钕铁硼废料焙砂的碳热还原试验研究
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摘要
钕铁硼废料中含有大量的铁,现有回转窑焙烧-HCl浸出预处理工艺难于将其回收利用。基于稀土氧化物和铁氧化物还原性质差异,以钕铁硼废料焙烧产物(简称为焙砂)为对象,在高温井式窑炉中开展焙砂碳热还原试验研究,考察了还原介质(焦炭、石墨和块煤)、介质粒度、还原温度、还原时间、配碳比、物料厚度等条件对铁还原率的影响。结果表明,焦炭具有较好的还原效果,在还原温度为1200℃,还原时间为4 h,配碳比为30%,物料厚度为22 mm的条件下,焙砂中铁的还原度高达88.08%,为综合回收利用钕铁硼废料中铁资源提供了理论基础和方法途径。
A large amount of iron contains in NdFeB scrap which is difficult to be recycled in the existing rotary kiln roasting-hydrochloric acid leaching pretreatment. Based on the difference reduction properties of rare earth oxide and iron oxide, calcination of neodymium iron boron scrap(abbreviated as calcine) was carried out in a high-temperature well-type kiln to investigate the effect of reducing medium(coke, graphite and lump coal), media particle size, reduction temperature, reduction time, carbon ratio, material thickness and other conditions on the iron reduction rate. The results showed that the coke has a good reduction effect. Under the conditions of reduction temperature of 1200 ℃, reduction time of 4 h, carbon ration of 30% and total mass of 50 g, the reduction degree of iron in calcine is up to 88.08%. It provides a theoretical basis and method approaches for the comprehensive recovery and utilization of iron resources of NdFeB scrap.
A large amount of iron contains in NdFeB scrap which is difficult to be recycled in the existing rotary kiln roasting-hydrochloric acid leaching pretreatment. Based on the difference reduction properties of rare earth oxide and iron oxide, calcination of neodymium iron boron scrap(abbreviated as calcine) was carried out in a high-temperature well-type kiln to investigate the effect of reducing medium(coke, graphite and lump coal), media particle size, reduction temperature, reduction time, carbon ratio, material thickness and other conditions on the iron reduction rate. The results showed that the coke has a good reduction effect. Under the conditions of reduction temperature of 1200 ℃, reduction time of 4 h, carbon ration of 30% and total mass of 50 g, the reduction degree of iron in calcine is up to 88.08%. It provides a theoretical basis and method approaches for the comprehensive recovery and utilization of iron resources of NdFeB scrap.
引文
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[11] 林河成. 用钕铁硼废料制取氧化钕的研究 [J]. 稀有金属与硬质合金, 1997, (3): 4.Lin H C. Preparation of Nd_2O_3 from NdFeB scraps [J]. Rare Metals and Cemented Carbide, 1997, (3): 4.
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[13] 王建英, 杜继宇, 张雪峰. 从白云鄂博稀土尾矿回收铁的新工艺 [J]. 中国稀土学报, 2017, 35(3): 413.Wang J Y, Du J Y, Zhang X F. A new method for recovery of iron from Bayan Obo tailing [J]. Journal of the Chinese Society of Rare Earths, 2017, 35(3): 413.
[14] 王常珍, 杨代银. 炉渣中稀土氧化物活度的测定 [J]. 金属学报, 1979, 15(3): 433.Wang C Z, Yang D Y. Determination of the activity of RE_2O_3 in liquid RE_2O_3-CaF_2 and RE_2O_3-CaO- CaF_2 slags [J]. Acta Metallurgica Sinica, 1979, 15(3): 433.
[15] 赵世喆. 稀土氧化物直接还原制备含稀土AZ31镁合金组织及性能的研究 [D]. 长春: 吉林大学, 2016.Zhao S Z. Study on Microstructure and Properties of AZ31 Magnesium Alloy Containing RE by Direct Reduction with Rare Earth Oxides [D]. Changchun: Jilin University, 2016.
[16] 姜银举, 郭海涛, 解萍, 焦伟利, 徐掌印. 氧化铈熔盐电解过程预还原反应的冶金热力学分析 [J]. 稀土, 2010, 31(2): 28.Jiang Y J, Guo H T, Xie P, Jiao W L, Xu Z Y. Thermodynamics analysis of pre-reduction reaction of cerium oxide in fused-salt electrolysis process [J]. Chinese Rare Earths, 2010, 31(2): 28.
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[2] 吴继平, 邓庚凤, 邓亮亮, 林程星, 潘贤斌. 从钕铁硼废料中提取稀土工艺研究 [J]. 有色金属科学与工程, 2016, 7(1): 119.Wu J P, Deng G F, Deng L L, Lin C X, Pan X B. Rare earth recovery from NdFeB magnet scrap [J]. Nonferrous Metals Science and Engineering, 2016, 7(1): 119.
[3] 许涛, 张翼明. 钕铁硼磁性材料废料的综合利用 [A]. 第十一届全国稀土分析化学学术报告会论文集 [C]. 海口, 2006. 16.Xu T, Zhang Y M. Comprehensive utilization of waste NdFeB magnetic material [A]. Eleventh National Conference on Rare Earth Analytical Chemistry Proceedings [C]. Haikou, 2006. 16.
