二维金属-有机骨架膜的制备及其在分离中的应用

doi:10.6023/A21030099

化学学报 ›› 2021, Vol. 79 ›› Issue (7): 869-884.DOI: 10.6023/A21030099 上一篇下一篇

所属专题：多孔材料：金属有机框架(MOF)

综述

二维金属-有机骨架膜的制备及其在分离中的应用

吕露茜^a, 赵娅俐^a, 魏嫣莹^a^,^*(), 王海辉^b^,^*()

a 华南理工大学化学与化工学院广州 510640
b 清华大学化学工程系北京 100084

投稿日期:2021-03-19 发布日期:2021-06-21
通讯作者: 魏嫣莹, 王海辉

作者简介:

吕露茜, 2019年本科毕业于华南理工大学, 目前在华南理工大学化学与化工学院魏嫣莹老师膜科学与能源材料研究组开展研究工作, 研究方向是金属-有机骨架材料应用于气体分离.

赵娅俐, 2018年本科毕业于湖南工程大学, 目前在华南理工大学化学与化工学院魏嫣莹老师膜科学与能源材料研究组开展研究工作, 研究方向是金属-有机骨架膜应用于分离.

魏嫣莹, 女, 华南理工大学化学与化工学院研究员. 2008年本科毕业于太原理工大学, 2013年博士毕业于华南理工大学. 2015年加入华南理工大学化学与化工学院王海辉老师课题组, 开展研究. 研究方向为无机膜分离(二维膜、MOF膜、混合导体膜)和催化膜反应器. 在国际化学、化工领域权威期刊发表SCI论文65篇, 第一或通讯作者身份发表42篇. 合作申请中国发明专利33项, 授权11项.

王海辉, 男, 清华大学化学工程系教授. 1998年本科毕业于安徽工业大学, 2003年博士毕业于中国科学院大连化学物理研究所. 2013年加入华南理工大学化学与化工学院, 成立膜科学与能源材料研究组, 开展研究. 2021年入职清华大学化工系. 研究方向为膜分离与膜催化, 新能源与器件. 在国际化学、化工领域权威期刊发表SCI论文220余篇, 论文被引用16400余次, H因子: 67. 申请中国发明专利50余件, 获得授权28件, 欧洲专利2件, 授权1件.

基金资助:
国家自然科学基金(22022805); 国家自然科学基金(22078107)

Preparation of Two-Dimensional Metal-Organic Framework Membranes and Their Applications in Separation

Luxi Lyu^a, Yali Zhao^a, Yanying Wei^a(), Haihui Wang^b()

a School of Chemistry & Chemical Engineering, South China University of Technology, Guangzhou 510640, China
b Department of Chemical Engineering, Tsinghua University, Beijing 100084, China

Received:2021-03-19 Published:2021-06-21
Contact: Yanying Wei, Haihui Wang
Supported by:
National Natural Science Foundation of China(22022805); National Natural Science Foundation of China(22078107)

文章分享

摘要/Abstract

膜分离在面向能源与环境问题的分离过程中具有极大的应用前景, 近几十年内发展迅速. 金属-有机骨架(MOFs)是一种新型微孔材料, 具有孔结构均一、可调控、多样化的特点, 用其制备的MOF膜在分离领域极具应用潜力. 而二维(2D)材料的飞速发展, 使2D MOF膜也成为倍受关注的一类新型分离膜. 由2D MOF纳米片构筑成的超薄分离膜, 通过MOF的固有孔径可以实现分子级别的筛分, 而纳米片之间的通道及纳米片面内通道为气体或水分子提供了更多的传质通道, 从而实现了优异的分离性能. 因此, 2D MOF膜被认为有望同时提高分离过程的渗透量和选择性, 成为满足工业分离需求的高性能分离膜.

