含钛铌铁精矿含碳球团熔分过程试验研究

为了实现我国白云鄂博地区含钛铌铁精矿资源的高效利用,以含钛铌铁精矿为原料,采用预还原-熔分的加热制度,研究熔分温度、熔分时间和碱度对含钛铌铁精矿含碳球团熔分行为以及渣系性质的影响.进一步采用X射线衍射、扫描电子显微镜等手段表征含碳球团在熔分过程中的微观结构及物相变化.实验结果表明:金属化率86.31 %的预还原含钛铌铁精矿含碳球团在1 400 ℃下熔分12 min后可实现渣铁有效分离,获得珠铁和富铌渣.随碱度升高,渣的熔点升高,渣的流动性指数降低,碱度为1.0时,球团的熔分效果较优;随熔分时间增加,含钛铌铁精矿含碳球团中的Ca₂Ti₂O₆相减少,Ca（Ti_0.4Fe_0.3Nb_0.3）O₃相增加,钙钛铌共生物的尺寸增加,呈十字树枝状.      

含铌铁矿粉氢气选择性还原过程中磷行为

 对白云鄂博含铌铁矿粉氢气选择性还原-熔分-铌铁冶炼的提铌方案中磷的行为进行试验研究。在该试验条件下,磷质量分数为0.100%的含铌铁矿粉通氢气还原后熔分,得到磷质量分数小于0.010%、铌质量分数为2.000%的富铌渣,铁中铌质量分数为0.008%、磷质量分数为0.230%,铌磷分离效果明显,同时熔分后铌品位是原来的3.5倍。试验结果表明,氢气在还原阶段能够在还原铁氧化物的同时将Ca3P2O8还原,通过熔分达到铌与磷、铁元素等分离的目的,铌有效地富集在渣中。     

钒钛磁铁矿碱熔低温冶炼工艺研究

为了实现钒钛磁铁矿的低温冶炼,以NaOH为碱熔剂,采用煤基直接还原技术,研究了钒钛磁铁矿直接还原—熔分工艺。主要考察了Na/Si对钒钛磁铁矿团块金属化率及熔分效果的影响,并通过XRD分析得出了Na/Si对金属化团块及熔渣物相组成的影响。采用Factsage热力学软件对不同Na/Si下Na_2O-SiO_2-TiO_2-Al_2O_3-CaO五元相的渣系熔点进行了计算。结果表明:Na/Si越高,渣系熔点越低。NaOH可有效改善钒钛磁铁矿的直接还原和熔分效果。随着团块Na/Si的升高,团块金属化率随之升高,但升高的幅度逐渐减小。当Na/Si=5.0、直接还原温度为1 150℃、C/O=1.4、直接还原时间为30 min时,团块金属化率就达到了93.17%。随着Na/Si升高,渣铁分离越彻底,当Na/Si4.0时,熔分所得粒铁表面平整度较好,熔分钛渣中无小尺寸粒铁分散。以NaOH处理钒钛磁铁矿金属化团块所得熔分渣中钛、硅、铝大多以钠酸盐形式存在,NaOH可以有效的降低钒钛磁铁矿的还原熔分难度,在1 460℃实现熔分,促进渣铁分离。     

直接还原-渣金熔分法回收钕铁硼废料

采用直接还原-渣金熔分法回收稀土钕铁硼废料中铁合金和稀土氧化物渣。将废料以一定质量比配加到铁精矿粉中,在反应罐直接还原,物料中金属铁和钴的氧化物Fe O、Co O被还原为金属单质Fe和Co,Al、Mn、RE等活性金属被氧化为Al2O3、Mn O、RE2O3;海绵铁渣金熔分中,呈单质态的元素Fe、Co形成合金,呈氧化态的稀土氧化物与铁精矿中的脉石形成REO-Si O2-Al2O3熔渣,渣中稀土氧化物含量达到48.42%,具有很高的再利用价值。对熔分渣进行熔化性温度、扫描电镜和能谱微区成分分析及X射线衍射结构分析。分析表明,熔渣的流动性良好,当废料配入比大于15%时,熔渣的软化熔融温度区间变窄;渣中的稀土以氧化物和铝酸盐的形式存在,形成树枝状晶体。     

