Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, Chinese Academy of Geological SciencesHost
2022 Vol. 42, No. 1
Article Contents

ZHAI Jingyu, LIU Guangyi. The Leaching Technology of Rare Earth Polishing Powder Waste in Thiourea-Hydrochloric Acid System and Recovery of Rare Earth Oxides from the Lixivium Through Oxalic Acid Precipitation[J]. Conservation and Utilization of Mineral Resources, 2022, 42(1): 158-164. doi: 10.13779/j.cnki.issn1001-0076.2022.01.023
Citation: ZHAI Jingyu, LIU Guangyi. The Leaching Technology of Rare Earth Polishing Powder Waste in Thiourea-Hydrochloric Acid System and Recovery of Rare Earth Oxides from the Lixivium Through Oxalic Acid Precipitation[J]. Conservation and Utilization of Mineral Resources, 2022, 42(1): 158-164. doi: 10.13779/j.cnki.issn1001-0076.2022.01.023

The Leaching Technology of Rare Earth Polishing Powder Waste in Thiourea-Hydrochloric Acid System and Recovery of Rare Earth Oxides from the Lixivium Through Oxalic Acid Precipitation

More Information
  • The solubility of Ce(Ⅲ) is far greater than that of Ce(Ⅳ). Thus, the thiourea was used to reduce Ce(Ⅳ) into Ce(Ⅲ) in dilute hydrochloric acid solutions to promote the recovery of rare earth oxides from a rare earth polishing powder waste. The effects of leaching temperature, leaching time, liquid-to-solid ratio (L/S), hydrochloric acid concentration and thiourea dosage on the leaching ratio of cerium from the rare earth polishing powder waste were investigated. The results showed that under the optimal technologies, hydrochloric acid concentration of 4 mol/L, L/S of 4.2, leaching temperature of 90 ℃, leaching time of 60 min, and thiourea dosage of 0.04 g/g, the cerium leaching ratio reached 99.37%. Then, the rare earth ions in leaching solutions were separated and recovered by oxalic acid precipitation approach. After adjusting pH to 1.8-2.0 by ammonia water, oxalic acid was added to deliver rare earth oxalate precipitates which were subsequently roasted under air to obtain the rare earth oxide (REO) product. The total REO content in the REO product was about 97% with 78.00% CeO2 and 18.93% La2O3, and their recovery ratio was 91.66% and 68.44%, respectively. In addition, the findings of laser particle size analysis, XRD and SEM showed that the rare earth oxide products were mainly composed by CeO2 square particles, and exhibited a narrow particle size distribution with a flat and angular surface.

  • 加载中
  • [1] BORRA C, VLUGT T, YANG Y, et al. Recovery of cerium from glass polishing waste: A critical review[J]. Metals, 2018, 8(10): 801-817. doi: 10.3390/met8100801

    CrossRef Google Scholar

    [2] UM N, HIRATO T. A hydrometallurgical method of energy saving type for separation of rare earth elements from rare earth polishing powder wastes with middle fraction of ceria[J]. Journal of Rare Earths, 2016, 34(5): 536-542. doi: 10.1016/S1002-0721(16)60059-5

    CrossRef Google Scholar

    [3] 罗天纵, 吴希桃, 包新军, 等. 废弃稀土抛光粉回收再利用研究进展[J]. 稀土, 2020, 41(3): 95-104.

    Google Scholar

    LUO T Z, WU X T, BAO X J, et al. Research process in recovering and reutilizing of rare earth polishing powder wastes[J]. Chinese Rare Earths, 2020, 41(3): 95-104.

    Google Scholar

    [4] OH M, NHO J, CHO S, et al. Polishing behaviors of ceria abrasives on silicon dioxide and silicon nitride CMP[J]. Powder Technology, 2011, 206(3): 239-245. doi: 10.1016/j.powtec.2010.09.025

    CrossRef Google Scholar

    [5] BINNEMANS K, JONES P T, BLANPAIN B, et al. Recycling of rare earths: a critical review[J]. Journal of Cleaner Production, 2013, 51: 1-22. doi: 10.1016/j.jclepro.2012.12.037

    CrossRef Google Scholar

    [6] MESHRAM P, ABHILASH. Recovery and recycling of cerium from primary and secondary resources- a critical review[J]. Mineral Processing and Extractive Metallurgy Review, 2020, 41(4): 279-310. doi: 10.1080/08827508.2019.1677647

    CrossRef Google Scholar

    [7] 李振民, 王勇, 牛京考. 中国稀土资源开发的生态环境影响及维护政策[J]. 稀土, 2017, 38(6): 144-154.