关键词: 膜分离, 金属-有机骨架, 二维膜, 纳米片

Membrane separation is very promising in solving energy and environmental challenges of separation process, and it has developed rapidly in recent decades. Metal-organic frameworks (MOFs) are a new type of microporous material with adjustable pores with uniform size, thus MOF membranes show promising potential for separation applications. With the rapid development of two-dimensional (2D) materials, 2D MOF membranes constructed with 2D MOF nanosheets, have attracted increasing attentions, where the pores of MOF could achieve molecular sieving, while both the nanochannels between the nanosheets and the pores of MOF nanosheets would provide mass transfer pathway for fast permeation. Therefore, 2D MOF membranes are expected to show both high permeability and selectivity, which might become a kind of high-performance membrane for industrial separations.

Key words: membrane separation, metal-organic framework, two-dimensional membrane, nanosheet

引用此文

吕露茜, 赵娅俐, 魏嫣莹, 王海辉. 二维金属-有机骨架膜的制备及其在分离中的应用[J]. 化学学报, 2021, 79(7): 869-884.

Luxi Lyu, Yali Zhao, Yanying Wei, Haihui Wang. Preparation of Two-Dimensional Metal-Organic Framework Membranes and Their Applications in Separation[J]. Acta Chimica Sinica, 2021, 79(7): 869-884.

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图/表 23

图1. 膜分离机理示意图[2]: (i) Knudson扩散; (ii) 表面扩散; (iii) 毛细管凝结; (iv) 分子筛和(v) 溶解扩散

Figure 1. Illustration of membrane separation mechanisms[2]: (i) Knudson diffusion; (ii) surface diffusion; (iii) capillary condensation; (iv) molecular sieving and (v) solution diffusion

图2. (a) 石墨烯晶体结构示意图[21]; (b) h-BN结构示意图[26]; (c) s-三嗪(左)和反-s-三嗪(右)的C3N4示意图[29], 蓝色和灰色的球分别代表氮和碳原子

Figure 2. (a) Schematics of the crystal structure of graphene[21]; (b) the illustration of h-BN structure[26]; (c) scheme of s-triazine (left) and tri-s-triazine (right) based connection in g-C3N4[29]. Blue and gray spheres represent nitrogen and carbon atoms

图3. [Cu2Br(IN)2]n (a)单层结构图; (b) 沿a轴的结构图; (c) 沉积在热解石墨(HOPG)上的纳米片AFM图, 插图为(c)中绿线的轮廓高度[53]. (d) 石墨烯浓度与溶剂表面能的关系. 插图显示了NMP(左)和DMF(右)的结构[56]

Figure 3. (a) View of a single layer framework of [Cu2Br(IN)2]n; (b) superposition of layers along the a axis of [Cu2Br(IN)2]n; (c) AFM topography image of [Cu2Br(IN)2]n nanosheets deposited on highly oriented pyrolytic graphite (HOPG), illustration shows height of profile across the green line in (c)[53]. (d) Dispersed graphene concentration as a function of solvent surface energy. Insets show the structures of NMP (left) and DMF (right)[56]

图4. (a) 上: Zn2(bim)3前体沿c轴的堆积图; 下: 层状前体Zn2(bim)3的扫描电子显微镜(SEM)图像. 剥离过程中显示的小分子代表甲醇和正丙醇; (b) 上: 分散在甲醇/正丙醇混合溶剂中的Zn2(bim)3纳米片; 下: Zn2(bim)3纳米片的透射电子显微镜(TEM)图像[58]

Figure 4. (a) Top: stacking diagram of Zn2(bim)3 precursors along c-axis; bottom: scanning electron microscope (SEM) image of the layered Zn2(bim)3 precursors. The small molecules shown in the exfoliation process represent the methanol and n-propanol; (b) top: Zn2(bim)3 nanosheets dispersed in methanol/n-propanol mixture; bottom: transmission electron microscope (TEM) image of Zn2(bim)3 nanosheets[58]

