硝酸法生产磷酸过程中稀土的浸出研究

研究了采用硝酸法生产磷酸工艺中稀土的浸出情况。详细探讨了温度、硝酸浓度、时间、粒度、液固比等因素对磷精矿中稀土浸出率的影响。结果表明,浸出稀土的适宜工艺条件是:40%HNO3、60℃、液固比2.5、搅拌转速300 r/min、-0.038 mm占82%、浸出90 min。此条件下稀土浸出率与磷矿分解率均大于98%。     

含稀土磷精矿酸解过程稀土的分布规律

研究了富集稀土的磷精矿酸浸过程在不同溶液初始磷酸浓度和液固比浸出时稀土的富集及分布规律。结果表明,高的初始磷酸浓度和液固比有利于提高稀土在溶液中的回收率,但稀土在溶液中的富集程度随液固比的增加先增加后降低。最佳浸出条件为:溶液初始磷酸浓度25%、硫酸过量系数1.0、液固比6、反应温度75℃、反应时间3h、矿浆浓度58%,在此条件下,∑REO的总回收率达到68.01%,P2O5总的回收率达90%以上。     

磷酸浸出渣中提取稀土的研究

以湿法磷酸工艺中产生的非石膏类伴生稀土渣为原料、硫酸为浸出剂,考察硫酸浓度、反应温度和时间、液固比等对稀土浸出率的影响。结果表明,在下述综合试验条件下稀土浸出率可以达到81.9%:硫酸浓度14%、温度90℃、液固比4∶1、反应时间2h,硫酸浸出渣主要由石英、针状石膏和柱状石膏晶体组成。     

从蒸馏渣中回收稀土工艺研究

以稀土电解熔盐渣经矿相重构—真空蒸馏处理后的蒸馏渣为原料,采用盐酸酸浸提取蒸馏渣中的稀土,研究了酸浸时间、酸浸温度、盐酸浓度、液固比(L/S)对稀土和铁浸出率的影响。结果表明,在酸浸温度50℃、盐酸浓度4mol/L、酸浸时间1h、液固比4的较优工艺条件下,稀土浸出率高达99.88%,铁浸出率为44.43%,达到了稀土优先溶出的目的。     

织金稀土磷精矿的硫酸循环浸出

采用硫酸循环浸出稀土磷精矿,对磷酸溶液和石膏洗液中P2O5与稀土的富集以及浸出率的情况进行研究。结果表明:在硫酸过量系数为1.03,液固比3.5∶1,时间3h,温度75℃的浸出条件下,再经2次石膏洗涤后,磷酸溶液中P2O5的浓度可以富集到280g/L,ΣREO的浓度可以富集到340mg/L左右,P2O5和ΣREO的浸出率分别为92.46%和31.76%。     

从某稀土尾矿中回收稀土试验研究

研究了采用浸出—净化—沉淀工艺从某离子吸附型稀土尾矿中回收稀土,考察了硫酸质量浓度、浸出时间、浸出温度、液固体积质量比等因素对稀土浸出率的影响。结果表明:在浸出时间3h、硫酸质量浓度150g/L、浸出温度80℃、液固体积质量比3∶1条件下,稀土浸出率达96.44%。该方法对于从同类矿石中回收稀土有一定参考意义。     

超声波强化浸出高品位混合稀土精矿

针对目前混合稀土精矿提取稀土工艺过程中存在的稀土浸出率低、浸出时间长、产品纯度低、"三废"污染严重等问题,采用超声波强化浸出过程,利用化学分析、X射线衍射(XRD)等实验手段表征了酸浸过程中HCl浓度、固液比、酸浸时间、酸浸温度、超声频率对稀土提取过程的影响。实验结果表明:当HCl浓度为7 mol·L-1、固液比为1∶3.77、酸浸时间为50 min、酸浸温度为60℃、超声功率为70 W时,稀土浸出率和Ce浸出率可以达到64.01%和69.26%;稀土浸出率和Ce浸出率均比无超声波强化浸出分别提高了24.40%和26.91%;当反应时间延长至180 min,无超声波强化浸出的稀土浸出率和Ce浸出率与反应时间为50 min时的超声强化浸出基本相同,但超声强化浸出的反应时间相比无超声波强化浸出的反应时间却缩短了72.22%,超声波对于混合稀土精矿的浸出具有明显的强化作用。     

含铅锌渣中铅的富集

提出低酸—高酸两段逆流浸出含铅锌渣新工艺,低酸浸出考察液固比、时间和温度对锌浸出率的影响,高酸浸出考察初始硫酸浓度、时间和温度对锌浸出率及铅品位的影响。结果表明,在低酸浸出,液固比6∶1、时间5h、温度60℃;高酸浸出,初始硫酸浓度170g/L、时间6h、温度95℃的最优条件下,锌浸出率99.29%,铅入渣率98.58%,高浸渣中铅品位62.25%。     