LiCl催化剂对含铌铁矿粉氢气选择性还原的影响

在自制的扩散床底供气管式电阻炉内进行实验,研究了添加LiCl催化剂对H2选择性还原白云鄂博含铌铁矿粉中铁氧化物的影响。发现含铌铁矿粉中加入LiCl催化剂后对还原反应有促进作用,还原度和金属化率明显提高,铁氧化物几乎全部被还原为金属铁。改变催化剂的加入比率（质量分数）分别为2.14%、1.71%、1.43%、1.00%、0.71%、0.43%,结果表明,70g含铌铁矿粉中添加质量分数为0.71%的LiCl催化剂的催化效果最好,且杂质含量相对较少,其还原度达到95.82%,金属化率达93.73%。     

钒钛磁铁矿金属化球团还原熔分试验及渣相分析

通过单因素试验考察了熔分温度、熔分时间和球团碱度对钒钛磁铁矿金属化球团熔分效果的影响,利用Factsage软件计算了不同碱度配比下的渣系三元相图,并结合XRD分析了熔分渣系特点,解释钒钛磁铁矿金属化球团还原熔分过程。结果表明,适当提高熔分温度、熔分时间和球团碱度有利于渣铁分离,但球团碱度超过1.0后,由于三元渣系组成移动到了高温区,使熔渣熔化性温度升高;熔分时间超过40min后,渣系中TiN逐渐增多,增加了熔渣的黏度,不利于渣铁分离。金属化球团熔分还原的最优条件为熔分温度1 550℃、球团碱度R=1.0、熔分时间40min。     

红土镍矿选择性还原-熔分制备镍铁合金

以硅镁型红土镍矿为原料,采用金属化焙烧-熔分工艺,通过正交试验制备金属化球团,将所得金属化球团在1500℃条件下熔融分离30 min提取镍铁合金,考察影响因素对实验结果的影响.结果表明:在选择性还原制备金属化球团过程中,对金属化率的影响程度从大到小的因素依次是C/O摩尔比、焙烧温度、焙烧时间和碱度;实验可获得镍品位19%的镍铁合金;在碱度为0.8-1.2范围内,S和P分配比随着碱度的升高而增大.利用X射线衍射和扫描电镜对金属化球团及熔融分离出的渣进行微观分析,发现加入的石灰石与复杂矿相反应可释放出简单镍氧化物和铁氧化物,促进还原反应的进行,当石灰石不足时,少量铁以Fe3+的形式存在于铁金属化率70%的金属化球团中.      

微波场中铌精矿碳热还原反应行为研究

目前铌资源的研究大多处于常规加热阶段,因为能耗高、冷中心等问题无法广泛推广。微波加热技术是一种新型加热技术,可以有效避免冷中心等问题。借助微波马弗炉将铌精矿碳热还原反应与微波加热相结合,探究还原温度、配碳比及保温时间对铌精矿金属化率的影响,以及金属颗粒的成长行为。研究结果表明,微波加热在碳热还原反应中优于常规加热,在微波加热下,还原温度为1100℃、保温30 min、配碳比为1时,金属化率达到94.84%;1000℃时NbC开始生成,1100℃时铌钛产物主要为(Ti,Nb)C,1300℃时,钛的产物主要以TiC形式存在。     