[4] 刘志强, 陈怀杰. 从NdFeB磁体废料中回收稀土的工艺 [J]. 材料研究与应用, 2009, (2): 134.Liu Z Q, Chen H J. The industrial practice of recycling rare earth from NdFeB scraps [J]. Materials Research and Application, 2009, (2): 134.
[5] 刘名清. NdFeB废渣中回收稀土的探讨 [J]. 科技资讯, 2009, (21): 131.Liu M Q. Discussion on recovery of rare earths from NdFeB waste [J]. Science & Technology Information, 2009, (21): 131.
[6] 黄劲松, 齐关富. 钕铁硼废料资源化利用工艺综述 [J]. 中国资源综合利用, 2008, 26(11): 4.Huang J S, Qi G F. Review on recovery technology of NdFeB waste materials [J]. China Resources Comprehensive Utilization, 2008, 26(11): 4.
[7] 王毅军, 刘宇辉, 翁国庆, 李四勇, 刘荣丽, 王素玲. 盐酸优溶法回收NdFeB废料中稀土元素的研究与生产 [J]. 稀有金属与硬质合金, 2007, 35(2): 25.Wang Y J, Liu Y H, Weng G Q, Li S Y, Liu R L, Wang S L. Study and practice of selective dissolution with HCl for the recovery of RE elements from NdFeB scrap [J]. Rare Metals and Cemented Carbides, 2007, 35(2): 25.
[8] 陈云锦. 全萃取法回收钕铁硼废渣中的稀土与钴 [J]. 中国资源综合利用, 2004, (6): 10.Chen Y J. Recovery of rare earths and cobalt in NdFeB waste by full extraction [J]. Comprehensive Utilization of China Resources, 2004, (6): 10.
[9] 尹小文, 刘敏, 赖伟鸿, 董传博, 岳明, 索红莉. 草酸盐沉淀法回收钕铁硼废料中稀土元素的研究 [J]. 稀有金属, 2014, 38(6): 1093.Yin X W, Liu M, Lai W H, Dong C H, Yue M, Suo H L. Recycle rare earth elements from NdFeB waste with oxalate precipitation method [J]. Chinese Journal of Rare Metals, 2014, 38(6): 1093.
[10] 陈玉凤, 林宝启, 黎先财. 从钕铁硼废料中提取氧化钕 [J]. 无机盐工业, 2001, 33(3): 37.Chen Y F, Liu B Q, Li X C. Extracting neodymium oxide from the NdFeB waste [J]. Inorganic Chemicals Industry, 2001, 33(3): 37.
[11] 林河成. 用钕铁硼废料制取氧化钕的研究 [J]. 稀有金属与硬质合金, 1997, (3): 4.Lin H C. Preparation of Nd_2O_3 from NdFeB scraps [J]. Rare Metals and Cemented Carbide, 1997, (3): 4.
[12] 李来超, 张榕贵, 余煜玺. 从掺钕钇铝石榴石晶体中回收稀土 [J]. 中国稀土学报, 2017, 35(2): 225.Li L C, Zhang R Q, Yu Y X. Recovery of rare earth from scrapped Nd:YAG crystal [J]. Journal of the Chinese Society of Rare Earths, 2017, 35(2): 225.
[13] 王建英, 杜继宇, 张雪峰. 从白云鄂博稀土尾矿回收铁的新工艺 [J]. 中国稀土学报, 2017, 35(3): 413.Wang J Y, Du J Y, Zhang X F. A new method for recovery of iron from Bayan Obo tailing [J]. Journal of the Chinese Society of Rare Earths, 2017, 35(3): 413.
[14] 王常珍, 杨代银. 炉渣中稀土氧化物活度的测定 [J]. 金属学报, 1979, 15(3): 433.Wang C Z, Yang D Y. Determination of the activity of RE_2O_3 in liquid RE_2O_3-CaF_2 and RE_2O_3-CaO- CaF_2 slags [J]. Acta Metallurgica Sinica, 1979, 15(3): 433.
[15] 赵世喆. 稀土氧化物直接还原制备含稀土AZ31镁合金组织及性能的研究 [D]. 长春: 吉林大学, 2016.Zhao S Z. Study on Microstructure and Properties of AZ31 Magnesium Alloy Containing RE by Direct Reduction with Rare Earth Oxides [D]. Changchun: Jilin University, 2016.
[16] 姜银举, 郭海涛, 解萍, 焦伟利, 徐掌印. 氧化铈熔盐电解过程预还原反应的冶金热力学分析 [J]. 稀土, 2010, 31(2): 28.Jiang Y J, Guo H T, Xie P, Jiao W L, Xu Z Y. Thermodynamics analysis of pre-reduction reaction of cerium oxide in fused-salt electrolysis process [J]. Chinese Rare Earths, 2010, 31(2): 28.
[17] 朱苗勇. 现代冶金学 [M]. 北京: 冶金工业出版社, 2005.Zhu M Y. Xian Dai Ye Jin Xue [M]. Beijing: Metallurgical Industry Press, 2005.
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