图5. (a) 冻融法剥离氧化石墨烯示意图[22]. (b) MAMS-1的晶体结构, ab平面以紫红色突出显示, 以显示层状结构; (c) MAMS-1晶体通过冻融法剥落成纳米片; (d) MAMS-1纳米片的TEM图像, 比例尺为1 mm(左)和3 nm(右)[59]

Figure 5. (a) Illustration of freeze-thaw exfoliation of graphene oxide[22]. (b) Crystal structure of MAMS-1. The ab planes are highlighted in magenta to illustrate the layered structure; (c) the freeze-thaw exfoliation of MAMS-1 crystals into dispersed nanosheets; (d) TEM image of MAMS-1 nanosheets. Scale bars, 1 mm (left) and 3 nm (right)[59]

图6. (a) 通过插层和化学剥离方法制备MOF纳米片的示意图; (b) 制备的MOF纳米片的TEM图像[63]. (c) 沿a轴观察的3D-Co柱状结构, 孔以黄色突出显示; (d) 柱状配体脱落的2D-Co沿b轴观察的层状结构, 交替使用蓝色和绿色的图层以说明层状结构; (e) 3D-Co的SEM图像; (f) 2D-Co纳米片的TEM图像, 插图为纳米片分散液的丁达尔效应[64]

Figure 6. (a) Schematic illustration of the overall process developed to produce 2D MOF nanosheets via an intercalation and chemical exfoliation approach; (b) TEM image of an individual exfoliated MOF nanosheet[63]. (c) 3D pillared-layer structure viewing along the a-axis with pore surface highlighted in yellow in 3D-Co; (d) 3D packing structure of the 2D layers viewing along the b-axis in 2D-Co. Alternate layers blue and green for clarity; (e) SEM images of 3D-Co; (f) a TEM image of 2D-Co nanosheets (inset: Tyndall effect of acolloidal solution)[64]

图7. (a) 金属-有机骨架纳米片阵列的合成工艺[69]. (b) 2D氧化物牺牲法制备2D MOF-74纳米片示意图[70]. (c) 2D Fe/Co-MOFs合成示意图[71]

Figure 7. (a) Synthetic process of metal-organic framework nanosheet array[69]. (b) Schematic illustration of the 2D oxide sacrifice approach to prepare 2D MOF-74 nanosheets[70]. (c) Illustration of the synthesis of 2D Fe/Co-MOFs[71]

图8. (a) 由[Hf6O4(OH)4(HCO2)6(羧酸盐)6]结构单元和苯-1,3,5-三苯甲酸酯配体形成2D晶格(C黑色, Hf蓝色, O红色); (b) [Hf6O4(OH)4(HCO2)6(BTB)3]纳米片的TEM图像[72]. (c) CO2封端合成2D MOF的原理示意图; (d) 在CO2/甲醇溶液中制备的Cu(BDC)纳米片的SEM图[76]

Figure 8. (a) Formation of the 2D lattice from [Hf6O4(OH)4(HCO2)6- (carboxylate)6] units and 1,3,5-benzenetricarboxylic (BTB) ligands. C black, Hf blue, O red; (b) TEM image of [Hf6O4(OH)4(HCO2)6(BTB)3] nanosheets[72]. (c) Illustration of the CO2-directed formation of 2D MOF nanosheets. (d) SEM image of Cu(BDC) nanosheets synthesized in CO2/methanol solution[76]

图9. (a) 二维h-MoO3合成的示意图[77]. (b) ZIF-67纳米片的盐模板合成示意图[78]

Figure 9. (a) Schematic representation of 2D h-MoO3 synthesis[77]. (b) Schematic illustration of the synthesis of ZIF-67 nanosheets via salt-template confined in situ growth[78]

图10. (a) 气/液界面合成单层Ni-MOF的示意图; (b) 单层Ni-MOF的AFM图像[84]. (c) 液/液界面合成的多层Zn-MOF纳米片的AFM图像和截面高度分析, 比例尺为5 mm; (d) 气/液界面合成的少层纳米片的AFM图像, 比例尺为2 mm[85]

