a large scale for transportation purposes.However, the environmental pollution by diesel-engine exhausts has become more and more serious in the lastdecade, and currently the regulation of diesel emissions becomes tightened especially with respect to nitrogen ox-ides (NOx) and particulate matters (PM). Since the reduc-tion of both NOx and PM to the admitted level cannot be …     

红土镍矿还原熔炼制备镍铁的试验研究

对低铁、高硅、高镁腐殖土型红土镍矿的脱水和碳还原过程进行DTA-TG分析,确定脱水和固体碳还原反应的温度区间。在煅烧-还原熔炼红土镍矿制备镍铁中,针对矿石自然渣型碱度低、黏度及密度大,不利于金属与渣分离及镍回收率提高等问题,采用控制CaO加入量的方法,调节CaO-FeO-MgO-SiO2系炉渣的黏度和密度;探讨还原剂焦粉及CaO用量、温度、时间对熔炼效果的影响。综合考虑镍铁品位和镍的回收率,确定最佳还原熔炼试验条件:焦粉、石灰与矿石质量比分别为9.0%和8.3%,温度为1 550℃,时间为40 min。在最佳试验条件下,产出的镍铁品位为22.0%,镍、钴回收率分别为92.5%和70.0%。     

Ferronickel enrichment by fine particle reduction and magnetic separation from nickel laterite ore

Ferronickel enrichment and extraction from nickel laterite ore were studied through reduction and magnetic separation. Reduction experiments were performed using hydrogen and carbon monoxide as reductants at different temperatures (700–1000°C). Magnetic separation of the reduced products was conducted using a SLon-100 cycle pulsating magnetic separator (1.2 T). Composition analysis indicates that the nickel laterite ore contains a total iron content of 22.50wt% and a total nickel content of 1.91wt%. Its mineral composition mainly consists of serpentine, hortonolite, and goethite. During the reduction process, the grade of nickel and iron in the products increases with increasing reduction temperature. Although a higher temperature is more favorable for reduction, the temperature exceeding 1000°C results in sintering of the products, preventing magnetic separation. After magnetic separation, the maximum total nickel and iron concentrations are 5.43wt% and 56.86wt%, and the corresponding recovery rates are 84.38% and 53.76%, respectively.     

东鞍山浮选尾矿预富集精矿悬浮磁化焙烧试验研究

为实现东鞍山铁矿石浮选尾矿的资源化利用,对浮选尾矿预富集精矿开展了悬浮磁化焙烧试验研究.结果表明,浮选尾矿预富集精矿主要矿物组成为赤褐铁矿、磁铁矿、菱铁矿和石英,TFe品位为31.13%.浮选尾矿预富集精矿适宜的悬浮磁化焙烧工艺参数为:气体流量600mL/min,氢气体积分数20%,焙烧温度520℃,焙烧时间20min.焙烧产品经弱磁选可得铁精矿的TFe品位为64.23%,回收率为79.53%.焙烧产品的铁物相,XRD,VSM分析表明,经过悬浮磁化焙烧后,原矿中赤褐铁矿和碳酸铁转变为磁铁矿,矿石的饱和磁化强度和磁化率增强.     

东鞍山含碳酸盐铁矿石悬浮磁化焙烧试验

介绍了一种半工业试验用悬浮焙烧设备,并考察了焙烧温度、还原气体CO及流化气体N₂用量对东鞍山含碳酸盐铁矿石预富集粗精矿悬浮焙烧效果的影响.试验结果表明,在焙烧温度540℃,还原气体CO用量4m³/h及流化气体N₂用量2m³/h的条件下,焙烧物料经磨矿-磁选后可获得铁品位66.1%,回收率91.2%的铁精矿.铁的化学物相、光学显微结构及穆斯堡尔谱分析表明,经悬浮焙烧后弱磁性的菱铁矿和赤铁矿转化为了强磁性的磁铁矿,部分结晶粒度较粗(>100μm)的赤铁矿仅颗粒表面转变为磁铁矿,但这种Fe₂O₃@Fe₃O₄核壳结构的新生磁铁矿由于磁性较强,在后续磁选过程中依然能够得到有效的回收,并不会影响分选效果.     

Two-stage reduction for the preparation of ferronickel alloy from nickel laterite ore with low Co and high MgO contents

The preparation of ferronickel alloy from the nickel laterite ore with low Co and high MgO contents was studied by using a pre-reduction-smelting method. The effects of reduction time, calcination temperature, quantity of reductant and calcium oxide (CaO), and pellet diameter on the reduction ratio of Fe and on the pellet strength were investigated. The results show that, for a roasting temperature >800℃, a roasting time >30 min, 1.5wt% added anthracite coal, 5wt% added CaO, and a pellet size of~10 mm, the reduction ratio of Fe exceeds 70% and the compressive strength of the pellets exceeds 10 kg per pellet. Reduction smelting experiments were performed by varying the smelting time, temperature, quantity of reductant and CaO, and reduction ratio of Fe in the pellets. Optimal conditions for the reduction smelting process are as follows:smelting time, 30-45 min; smelting temperature, 1550℃; quantity of reductant, 4wt%-5wt%; and quantity of CaO, 5wt%; leading to an Fe reduction ratio of 75% in the pellets. In addition, the mineral composition of the raw ore and that during the reduction process were investigated by process mineralogy.     

