水热法合成立方形碳酸锰及其在提锂中的应用  

Preparation of cubic manganese carbonate by hydrothermal method and its application in extraction of lithium

作　　者：王瑞瑞 朱朝梁[1,2] 牟兵 马婉霞 樊洁 徐国旺[1,2] 史一飞 邓小川 卿彬菊[1,2] WANG Ruirui;ZHU Chaoliang;MU Bing;MA Wanxia;FAN Jie;XU Guowang;SHI Yifei;DENG Xiaochuan;QING Binju(Key Laboratory of Green and High-end Utilization of Salt Lake Resources,Qinghai Institute of Salt Lakes,Chinese Academy of Sciences,Xining 810008,China;Qinghai Engineering and Technology Research Center of Comprehensive Utiliza-tion of Salt Lake Resources,Xining 810008,China;University of Chinese Academy of Sciences,Beijing 100049,China)

机构地区：[1]中国科学院青海盐湖研究所,盐湖资源绿色高值利用重点实验室,青海西宁810008 [2]青海省盐湖资源综合利用工程技术中心,青海西宁810008 [3]中国科学院大学,北京100049

出　　处：《无机盐工业》2024年第12期94-103,共10页Inorganic Chemicals Industry

摘　　要：吸附剂的微观形貌对其在溶液中的分散及吸附行为有着显著影响,以水热法合成立方形MnCO_(3)作为自模板,制备形貌可控、粒径均一的锰系锂吸附剂。以KMnO_4、蔗糖、酒石酸为原料,考察了反应物浓度、溶液pH、水热温度、水热时间对水热产物立方形MnCO_(3)形貌及对应吸附剂的晶体结构、吸附量的影响。结果表明,水热法合成立方形MnCO_(3)的最佳工艺条件:反应物质量浓度为7.4062 g/L(以KMnO_4计),以LiOH·H_(2)O溶液作pH调节剂,调节反应溶液pH至3.00,水热温度为120℃,水热时间为36 h。最佳水热条件下对应立方形吸附剂对Li~+吸附量最高可达50.62 mg/g,在5次吸/脱附循环中吸附量稳定在38.50 mg/g以上、Li~+解吸率均在80%以上。利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、同步热分析仪(TGA-DSC)对最佳水热条件下制备的MnCO_(3)进行表征,结果表明,水热产物MnCO_(3)呈规则立方形结构,单个颗粒棱长约为8μm,颗粒之间分散性好且粒径均一,所含杂质较少,兼具有良好的热稳定性,是合成立方形锰系锂吸附剂的理想原料。The micromorphology of the adsorbent has a significant effect on its dispersion and adsorption behavior in solution.The manganous lithium adsorbent with controllable morphology and uniform particle size was prepared by hydrothermal synthesis of cubic MnCO_(3)as a selftemplate.Using potassium permanganate,sucrose,and tartaric acid as raw materials,the effects of reactant concentration,solution pH,hydrothermal temperature,and hydrothermal time on the morphology of cubic MnCO_(3)and the crystal structure and adsorption capacity of the corresponding adsorbent were investigated.The results showed that the optimum conditions for preparing cubic MnCO_(3)by the hydrothermal method were as follows:the optimal reactant concentration was 7.4062 g/L(in KMnO4),LiOH·H2O solution was used as pH regulator to adjust the pH of the reaction solution to 3.00,the hydrothermal temperature was 120℃and the hydrothermal time was 36 h.Under the optimal hydrothermal conditions,the maximum adsorption capacity of the corresponding C-HMO for Li^(+)was 50.62 mg/g,the adsorption capacity was stable above 38.50 mg/g and the desorption rate of Li^(+)was above 80%in 5 adsorptiondesorption cycles.X-ray diffractometer(XRD),scanning electron microscope(SEM),and synchronous thermal analyzer(TGA-DSC)were used to characterize the MnCO_(3)prepared under optimal hydrothermal conditions.The results showed that the hydrothermal product MnCO_(3)had a regular cubic structure,the single particle edge length was about 8μm,the dispersion between the particles was good,the particle size was uniform,the impurity was less,and it had good thermal stability,which was an ideal raw material for the formation of cubic manganese series lithium adsorbent.

关 键 词：水热法 立方形碳酸锰 锰系 锂吸附剂 

分 类 号：TQ131.11[化学工程—无机化工]