钒钛铁精矿非自然碱度含碳球团高温固态还原试验

为了研究钒钛铁精矿非自然碱度含碳球团高温固态还原规律,以钒钛铁精矿为原料,在实验室条件下,探索了还原温度、还原时间、碱度和配煤比对钒钛铁精矿非自然碱度含碳球团高温固态还原的影响,采用X射线衍射仪测定了金属化球团的物相组成。研究结果表明,适当提高还原温度、延长还原时间、提高碱度和配煤比均可促使球团的金属化率提高;对于钒钛铁精矿金属化球团物相组成,在还原温度高于1 400℃时,金属化球团中出现大量碳氮化钛,碱度的提高有利于抑制还原产物中碳氮化钛的生成,配煤比的增加促进了碳氮化钛的生成。从后续熔分工序对钒钛铁精矿金属化球团质量要求的角度来说,高温固态还原的适宜条件,还原温度为1 350℃,碱度为1.0,还原时间为30 min,配煤比为1.3,在此条件下,球团的金属化率为93.72%,金属化球团碳质量分数为6.08%,主要物相为黑钛石和金属铁。     

用超声波预处理含铌原料的尝试

包头富铌炉料还原冶炼时,铌的还原回收率偏低(仅50％左右)。为了提高铌的还原回收率,在炉料入炉前,我们采用简单的超声波发生器对其进行预处理,取得了明显的效果。 (一)炉料成分、试验设备及试验方法 1,炉料成分 试验用原料为富铌低铁精矿的烧结矿,其成分列于表1。还     

Niobium and phosphorus behavior during melting-separation process of pre-reduced niobium ore concentrate

The pre-reduced Bayan Obo ferroniobium(FeNb)ore concentrate block was taken as raw materials for studying the physical properties of niobium-enriched slag and changes in niobium recovery rate.In addition,the dephosphorization rate of the slag under different melting-separation conditions was investigated using the melting-separation test.The research results demonstrate that(i)the niobium recovery rate and dephosphorization rate of the slag decrease with the increase in melting-separation temperature;(ii)the niobium recovery rate of the slag initially increases and then decreases with increase in basicity and time;and(iii)the dephosphorization rate of the slag increases with the increase in basicity and time.When the test was performed under the conditions of basicity of 0.6-0.7,time of 7-10min,and temperature of 1400-1450°C,the niobium recovery rate and dephosphorization rate are over 96%and 95%,respectively.By scanning electron microscopy,it is observed that niobium mainly exists in the form of calcium and titanium silicate within the slag phase,with uneven distribution.     

含铌铁水直接冶炼含铌微合金钢的试验

 含铌铁水通过脱碳保铌探索作为合金化元素回收铁水中铌并直接冶炼为含铌微合金钢的方法。试验在真空碳管炉内进行,铁水温度为1 500 ℃,氧化剂为Fe2O3,真空度为10 Pa,分别进行有SiO2-CaO-Al2O3系造渣剂、无渣真空氧化冶炼研究。结果表明：在无渣条件下,加入Fe2O3铁水中硅、铌和碳同时氧化,不能脱碳保铌;加入造渣剂时,造渣剂的碱度越低,铁水中的硅氧化量越低,碳氧化量越高,碳质量分数最低下降到0.032%,铌质量分数最低值从0.09%下降到0.082%;碱度越高,铁水中硅氧化量越高,铌的氧化量也越高;真空氧化冶炼能够促进碳氧化,减少硅的氧化,抑止铌氧化。在50 kg级真空感应电炉内成功进行了回收铁水中铌直接冶炼为含铌钢试验,为回收含铌铁水中的铌提供新方法,也为工业化直接冶炼含铌钢提供试验依据。     

Direct Reduction of High-phosphorus Oolitic Hematite Ore Based on Biomass Pyrolysis

Direct reduction of high-phosphorus oolitic hematite ore based on biomass pyrolysis gases(CO,H_2,and CH_4),tar,and char was conducted to investigate the effects of reduction temperature,iron ore-biomass mass ratio,and reduction time on the metallization rate.In addition,the effect of particle size on the dephosphorization and iron recovery rate was studied by magnetic separation.It was determined that the metallization rate of the hematite ore could reach 99.35% at iron ore-biomass mass ratio of 1∶0.6,reduction temperature of 1 100℃,and reduction time of 55 min.The metallization rate and the aggregation degree of iron particles increase with the increase of reduction temperature.The particle size of direct reduced iron(DRI) has a great influence on the quality of the iron concentrate during magnetic separation.The separation degree of slag and iron was improved by the addition of 15 mass% sodium carbonate.DRI with iron grade of 89.11%,iron recovery rate of 83.47%,and phosphorus content of 0.28% can be obtained when ore fines with particle size of-10 μm account for 78.15%.     