某高磷鲕状赤铁矿磷赋存状态及还原焙烧脱磷研究

采用浸出、电渗析等试验方法研究了尼日利亚高磷鲕状赤铁矿中磷的赋存状态并采用XRD和SEM分析添加脱磷剂Na2CO3直接还原焙烧产物的特性.结果表明,含磷矿物主要是呈微细粒包裹体嵌布在铁矿物鲕粒的裂隙或孔洞中的纤磷钙铝石(CaAl3(OH)6(HPO4)(PO4))、蓝磷铝铁矿(FeAl2(PO4)2OH·6H2O)以及均匀分散在铁矿物中的磷.通过添加脱磷剂Na2CO3的还原焙烧磁选可实现高效铁磷分离.磷通过两种方式去除:一部分含磷矿物与金属铁分离,存在于脉石矿物中,通过磨矿磁选可以有效去除,一部分含磷矿物与Na2CO3反应生成溶于水的磷矿物,最终使得还原铁产品中的磷含量降低.     

蛇纹石型红土矿常压酸浸实验研究

主要探讨了常压下盐酸对蛇纹石型红土镍矿进行浸出的工艺条件。考察了酸矿比、液固比、反应温度、反应时间等对蛇纹石型红土镍矿浸出的影响。通过实验得出最佳工艺条件:酸矿比为2.5∶1、液固比为5∶1、反应时间为0.5 h、反应温度为100℃。在此条件下镍、钴、铁浸出率分别为100%、100%和90%。     

Synthesis and characterization of Co<Subscript>3</Subscript>O<Subscript>4</Subscript> prepared from atmospheric pressure acid leach liquors of nickel laterite ores

A chemical precipitation-thermal decomposition method was developed to synthesize Co₃O₄ nanoparticles using cobalt liquor obtained from the atmospheric pressure acid leaching process of nickel laterite ores. The effects of the precursor reaction temperature, the concentration of Co2+, and the calcination temperature on the specific surface area, morphology, and the electrochemical behavior of the obtained Co₃O₄ particles were investigated. The precursor basic cobaltous carbonate and cobaltosic oxide products were characterized and analyzed by Fourier transform infrared spectroscopy, thermogravimetric differential thermal analysis, X-ray diffraction, field-emission scanning electron microscopy, specific surface area analysis, and electrochemical analysis. The results indicate that the specific surface area of the Co₃O₄ particles with a diameter of 30 nm, which were obtained under the optimum conditions of a precursor reaction temperature of 30℃, 0.25 mol/L Co2+, and a calcination temperature of 350℃, was 48.89 m2/g. Electrodes fabricated using Co₃O₄ nanoparticles exhibited good electrochemical properties, with a specific capacitance of 216.3 F/g at a scan rate of 100 mV/s.     

红土镍矿深度还原-磁选富集镍铁实验研究

采用深度还原-磁选工艺,以煤粉为还原剂,添加氧化钙作助溶剂,在微熔化,不完全造渣的条件下,将矿石中镍和铁的氧化物还原成金属镍铁,然后经磁选方法使金属镍铁在磁性产品中得到富集.结果表明,深度还原最佳工艺条件为:还原温度1 300℃,还原时间60 min,配煤过剩倍数2.在此工艺条件下得到镍、铁质量分数分别为5.01%,22.46%的镍铁产品,镍、铁回收率分别为96.05%,79.69%.对深度还原过程研究表明,还原物料中镍和铁以金属合金颗粒形式存在,高温有利于镍铁金属相凝聚,适当延长还原反应时间有利于镍铁颗粒的还原和聚集长大,进而有利于磁选富集.     

One-pot synthesis of PVP-coated Ni<Subscript>0.6</Subscript>Fe<Subscript>2.4</Subscript>O<Subscript>4</Subscript> nanocrystals

Novel poly(N-vinyl-2-pyrrolidone) (PVP)-coated nickel ferrite nanocrystals were prepared by simultaneously pyrolyzing nickel(II) acetylacetonate (Ni(acac)₂) and iron(III) acetylacetonate (Fe(acac)₃) in N-vinyl-2-pyrrolidone (NVP). The PVP coating was formed in situ through polymerization of NVP. The crystalline structure of the resultant nickel ferrite was analyzed by high-resolution transmission electron microscopy, electron diffraction patterns, and powder X-ray diffraction. In addition, the valence state of Ni and the metal contents of Ni and Fe in different valence states were analyzed by X-ray photoelectron spectroscopy (XPS), atomic absorption and the phenanthroline method. The surface coating layer of PVP and its binding states were characterized by Fourier transform infrared spectroscopy in combination with XPS. Colloidal stability experiments revealed that the nanocrystals could be dispersed well in both phosphate-buffered saline and Dulbecco’s Modified Eagle Medium.     

