微反应器中Ce2O(CO3)2·H2O前驱体的合成及CeO2的制备研究  

Synthesis of Cerium Oxide Carbonate Hydrate Precursor in Microreactor and Preparation of Ceria

作　　者：罗尧尧 王天 刘秉国[1] 张利波[1] 张利华[1] Luo Yaoyao;Wang Tian;Liu Bingguo;Zhang Libo;Zhang Lihua(State Key Laboratory of Complex Nonferrous Metal Resources Clean Utilization,Key Laboratory of Unconventional Metallurgy,Ministry of Education,Faculty of Metallurgical and Energy Engineering,Kunming University of Science and Technology,Kunming 650093,China)

机构地区：[1]省部共建复杂有色金属资源清洁利用国家重点实验室,非常规冶金教育部重点实验室,昆明理工大学冶金与能源工程学院,云南昆明650093

出　　处：《中国稀土学报》2020年第4期474-482,I0001,共10页Journal of the Chinese Society of Rare Earths

基　　金：国家自然科学基金项目(51404116);昆明理工大学人才培养项目(KKZ3201852050)资助。

摘　　要：以Ce(NO3)3和NH4HCO3为原料,在微反应器中采用液-液沉淀法制备出水合碳酸氧铈(Ce2O(CO3)2·H2O)前驱体材料,将前驱体样品进行热处理后获得纯净的CeO2产品。分别采用电感耦合等离子体质谱仪(ICP-MS)、X射线衍射仪(XRD)、场发射扫描电镜(FESEM)和能谱分析仪(EDS)、热重-差热分析仪(TG-DTA)等对制备的前驱体和热解产品进行分析表征。结果表明:微反应器内23.6 s的停留时间,Ce^3+在不同反应温度下均可达到99.8%以上的沉淀率。反应温度为70℃及以上时,获得结晶度更好的Ce2O(CO3)2·H2O前驱体,为类六棱形片叠加的花瓣状规则形貌,粒径较小。此前驱体样品在600℃下热处理2 h后制备得到了纯净单一的立方晶系CeO2产品,无其他杂质,形貌与Ce2O(CO3)2·H2O前驱体一致。The sample of cerium oxide carbonate hydrate precursor were synthesized by liquid precipitation method in the microreactor using Ce(NO3)3 and NH4HCO3 as raw materials,then pure ceria products were obtained from the precursor after heat treatment.The synthesized precursor and product were characterized by ICP-MS,X-ray diffraction(XRD),FESEM,EDS,and TG-DTA.The results showed that with 23.6 s residence time in the microreactor,above 99.8%of Ce^3+was precipitated from aqueous solutions at different reaction temperatures.When the reaction temperature was over 70℃,Ce2O(CO3)2·H2O precursor with better crystallinity was obtained,and the morphology was regular hexarhombic sheets superimposed as petals with small size distribution.Then,the precursor synthesized at 70℃was heated at 600℃with 2 h,and pure cubic CeO2 product was obtained.The morphology of CeO2 was the same as that of Ce2O(CO3)2·H2O precursor.

关 键 词：微反应器 液相沉淀 Ce2O(CO3)2·H2O 前驱体 CEO2 

分 类 号：TQ113.21[化学工程—无机化工]