两例新的镧系金属-有机框架化合物高效去除Cs+离子研究※

doi:10.6023/A21120614

化学学报 ›› 2022, Vol. 80 ›› Issue (5): 640-646.DOI: 10.6023/A21120614 上一篇下一篇

所属专题：中国科学院青年创新促进会合辑

研究论文

两例新的镧系金属-有机框架化合物高效去除Cs⁺离子研究^※

吕天天^a^,^b, 马文^b, 詹冬笋^b, 邹燕敏^b, 李继龙^b, 冯美玲^b^,^*(), 黄小荥^b

a 中北大学材料科学与工程学院太原 030051
b 中国科学院福建物质结构研究所结构化学国家重点实验室福州 350002

投稿日期:2021-12-31 发布日期:2022-05-31
通讯作者: 冯美玲
作者简介:
^※庆祝中国科学院青年创新促进会十年华诞.
基金资助:
国家自然科学基金(U21A20296); 国家自然科学基金(22076185); 国家自然科学基金(21771183); 福建省自然科学基金(2020J06033)

Two New Three-Dimensional Lanthanide Metal-organic Frameworks for the Highly Efficient Removal of Cs⁺ Ions^※

Tiantian Lü^a^,^b, Wen Ma^b, Dongsun Zhan^b, Yanmin Zou^b, Jilong Li^b, Meiling Feng^b(), Xiaoying Huang^b

a College of Material Science and Engineering, North University of China, Taiyuan 030051
b State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002

Received:2021-12-31 Published:2022-05-31
Contact: Meiling Feng
About author:
^※Dedicated to the 10th anniversary of the Youth Innovation Promotion Association, CAS.
Supported by:
National Natural Science Foundation of China(U21A20296); National Natural Science Foundation of China(22076185); National Natural Science Foundation of China(21771183); Natural Science Foundation of Fujian Province(2020J06033)

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摘要/Abstract

¹³⁷Cs具有强放射性和较长半衰期, 一旦从核废液中泄露将对人类健康和环境造成很大危害. 由于¹³⁷Cs⁺的高溶解性、易迁移性和废液中干扰离子的影响, 从复杂的放射性废液中有效去除¹³⁷Cs⁺仍然是一个挑战. 本研究通过溶剂热法合成了两例新的三维微孔镧系金属-有机框架化合物(Me₂NH₂)_0.5(H₃O)_0.25Na_0.25Ln(OH)(stp)•0.25H₂O (FJSM-LnMOF; Ln=Eu, Tb; H₃stp=2-磺酸基对苯二甲酸), 它们具有良好的水稳定性和一定的耐酸碱性. FJSM-EuMOF和FJSM-TbMOF对Cs⁺离子吸附具有快速的动力学和高的吸附量(q_m^Cs分别为229.25和211.28 mg/g). 它们对Cs⁺离子具有良好的选择性(K_d^Cs值高达2.18×10³ mL/g). 即使在Na⁺, K⁺, Mg²⁺, Ca²⁺离子干扰的情况下, 它们仍然表现出对Cs⁺离子的选择性吸附性能. 我们成功获得了Cs⁺吸附产物的单晶结构, 通过单晶结构分析结合X射线光电子能谱(XPS), 红外(IR), 扫描电镜能量色散谱(EDS)和元素分析(EA)等多种表征方法, 证实了FJSM-EuMOF对Cs⁺离子的吸附为离子交换的机理. 结果表明, FJSM-EuMOF对Cs⁺离子的高效吸附主要源于镧系金属-有机阴离子框架中有机配体上的 COO^–和 $\text{SO}_{3}^{}$官能团对Cs⁺离子强的作用力以及通道内存在易交换的[Me₂NH₂]⁺阳离子和[H₃O]⁺离子. 这项工作表明, 镧系金属-有机框架化合物在放射性铯的修复中具有潜在的应用价值.

关键词: 镧系金属-有机框架, 晶体结构, 去除铯, 离子交换, 动力学, 吸附量, 选择性

¹³⁷Cs has the strong radioactivity and long half-life. In the event of leaking, it will pose a great danger to human health and the environment. The effective removal of ¹³⁷Cs⁺ from complex radioactive waste streams remains a challenge due to its high solubility, easy migration and the influence of interfering ions in the waste streams. In this study, two new three-dimensional microporous lanthanide metal-organic framework compounds (Me₂NH₂)_0.5(H₃O)_0.25Na_0.25Ln(OH)(stp)• 0.25H₂O (FJSM-LnMOF; Ln=Eu, Tb; H₃stp=2-sulfonic acid terephthalic acid) are synthesized by the solvothermal method, which have the good water stability and acid-base resistance. The adsorption performance of FJSM-LnMOFs for Cs⁺ are tested with solid-liquid ratio of 1∶1 under stirring at room temperature for 8 h. The adsorption kinetics of FJSM-EuMOF for Cs⁺ are tested with low-concentration Cs⁺ solution. FJSM-LnMOFs show fast kinetics and high adsorption capacities of Cs⁺ ions (the maximum adsorption capacities q_m^Cs of FJSM-EuMOF and FJSM-TbMOF are 229.25 and 211.28 mg/g, respectively). They have good selectivity for Cs⁺ ions (K_d^Cs value up to 2.18×10³ mL/g). Even in the presence of interfering Na⁺, K⁺, Mg²⁺, Ca²⁺ ions, they still show selective adsorption performance for Cs⁺ ions. Impressively, we successfully obtain the single crystal structure of Cs⁺-absorbed product by soaking FJSM-EuMOF crystals in 20,000 mg/L Cs⁺ solution, which confirms that the adsorption mechanism of Cs⁺ ions is ion exchange by the means of single crystal structure analysis combined with various characterization methods including X-ray photoelectron spectroscopy (XPS), infrared spectroscopy (IR), energy dispersion spectrum (EDS), elemental analysis (EA). The results indicate that the highly efficient Cs⁺ adsorption of FJSM-LnMOF mainly originates from the strong interactions between COO^– and $\text{SO}_{3}^{}$ functional groups from organic ligands and Cs⁺ ions, and the presence of easily exchangeable [Me₂NH₂]⁺ cations and [H₃O]⁺ located in the channels. This work indicates the potential application of lanthanide metal-organic frameworks in the remediation of radioactive cesium.