Figure 10. (a) Illustration of the synthesis of single layer Ni-MOF on the gas/liquid interfacial; (b) AFM topological image of single-layer Ni-MOF[84]. (c) AFM image of multilayer Zn-MOF nanosheets and its cross-section analysis. Scale bar, 5 mm; (d) AFM image of single-layer Zn-MOF nanosheets. Scale bar, 2 mm[85]

图11. (a) [Zn(BeIM)OAc]与CTAB形成的复合结构, [Zn(BeIM)OAc] (红色)沿[001]堆叠, CTAB(黑色); (b) 复合结构纳米片的侧视TEM 图[94]. (c) Zn-TCPP的传统合成和表面活性剂辅助合成. 上: 各向同性生长为块状MOF晶体. 下: 表面活性剂在MOF表面上附着导致其各向异性生长, 形成超薄的MOF纳米片. Zn-TCPP层分别绘制为蓝色和紫色, 以使层状结构清晰可见; (d) Zn-TCPP纳米片的TEM图像[95]

Figure 11. (a) Composite structure of [Zn(BeIM)OAc] and CTAB, composed of [Zn(BeIM)OAc] (in red) stacked along [001], and CTAB is black; (b) side TEM view onto the lamellae composite nanosheet structure [94]. (c) The traditional synthesis and surfactant-assisted synthesis of Zn-TCPP. Top: The isotropic growth generates the bulk crystal of MOFs. Bottom: The attachment of surfactants on the surface of MOFs leads to their anisotropic growth, resulting in the formation of ultrathin MOF nanosheets. The Zn-TCPP layers are drawn in blue and purple, respectively, in order to make the layered structures clear; (d) TEM image of a single Zn-TCPP nanosheets[95]

图12. (a) Zn/Ni-MOF-2晶体结构转换的示意图. 氢原子和终端溶剂分子被省略[99]; (b)通过自下而上和自上而下的整体策略设计和制备了一种化学稳定的MOF纳米片[101]

Figure 12. (a) Schematic illustration of crystal-structure transformation of Zn/Ni-MOF-2 combined with its shape evolution. Hydrogen atoms and terminal solvent molecules have been omitted[99]; (b) the design and preparation of a chemically stable MOF nanosheets via a bottom-up and a top-down integral strategy[101]

方法类型	合成方法	横向尺寸	厚度	均匀性	收率	实验条件	前体	文献
自上而下	超声剥离	一般	薄	一般	低	简单	2D MOF	^{[50,52⇓⇓-55]}
	球磨-超声	一般	薄	一般	低	特殊溶剂	2D MOF	^[57-58]
	冻融法	大	薄	好	低	大温差	2D MOF	^[59]
	化学剥离	小	薄	好	低	较复杂	2D/3D MOF	^[62⇓-64]
自下而上	直接合成	一般	一般	好	高	简单	2D/3D MOF	^{[67,69⇓-71]}
	封端剂/调节剂合成	大	薄	一般	一般	较复杂	2D MOF	^{[72⇓⇓⇓-76,97]}
	模板合成	大	薄	好	一般	简单	2D/3D MOF	^[78]
	气/固界面合成	小	超薄	好	低	界面要求高	部分2D MOF	^[83]
	气/液界面合成	极大	超薄	好	一般	界面要求高	部分2D MOF	^[84-85]
	液/液界面合成	极大	超薄	好	一般	界面要求高	部分2D MOF	^[84-85]
	L-B	极大	超薄	好	一般	界面、仪器要求高	部分2D MOF	^[92]
组合策略		大	薄	一般	低	较复杂	2D/3D MOF	^{[94⇓-96,98⇓⇓-101]}

表1. 2D MOF纳米片的各种制备方法对比[102]

Table 1. Comparison of the approaches for 2D MOF nanosheets synthesis[102]