含铌铁精矿煤基直接还原过程中铌的行为研究

以含铌铁精矿为研究对象,采用固态煤作还原剂还原焙烧,再经磁选得到还原铁产品.在不同焙烧温度、还原剂用量、助熔剂用量条件下,分别以褐煤和无烟煤为还原剂,研究了各因素对直接还原焙烧-磁选结果的影响,考察焙烧过程中铌分别在渣相和金属相中的分布.试验结果表明,1200℃时80％的铌矿物进入尾矿中;而1300℃时添加助熔剂TS2用量10％条件下,90％铌矿物在直接还原焙烧-磁选得到还原铁产品中富集.     

Analysis of reduction of iron ore and oxidation of reducing gas in moving bed

To investigate the influence of technical parameters on reduction of iron ore and oxidation of reducing gas in moving bed, the coupling kinetic model of iron oxide reduction and reducing gas oxidation in moving bed was established. The model was applied in pre- reduction shaft furnace of C- 3000, and main calculating results were in a good accordance with production data. At a certain ratio of gas flow to ore mass, improving gas velocity at standard state can increase output of metal iron, yet decrease ratio of metallization and gas utilization rate. At a certain gas velocity at standard state, improving ratio of gas flow to ore mass can increase ratio of metallization, yet decrease output of metal iron and gas utilization rate. Reduction potential of gas has a substantial effect on reduction efficiency. It is suggested to improve reduction potential of gas to a 95% level for a high ratio of metallization. At a certain gas velocity at standard state, increasing gas pressure can improve ratio of metallization and gas utilization rate. Inert gas content has a disadvantageous effect on reduction reaction in moving bed. It is advantageous for improving reduction efficiency in moving bed by adjusting increasing ratio of pellet or adding part of rich- hydrogen gas in reducing gas.     

Phosphorus Removal of High Phosphorus Iron Ore byGasBased Reduction and Melt Separation

A large deposit of high phosphorus iron ore in China contains an average of 1.2% phosphorus and 50% iron and it has not been utilized. In current work, a novel process to remove phosphorus of the ore has been proposed. The novel process has been demonstrated theoretically and experimentally. The theoretical work (numerical simulation) was carried out with HSC chemistry package and a mathematical model developed using the coexistence theory of slag structure. Gas-based reduction and melt separation experiments were then designed and conducted. Simulation results shows that that all iron compounds in the ore could be reduced to metallic iron using CO/ H2 under temperature above 1000K and the yield of iron is more than 90% under either atmosphere; P can not be reduced and exists as Ca3(PO4)2; in the melt separation process, iron metallization ratio, melting temperature and CaO-adding ratio affect the phosphorus partition between slag and molten metal and CaO-adding ratio is the most distinguished parameter. Results of gas-based reduction agreed well with the simulation except for iron metallization ratio being less than predicted. This difference is mainly attributed to kinetic condition. Results of melt separation experiment show most P is left in the slag sample and some P in the metal sample exists as slag inclusion..     

Reduction kinetics of manganese oxide in basic oxygen furnace type slag

In order to improve manganese yield during the reduction of manganese ore, the reduction kinetics of manganese oxide in BOF type slag has been investigated on an experimental scale. The reduction rate of (MnO) was promoted for the slag of low basicity and high contents of (FeO). The maximum reduction rate of (MnO) has been found for an iron melt with carbon mass contents of 1.9 %. The silicon in metal may accelerate the reduction of manganese oxide in slag. The kinetic model for the reduction rate of (MnO) has been formulated based on the assumption that the reduction of (MnO) was controlled by the mass transfer through the metal and slag boundary layers at the metal/slag interface. The result calculated by the kinetic model showed a good agreement with the experimental one. The reduction behaviour of (MnO) can be described by the present model.