高铁含锌烟尘浸出工艺研究

对锌烟尘硫酸浸出提取锌工艺条件进行了研究,分别采用正交试验与单因素试验考察浸出酸浓度、液固比、浸出时间、浸出温度对锌烟尘中锌、铁的浸出率的影响。结果表明:较优浸出工艺条件为硫酸浓度150 g/L、液固比7∶1、浸出时间3 h、浸出温度90℃,在较优浸出条件下,锌浸出率可达95%以上。     

氢氧化钠焙烧法提取稀土电解渣中稀土的工艺研究

针对目前从氟盐体系稀土熔盐电解渣中回收稀土效率低的问题,提出了一种NaOH焙烧-盐酸优溶浸出法。系统考察了焙烧温度、焙烧时间、NaOH添加量,以及盐酸浓度、液固比、浸出温度、浸出时间对渣中稀土提取效果的影响。结果表明:在焙烧温度600℃、焙烧时间1.5h、NaOH与稀土熔盐电解渣质量比0.8∶1、盐酸浓度2mol/L、液固比8∶1、浸出温度40℃、浸出时间15min的工艺条件下,稀土浸出率为99.22%。     

Simultaneous recovery of rare earth elements and phosphorus from phosphate rock by phosphoric acid leaching and selective precipitation:Towards green process

Phosphate rock has been considered as one of the potential promising resources for rare earth elements(REEs). But the cost issues and the technical challenges caused by the low content of REEs in ores did hinder the further development of REEs recovery technologies. In order to explore a green process for the recovery of REEs from phosphate rock, this study investigates the effects of phosphoric acid concentration, liquid-to-solid ratio(L/S ratio), leaching time and temperature on the leaching efficiencies of the major components from phosphate rock. A REEs recovery of 94.3% and a phosphorus recovery of 95.3%are achieved under the optimal conditions of attacking phosphate rock using 30%P_2 O_5 acid with an L/S ratio of 10:1 and a stirring speed of 250 r/min at 25 ℃ for 4 h. Then,the selective precipitation of REEs with 81.3% REEs recovery is realized by heating up the leaching solution from 25 to 90 ℃ and keeping for4 h. Thereafter, more than 95% phosphoric acid is recovered by H_2 SO_4 and high purity gypsum, more than95% CaSO_4(tested by XRF), is also produced at the same time. Ultimately, a green process that leaches phosphate rock with H_3 PO_4, selectively precipitates REEs from leaching solution by heating up, recovers H_3 PO_4 with H2 SO4 is proposed. Compared with REE recovery in traditional processes, this process owns the merits of simple operation, energy saving and minimum wastes.     

铅反射炉含铟烟尘氧压酸浸的研究

采用氧压酸浸技术对铅冶炼富铟烟尘进行浸出试验研究,详细考察了硫酸用量、氧分压、温度、液固比、时间、粒度等因素对铟浸出效果的影响,确定了氧压酸浸的最佳条件。结果表明,在下述最佳条件下:初始硫酸浓度180g/L、氧分压0.8MPa、温度150℃、液固比5∶1、时间120min、反应物粒度0.15～0.12mm,铟和锌的浸出率分别达到96.74%和99.19%,渣含铟小于0.02%。     

从废荧光粉中回收稀土的工艺研究

研究了从废荧光粉(REO^12.00%)中回收稀土元素的工艺。采用碳酸钠焙烧-酸浸出工艺回收废荧光粉中的稀土,研究了碳酸钠加入量、焙烧温度、焙烧时间以及浸出条件对稀土回收率的影响。研究结果表明,碳酸钠焙烧试验的最佳条件为碳酸钠与荧光粉焙烧比例1∶2,焙烧温度700℃,焙烧时间1 h;焙烧产物用盐酸浸出,浸出试验最佳条件:盐酸浓度、液固比、浸出温度、浸出时间分别为3 mol/L、10∶1、70℃、2 h,在上述焙烧及浸出最优条件下,稀土总回收率(REO)达97%以上。     

Recovering REEs from NdFeB wastes with high purity and efficiency by leaching and selective precipitation process with modified agents

A leaching and selective precipitation approach is proposed in this work to recover rare earth elements (REEs) from NdFeB magnet wastes collected from industry. Hydrochloric acid and oxalic acid were employed as the leaching and precipitation agents, respectively. Hexamethylenetetramine (HMTA) or tartaric acid was used as the chelating agent during leaching. Both leaching and precipitation processes were optimized individually. For leaching process, the effects of two different chelating agents, the concentrations of leaching agent, chelating agent, and temperature on the extraction and recovery yields were investigated. The optimized process based on the factorial experiment was determined to be the hydrochloric acid concentration of 6 mol/L, the tartaric acid concentration of 50 g/L, and the temperature of 313 K, by which the extraction yields of Fe and REEs up to 67.99% and 99.27%, respectively, are obtained. For the precipitation process, the optimized oxalic acid dosage and pH value were also determined. The produced RE oxide products have the purity and recovery yield up to 95.83% and 90.18%, respectively. These results indicate that the present method with low acid consumption and high product purity has advantages over many other approaches for REE recovery.     