Key words: lanthanide-organic framework, crystal structure, removal of cesium, adsorption mechanism, ion exchange, kinetics, adsorption capacity, selectivity

引用此文

吕天天, 马文, 詹冬笋, 邹燕敏, 李继龙, 冯美玲, 黄小荥. 两例新的镧系金属-有机框架化合物高效去除Cs⁺离子研究^※[J]. 化学学报, 2022, 80(5): 640-646.

Tiantian Lü, Wen Ma, Dongsun Zhan, Yanmin Zou, Jilong Li, Meiling Feng, Xiaoying Huang. Two New Three-Dimensional Lanthanide Metal-organic Frameworks for the Highly Efficient Removal of Cs⁺ Ions^※[J]. Acta Chimica Sinica, 2022, 80(5): 640-646.

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图/表 4

图1. (a) FJSM-EuMOF和FJSM-EuMOF-Cs粉末和晶体照片. (b) FJSM-EuMOF及FJSM-EuMOF-Cs的模拟和实验PXRD图. (c) FJSM-EuMOF沿c轴方向的三维结构图. (d) FJSM-EuMOF-Cs沿c轴方向的三维结构图. (e) FJSM-EuMOF中的[Eu4]单元. (f) [Eu4]单元通过stp3–配体连接形成的沿着c轴延展的一维链

Figure 1. (a) Photographs of FJSM-EuMOF and FJSM-EuMOF-Cs powders and crystals. (b) Simulated and experimental PXRD patterns of FJSM-EuMOF and FJSM-EuMOF-Cs. (c) Three-dimensional structure of FJSM-EuMOF along the c-axis direction. (d) Three-dimensional structure of FJSM-EuMOF-Cs along the c-axis direction. (e) The [Eu4] unit in FJSM-EuMOF. (f) A one-dimensional chain along the c axis formed by interlinking [Eu4] units via stp3– ligands

图2. (a) FJSM-EuMOF吸收Cs+的动力学, 以CtCs (mg/L)(黑线)和RCs(%)(蓝线)与时间t (min)的关系绘制. (b)用准二阶动力学模型对FJSM-EuMOF的Cs+吸附动力学的拟合结果. 用Langmuir(蓝线)、Langmuir-Freundlich(红线)和Freundlich模型(黑线)拟合的FJSM-EuMOF (c)和FJSM-TbMOF (d)对Cs+的吸附等温线

Figure 2. (a) Kinetics of FJSM-EuMOF for Cs+ absorption plotted as CtCs (mg/L) (black line) and RCs (%) (blue line) vs. the time t (min). (b) The fitting results with pseudo-second-order kinetic model for the Cs+ absorption kinetics of FJSM-EuMOF. Adsorption isotherms of FJSM-EuMOF (c) and FJSM-TbMOF (d) for Cs+ fitted by Langmuir (blue line), Langmuir-Freundlich (red line) and Freundlich models (black line)

图3. (a) FJSM-EuMOF在不同初始pH值下的KdCs(柱状)和RCs(点图). (b) 在不同Na/Cs物质的量比情况下, FJSM-EuMOF的KdCs和KdNa. (c) FJSM-EuMOF在混合溶液1和溶液2中吸附各离子的Kd. (d) 在添加Cs+的自来水中FJSM-EuMOF吸附各离子的R

Figure 3. (a) KdCs (column) and RCs (line chart) values of FJSM-EuMOF at various initial pH values. (b) KdCs and KdNa of FJSM-EuMOF under the different molar ratios of Na/Cs. (c) Kd of FJSM-EuMOF for various metal ions in the solution 1 and solution 2. (d) R values of metal ion adsorbed by FJSM-EuMOF in tap water spiked with Cs+

图4. (a) FJSM-EuMOF-Cs的元素分布图. (b) FJSM-EuMOF和FJSM-EuMOF-Cs的XPS光谱. (c) FJSM-EuMOF-Cs中Cs的XPS光谱

Figure 4. (a) The elemental distribution mappings of FJSM-EuMOF-Cs. (b) XPS spectra of FJSM-EuMOF before and after Cs+ adsorption. (c) XPS of cesium for FJSM-EuMOF-Cs

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两例新的镧系金属-有机框架化合物高效去除Cs⁺离子研究^※

Two New Three-Dimensional Lanthanide Metal-organic Frameworks for the Highly Efficient Removal of Cs⁺ Ions^※

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两例新的镧系金属-有机框架化合物高效去除Cs+离子研究※

Two New Three-Dimensional Lanthanide Metal-organic Frameworks for the Highly Efficient Removal of Cs+ Ions※

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两例新的镧系金属-有机框架化合物高效去除Cs⁺离子研究^※

Two New Three-Dimensional Lanthanide Metal-organic Frameworks for the Highly Efficient Removal of Cs⁺ Ions^※