图13. (a) 在α-Al2O3基底上抽滤得到的膜. 上: CuBDC-GO膜(左: 潮湿, 右: 干燥后). 下: CuBDC膜(左: 潮湿, 右: 干燥后). 右: 抽滤在尼龙-6基底上以弯曲测试机械强度; (b, c) CuBDC-GO膜的SEM 图[103]. (d) 在尼龙基底上抽滤得到的2D Zn-TCP膜的俯视(上)和截面(下)SEM图(白箭头指向膜的褶皱)[105]. (e) 将PAMAM接枝到Zn2bim3纳米片上, 再进行抽滤制备的2D MOF膜的SEM图[106]. (f) 抽滤在AAO上的2D Ni3(HITP)2膜的SEM图[107]

Figure 13. (a) Digital photographs of the membranes prepared on α-Al 2O3 supports. Up: CuBDC-GO membranes (left: fresh, right: dried). Down: CuBDC membranes (left: fresh, right: dried). Right: Membranes prepared on nylon-6 organic porous substrates; (b, c) SEM images of top-view of CuBDC-GO membrane[103]. (d) SEM image of the 2D Zn-TCP(Fe) selective layer on nylon support prepared by the vacuum filtration method (wrinkles are denoted by the white arrow) and cross-sectional SEM image of Zn-TCP(Fe) selective layer[105]. (e) SEM images of the top view of the as-synthesized 2D MOF membrane using Zn2bim3 nanosheets modified with PAMAM[106]. (f) SEM top view of a Ni3(HITP)2 membranes on AAO support[107]

图14. (a) 热滴涂装置[58]. (b~d) 不同厚度(4, 12, 40 nm)的2D MAMS-1膜的正面场发射扫描电子显微镜(FE-SEM)图, 标尺为2 μm [59]

Figure 14. (a) Illustration of the hot-drop coating apparatus[58]. (b~d) FE-SEM images (top view) of 4-nm, 12-nm and 40-nm 2D MAMS-1 membranes, respectively. Scale bars, 2 μm [59]

图15. (a) 通过L-B生长的2D MOF薄膜转移到SiO2(300 nm)/Si上的AFM图; (b) 2D MOF薄膜沉积在TEM栅格上的SEM图; (c) 2D多层MOF膜的TEM图, 插图为SAED衍射图案; (d) MOF薄膜的AFM图像(约2 nm, 16.6 μm×16.6 μm) [108]

Figure 15. (a) AFM image of the 2D MOF film synthesized by L-B method deposited on SiO2(300 nm)/Si; (b) SEM image of the 2D MOF film suspended over a TEM grid; (c) TEM image of a multilayer MOF film. The insert is a SAED pattern of a multilayer film; (d) AFM image of a MOF film (16.6 μm×16.6 μm) with a thickness of ~2 nm [108]

图16. GO引导的ZnO纳米棒热转化为高取向2D Zn2(bim)4纳米片膜的示意图[110]

Figure 16. Scheme depicting the preparation procedure of highly oriented Zn2(bim)4 nanosheet membranes by ZnO self-conversion growth in a GO confined space[110]

2D MOF膜合成方法	优势	不足	文献
真空抽滤	简单, 通用	膜厚, 纳米片堆叠方式不可控	^[103-107]
热滴涂	膜薄, 可调控堆叠方式	受实验条件影响, 重现性差	^[57⇓-59]
L-B	一步合成, 膜薄	实验条件苛刻, 可控性差	^[108]
直接生长	简单, 可控	膜厚	^[109-110]

表2. 2D MOF纳米片膜制备方法对比

Table 2. Comparison of synthesis methods of 2D MOF nanosheets membrane

图17. (a) 旋涂法制备2D膜的示意图[22]. (b) 电泳沉积制备2D膜的示意图[118]

Figure 17. (a) Schematic illustration for 2D membrane synthesis by spin coating[22]. (b) Schematic illustration for 2D membrane synthesis by electrophoretic deposite[118]