Effect of reduction roasting by using bio-char derived from empty fruit bunch on the magnetic properties of Malaysian iron ore

Beneficiation of Malaysian iron ore is becoming necessary as iron resources are depleting. However, the upgrading process is challenging because of the weak magnetic properties of Malaysian iron ore. In this study, bio-char derived from oil palm empty fruit bunch (EFB) was utilized as an energy source for reduction roasting. Mixtures of Malaysian iron ore and the bio-char were pressed into briquettes and subjected to reduction roasting processes at 873–1173 K. The extent of reduction was estimated on the basis of mass loss, and the magnetization of samples was measured using a vibrating sample magnetometer (VSM). When reduced at 873 K, the original goethite-rich ore was converted into hematite. An increase in temperature to 1073 K caused a significant conversion of hematite into magnetite and enhanced the magnetic susceptibility and saturation magnetization of samples. The magnetic properties diminished at 1173 K as the iron ore was partially reduced to wustite. This reduction roasting by using the bio-char can assist in upgrading the iron ore by improving its magnetic properties.     

红土镍矿微波水热法浸提镍钴

采用微波水热盐酸浸出方法对腐泥土型红土镍矿提取镍钴进行了研究,详细探讨了焙烧预处理、微波水热浸出温度和浸出时间对镍钴浸出率的影响.对于300℃焙烧预处理后的红土镍矿,微波水热温度为50℃,浸出时间为1 h时,镍的浸出率高达93.65%,钴的浸出率为87.86%.红土镍矿的微波水热浸出体系与普通水热浸出体系相比,镍和钴的浸出效果更好.研究表明,扩散过程是镍、钴浸出过程的主要限制环节.     

CaF2强化红土镍矿自还原过程中金属相聚集长大行为

针对高镁高硅型中低品位红土镍矿,采用煤基自还原-细磨-磁选工艺制备镍铁粉,研究了内配碳比对红土镍矿中铁、镍氧化物自还原的影响,CaF_2对红土镍矿自还原过程中氧化物的还原、金属相的析出及聚集长大的影响规律。研究表明在CaF_2作用下通过降低内配碳比可抑制氧化铁的还原,从而获得镍品位较高的镍铁粉,但相应牺牲镍的回收率;CaF_2能与红土镍矿中高熔点的硅酸盐脉石通过固相反应生成低熔点的透闪石(Ca_2Mg_5(Si_4O_(11))_2F_2),使硅酸盐矿物结构由岛状转变为链状,提高硅酸盐矿物反应活性,促进镍、铁氧化物的还原;通过降低红土镍矿脉石相的熔化性温度,CaF_2能明显强化红土镍矿自还原过程中金属相的析出、聚集和长大,促进镍铁与脉石的有效分离,从而大幅度提高镍铁粉中镍和铁的品位及金属元素的回收率。     

稀酸浸出还原焙烧红土矿时铁还原度对浸出的影响

对含镍的红土矿进行了微波加热还原焙烧-稀硫酸浸出的实验研究,考察了活性炭粉加入量、微波功率和加热时间对铁还原程度的影响,并分析了铁还原度对浸出过程中镍和铁浸出率的影响.结果表明红土矿中铁的还原程度随碳粉加入量、微波功率和加热时间的增加而增大,在800 W的微波功率下加热约12.5 min即可完成还原反应.镍的浸出率与铁的还原度近似呈线性关系,但铁的浸出率在铁还原度超过60%后增长迅速.因此铁还原度控制在60%为宜,相应的镍浸出率约为85%,而铁的浸出率不超过30%.     

铬铁矿的还原焙烧与磁选分离

以南非铬铁矿为原料,以潞安煤粉为还原剂,进行了铬铁矿粉还原焙烧与磁选分离实验。借助扫描电镜、能谱分析和X射线衍射分析,对碳热还原和磁选分离过程中的物相变化进行了系统研究。实验发现,当温度低于1 200℃时,铬铁矿仅发生少量铁氧化物的还原,当温度高于1 300℃时,铬铁矿中铬氧化物开始被还原成碳化铬。随着还原反应的不断进行,铬铁尖晶石结构逐渐发生转变并被破坏。在本实验条件下,铬铁矿较为适宜的预处理温度为1 200℃,此温度下的还原产物磁选后,磁选产物几乎全部为金属铁,磁选所得尾渣的除铁率为46%,铬的收得率为80%,w(Cr2O3)/w(ΣFe O)值高达3.75。研究工作对于铬铁矿预处理工艺的设计开发及低品位铬铁矿的综合利用具有理论指导意义。