    Google Scholar

    LI Z M, WANG Y, NIU J K. The influence of rare earth resources exploitation on ecology and environment and the protection plicy[J]. Chinese Rare Earths, 2017, 38(6): 144-154.

    Google Scholar

    [8] TING M H, SEAMAN J. Rare earths: future elements of conflict in asia[J]. Asian Studies Review, 2013, 37(2): 234-252. doi: 10.1080/10357823.2013.767313

    CrossRef Google Scholar

    [9] 涂雅洁. 废弃稀土抛光渣梯级循环利用的研究[D]. 武汉: 武汉理工大学, 2012.

    Google Scholar

    TU Y J. The study for step recycling of easte rare earth polishing powder[D]. Wuhan: Wuhan University of Technology, 2012.

    Google Scholar

    [10] KIM J, KIM U, BYEON M, et al. Recovery of cerium from glass polishing slurry[J]. Journal of Rare Earths, 2011, 29(11): 1075-1078. doi: 10.1016/S1002-0721(10)60601-1

    CrossRef Google Scholar

    [11] WANG L, LIU P, CHEN Y. Recovery of cerium oxide abrasive from an abrasive-glass polishing waste through alkaline roasting followed by water leaching[J]. Metals, 2020, 10(6): 752-767. doi: 10.3390/met10060752

    CrossRef Google Scholar

    [12] 刘晓杰, 于亚辉, 许涛, 等. 碱焙烧法从稀土抛光粉废渣中回收稀土[J]. 稀土, 2015, 36(4): 75-80.

    Google Scholar

    LIU X J, YU Y H, XU T, et al. Recovery of RE from waste RE polishing powder by Alkali roasting[J]. Chinese Rare Earths, 2015, 36(4): 75-80.

    Google Scholar

    [13] ZOU D, LI H, DENG Y, et al. Recovery of lanthanum and cerium from rare earth polishing powder wastes utilizing acid baking-water leaching-precipitation process[J]. Separation and Purification Technology, 2021, 261: 118244. doi: 10.1016/j.seppur.2020.118244

    CrossRef Google Scholar

    [14] 罗磊. 从废弃稀土抛光粉中回收稀土金属的工艺条件研究[D]. 合肥: 合肥工业大学, 2015.

    Google Scholar

    LUO L. Technological conditions of recovering rare earth metals from an abandoned rare earth polishing power[D]. Hefei: Hefei University of Technology, 2015.

    Google Scholar

    [15] POSCHER A, LUIDOLD S, ANTREKOWITSCH H. Extraction of cerium and lanthanum from spent glass polishing agent: rare earth elements symposium[C]. Montreal, 2013.

    Google Scholar

    [16] JANOŠ P, KURÁÑ P, EDERER J, et al. Recovery of cerium dioxide from spent glass-polishing slurry and its utilization as a reactive sorbent for fast degradation of toxic organophosphates[J]. Advances in Materials Science and Engineering, 2015(22): 1-8.

    Google Scholar

    [17] LU S, SUN S, HUANG X, et al. Optimization of recovering cerium from the waste polishing powder using response surface methodology[J]. Green Processing and Synthesis, 2017, 6(2): 217-224.

    Google Scholar

    [18] JING-YING L, XIU-LI X, WEN-QUAN L. Thiourea leaching gold and silver from the printed circuit boards of waste mobile phones[J]. Waste Management, 2012, 32(6): 1209-1212. doi: 10.1016/j.wasman.2012.01.026

    CrossRef Google Scholar

    [19] SADRI F, RASHCHI F, AMINI A. Hydrometallurgical digestion and leaching of Iranian monazite concentrate containing rare earth elements Th, Ce, La and Nd[J]. International Journal of Mineral Processing, 2017, 159: 7-15. doi: 10.1016/j.minpro.2016.12.003

    CrossRef Google Scholar

    [20] 全国稀土标准化技术委员会. 稀土抛光粉化学分析方法第1部分: 氧化铈量的测定滴定法[S]. 北京: 中国标准出版社, 2012.