膜种类	膜制备方法	膜厚度	H₂渗透量/ (*10^-8 mol•m^-2•s^-1•Pa^-1)	H₂/CO₂ 选择性	膜类型	文献
Zn₂bim₄	热滴涂	<10 nm	92	291	片状	^[57]
Zn₂bim₃	热滴涂	<10 nm	65	128	片状	^[58]
MAMS-1	热滴涂	12 nm	227	40	片状	^[59]
MAMS-1		40 nm	13	215	片状	^[59]
CuBDC/GO (12∶1)^a	真空抽滤	700 nm	96	95	片状	^[103]
CuBDC/GO (2.4∶1)^a		700 nm	18	232	片状	^[103]
Zn₂bim₄	直接生长	50 nm	20	53	管状	^[109]
Zn₂bim₄/GO	直接生长	100 nm	14	106	管状	^[110]

表3. 2D MOF膜应用于气体分离(H2/CO2)的性能

Table 3. Gas separation (H2/CO2) performance of 2D MOF membrane

图18. (a) 多孔Zn2(Bim)3纳米片进行气体分离的原理图; (b) 温度变化对150 ℃制备的Zn2(Bim)3纳米片膜的H2/CO2渗透量和选择性的影响[58]. (c) 40 nm 2D MAMS-1膜在两个升/降温循环中的H2渗透量; (d) 40 nm 2D MAMS-1膜在七个升/降温循环中的H2/CO2渗透量和选择性. 蓝色: 20 ℃; 洋红色: 40 ℃; 绿色: 60 ℃; 橙色: 80 ℃; 红色: 100 ℃; 黑色: 120 ℃[59]

Figure 18. (a) Illustration of the hypothesis of gas separation through porous Zn2(Bim)3 nanosheets; (b) effect of varying temperature on H2/CO2permeance and mixture separation factor of a Zn2(Bim)3 nanosheet membrane prepared at 150 ℃[58]. (c) H2 permeance of 40-nm 2D MAMS-1 membranes under two heating/cooling cycles. (d) H2/CO2 gas permeance and separation factors of the 40-nm 2D MAMS-1 membrane under seven heating/cooling cycles. Different colours represent various temperatures: blue, 20 ℃; magenta, 40 ℃; olive, 60 ℃; orange, 80 ℃; red, 100 ℃ and black, 120 ℃[59]

图19. (a) 在30 ℃下测试的2D Zn2bim4纳米片膜的H2渗透量和H2/CO2选择性与H2分压的函数; (b) 2D Zn2bim4纳米片膜的H2/CO2渗透量和选择性与温度的函数[110]

Figure 19. (a) H2/CO2 selectivity and permeances of the 2D Zn2bim4 nanosheet membrane as function of the H2 partial pressure at 30 ℃; (b) H2/CO2 permeances and selectivity as a function of temperature difference of the 2D Zn2bim4 nanosheet membrane[110]

图20. (a) AAO上10 nm厚的2D Al-MOF层状膜的SEM图; (b) 具有不同厚度的2D Al-MOF膜的截面放大图, 比例尺500 nm; (c) 使用100 nm厚的Al-MOF膜进行不同离子溶液(0.5 mol•L-1)的离子渗透率和水通量; (d) 2D Al-MOF膜和其他2D层状膜的水通量和水/盐选择性的关系, 每种符号表示不同的盐[121]

Figure 20. (a) SEM image of a 10-nm-thick Al-MOF laminar membrane on AAO substrate; (b) Magnified cross-sectional views of 2D Al-MOF membranes with different thicknesses. Scale bars, 500 nm; (c) Water flux through a 100-nm-thick Al-MOF membrane using different ion solutions (0.5 mol•L-1) and the corresponding ion permeation rates. (d) Correlation between water flux and water/salt selectivity of 2D Al-MOF membranes and other representative 2D laminar membranes. Each set of symbols represents a different salt[121]

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二维金属-有机骨架膜的制备及其在分离中的应用

Preparation of Two-Dimensional Metal-Organic Framework Membranes and Their Applications in Separation

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