Evaluating organic acids as alternative leaching reagents for rare earth elements recovery from NdFeB magnets

This study proposes an advanced leaching method using organic acids to recover rare earth elements (REEs) from NdFeB permanent magnets from end-of-life computers hard disk drives (HDDs). The end-of-life HDDs were first dismantled in order to recover NdFeB magnets, which were then thermally demagnetized at 350 °C during 30 min before crushing in a ball mill under inert atmosphere. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) analyses performed on the NdFeB magnets show the heterogeneous structure containing the major matric phase Nd₂Fe₁₄B and the REEs-rich phase containing Nd and Pr oxides. Additionally, X-ray diffraction (XRD) and Mössbauer spectroscopy (MS) analyses on the ground NdFeB magnet show that grinding NdFeB magnets under inert atmosphere helps to minimize its oxidation. Chemical analysis shows that the composition of the ground sample is Nd: 22.8 wt%, Pr: 3.3 wt%, Dy: 1.2 wt%, Fe: 62.6 wt%, Co: 1.5 wt%, B: 0.9 wt%, Ni: 0.6 wt%. Diagrams of speciation and equilibrium phases (E_h vs. pH) were calculated to determine the predominance of the formed species in the REEs–organic acids systems. The influence of the organic acid type (acetic acid, formic acid, citric acid and tartaric acid), the acid concentration (10 vol%, up to saturation), and the solid/liquid (S/L) ratio (0.5%–10%) on NdFeB magnets leaching was investigated employing an optimal experimental design conceived by the statistical software JMP. Acetic acid (CH₃COOH) shows the highest leaching performance of REEs, allowing leaching yields over 90% for Nd, Dy and Pr in the acid concentration range of 1.6–10 mol/L and the S/L ratio range of 0.5%–5% at a temperature of 60 °C. The results presented in this investigation suggest that REEs can be recovered from magnets of end-of-life HDDs using an eco-friendly method assisted by organic acids.     

某浮选铜精矿中铜、金浸出试验研究

在氯盐酸性体系中，对某浮选铜精矿进行了加压氧化浸铜的试验研究，探讨了温度、氧气分压、硫酸用量、氯化钠用量等对铜精矿中铜、铁浸出的影响。试验结果表明：在氧化温度110℃、氧分压0．45MPa、矿样粒度-0．043mm占85％、硫酸用量90g／L、氯化钠用量30g／L、液固比5／1、浸出时间2、5h、搅拌速度750r／min初始条件下，获得铜浸出率为92．18％。铜浸出渣经摇床重选脱硫，脱硫渣氰化浸金。当浮选精矿铜浸出率达到90％上时，对应渣中金的氰化浸出率都在96％以上。     

铜冶炼白烟尘综合回收研究

介绍了铜冶炼白烟尘在不同浸出体系下的浸出效果。结果表明,酸浸体系较水浸、碱浸体系效果更好。在H2SO4浓度2mol/L、液固比4:1、温度50℃、浸出时间2h、搅拌速度400r/min的最佳酸浸条件下,铜、锌、砷、镉和铁的浸出率分别为99.75%、99.81%、86.85%、95.85%和57.83%。采用铁粉置换-铁盐沉砷-中和沉锌镉的方法从酸浸液中回收Cu、As、Zn和Cd,在最优条件下,铜、砷、锌和镉回收率分别为99.70%、98.81%、99.47%和99.98%。     

废旧锂电池正极极片粉中钴的浸出

针对废旧钴酸锂电池正极极片中钴的回收,以破碎后的LiCoO2正极材料为原料,对比研究了LiCoO2在H2SO4和H2SO4+H2O2两种条件下钴的浸出效果。结果表明:正极极片粉中LiCoO2在H2SO4+H2O2作用下的还原浸出效果优于单独H2SO4浸出。在H2O2还原浸出条件下,在反应温度80℃、液固比6、初始硫酸浓度250g/L、双氧水加入量3%、反应120min的条件下,钴浸出率能达到95%以上。SEM分析显示,不规则多边形状的LiCoO2物象消失,表明LiCoO2已完全分解。     

废旧锂离子电池正极材料中钴铝同浸过程研究

通过基础热力学数据计算以及绘制反应体系的E-pH图,对废旧锂离子电池正极材料回收中钴铝同浸过程进行研究,考察了硫酸浓度、浸出时间、浸出温度、双氧水用量及液固比对钴、铝浸出率的影响。结果表明,在273K,-0.277相似文献