    Google Scholar

    National rare earth standardization technical committee. GB/T 20166.1-2012, Chemical analysis methods of rare earth polishing powder-Part1: Determination of cerium oxide content-Titrimetry[S]. Beijing: China Standard Press, 2012.

    Google Scholar

    [21] 赵林治, 杨书廷. 硫脲稳定性研究[J]. 河南师范大学学报(自然科学版), 1992(1): 98-102.

    Google Scholar

    ZHAO L Z, YANG S T. Study on the stability of thiourea[J]. Journal of Henan Normal University (Natural Science), 1992(1): 98-102.

    Google Scholar

    [22] CALLA-CHOQUE D, LAPIDUS G T. Acid decomposition and silver leaching with thiourea and oxalate from an industrial jarosite sample[J]. Hydrometallurgy, 2020, 192: 105289. doi: 10.1016/j.hydromet.2020.105289

    CrossRef Google Scholar

    [23] GABAL M A, ELROBY S A K, OBAID A Y. Synthesis and characterization of nano-sized ceria powder via oxalate decomposition route[J]. Powder Technology, 2012, 229: 112-118. doi: 10.1016/j.powtec.2012.06.017

    CrossRef Google Scholar

    [24] 李梅, 杨来东, 柳召刚, 等. 粒度及粒度分布对铈基稀土抛光粉性能影响的研究[J]. 稀土, 2016, 37(4): 144-147.

    Google Scholar

    LIM, YANG L D, LIU Z G, et al. The study of the ipact of particle size and particle size distribution of the Ce-based rare earth polishing powder on its performance[J]. Chinese Rare Earths, 2016, 37(4): 144-147.

    Google Scholar

    [25] YU B, JIANG J, YANG C. Conversion of lanthanum and cerium recovered from hazardous waste polishing powders to hazardous ammonia decomposition catalysts[J]. Journal of Hazardous Materials, 2019, 379: 120773. doi: 10.1016/j.jhazmat.2019.120773

    CrossRef Google Scholar

    [26] 周筱桐, 肖汉宁, 刘井雄, 等. 草酸沉淀法制备稀土抛光粉及其抛光性能[J]. 机械工程材料, 2014, 38(8): 57-60.

    Google Scholar

    ZHOU X T, XIAO H N, LIU J X, et al. Preparation of polishing powders by oxalate deposition and its polishing performance[J]. Materials of Mechanical Engineering, 2014, 38(8): 57-60.

    Google Scholar

    [27] ZHAN G, YU J, XU Z, et al. Kinetics of thermal decomposition of lanthanum oxalate hydrate[J]. Transactions of Nonferrous Metals Society of China, 2012, 22(4): 925-934. doi: 10.1016/S1003-6326(11)61266-1

    CrossRef Google Scholar

    [28] ANJANEYA K C, NAYAKA G P, MANJANNA J, et al. Studies on structural, morphological and electrical properties of Ce0.8Ln0.2O2-δ (Ln=Y3+, Gd3+, SM3+, Nd3+ and La3+) solid solutions prepared by citrate complexation method[J]. Journal of Alloys and Compounds, 2014, 585: 594-601. doi: 10.1016/j.jallcom.2013.09.101

    CrossRef Google Scholar

  • 加载中
通讯作者: 陈斌, bchen63@163.com
  • 1. 

    沈阳化工大学材料科学与工程学院 沈阳 110142

  1. 本站搜索
  2. 百度学术搜索
  3. 万方数据库搜索
  4. CNKI搜索

Figures(11)

Tables(2)

Article Metrics

Article views(1727) PDF downloads(124) Cited by(0)

Access History

Other Articles By Authors

Catalog

    /

    DownLoad:  Full-Size Img  PowerPoint