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收稿日期:
2024-07-18
修回日期:
2024-08-28
通讯作者:
周阿武,李建荣
作者简介:
安昊天(1997—),男,博士研究生,anhaotian@emails.bjut.edu.cn
基金资助:
Haotian AN(), Zhangye HAN, Muyao LU, Awu ZHOU(), Jianrong LI()
Received:
2024-07-18
Revised:
2024-08-28
Contact:
Awu ZHOU, Jianrong LI
摘要:
金属-有机框架(MOF)是一类由金属离子或金属簇与有机配体通过配位键形成的新型多孔材料。它们展现出结构多样、高比表面积、高孔隙率、结构与性质多样化调控等优点。近年来,MOF在吸附、分离、催化和传感等不同领域的应用逐渐受到关注。然而,MOF宏量制备面临着许多化学工程领域的挑战,包括:合成条件严苛、反应时间延长、产量低以及成本高等。因此,研究人员正在探索各种新的合成方法,如水热/溶剂热法、常温快速合成法、溶剂回流法、碱辅助法、机械化学法、电化学法、微波辅助法、超声波辅助法、喷雾干燥法、干凝胶转化法、加速老化法等。以此为主题,综述了宏量制备MOF的方法,并对成本、环境影响、安全性和可行性进行了评价,也简要讨论了MOF成型加工技术的最新进展,展望了未来MOF材料在宏量制备与成型方面的挑战与机遇。
中图分类号:
安昊天, 韩章烨, 陆慕瑶, 周阿武, 李建荣. 推进MOF产业化应用:宏量制备与成型[J]. 化工学报, DOI: 10.11949/0438-1157.20240819.
Haotian AN, Zhangye HAN, Muyao LU, Awu ZHOU, Jianrong LI. Promoting Industrial Application of MOF: Scale-up Preparation and Shaping[J]. CIESC Journal, DOI: 10.11949/0438-1157.20240819.
图4 (a) MOF-303结构示意图,(b) 在200 L反应容器中合成3.5 kg规模的MOF-303[26]
Fig. 4 (a) Schematic of MOF-303 structure, (b) synthesis of 3.5 kg scale MOF-303 in a 200 L reaction vessel[26]
图5 (a) 用于UiO-66-NH2连续生产的双螺杆挤出装置示意图,(b) 水辅助机械化学绿色合成Zr-MOF示意图[38]
Fig. 5 (a) TSE setup used for continuous mechanochemical synthesis of UiO-66-NH2, (b) water-assisted mechanochemical procedure for green synthesis of zirconium MOF[38]
图6 (a) 高熵-ZIF的机械化学合成示意图,(b) 高熵-ZIF的TEM图像和EDS元素分布图[39]
Fig. 6 (a) Schematic of mechanochemical synthesis of high-entropy ZIFs, (b) TEM image and EDS elemental distribution of high-entropy ZIFs[39]
图7 在羧基功能化的ITO电极表面直接电化学合成MIL-101(Fe)薄膜[45]
Fig. 7 Surface functionalization of ITO electrodes with carboxylic acid groups enables direct electrosynthesis of Fe-MIL-101 films on the inert conducting support[45]
图8 MOF-808_15(红色)、MOF-808_60(蓝色)和 MOF-808_120(绿色)的:(a) 用于制备MOF-808(实线)和对照材料(虚线)的受控加热斜率,(b) 粉末X射线衍射图,(c) 77 K下的N2吸附曲线,(d) SEM图像,比例尺:1 μm[59]
Fig. 8 MOF-808_15 (red), MOF-808_60 (blue) and MOF-808_120 (green): (a) controlled-heating ramp used in the preparation of MOF-808 (continuous lines) and control materials (dashed lines), (b) powder X-ray diffractograms, (c) N2 adsorption at 77 K, (d) SEM images, Scale bar: 1 μm[59]
宏量制备方法 | 典型MOF | 温度/ ℃① | 时间① | 溶剂① | 金属源 | 时空产率/ (kg m-3 day-1)① | 参考文献 |
---|---|---|---|---|---|---|---|
水热法/溶剂热法 | UiO-66 | 120 | 24 h | DMF | ZrCl4 | / | [ |
HKUST-1 | 90 | 12 min | DMF、乙醇、水 | Cu(NO3)2·H2O | 5.8 | [ | |
MOF-5 | 120 | 12 min | DMF | Zn(NO3)2·6H2O | / | ||
IRMOF-3 | 120 | 12 min | DMF | Zn(NO3)2·6H2O | / | ||
UiO-66 | 140 | 15 min | DMF | ZrCl4 | / | ||
常温快速合成法/溶剂回流法 | UiO-66-(COOH)2 | 100 | 16 h | 水 | ZrCl4 | 96 | [ |
MIP-202(Zr) | 120 | 1 h | 水 | ZrCl4 | 7030 | [ | |
MOF-801(Zr) | 室温 | 5.5 h | 水 | ZrOCl2·8H2O | 168 | [ | |
NKMOF-8-Br | 室温 | 1 min | 乙腈 | CuI | / | [ | |
Cu-AD-SA | 80 | 24 h | DMF、水 | Cu(NO3)2·3H2O | 160 | [ | |
碱辅助法 | MOF-5 | 室温 | 24 h | DMF | Zn(NO3)2·6H2O | / | [ |
MIL-53(Al) | 室温 | 7天 | 水 | Al(NO3)3·9H2O | / | ||
MOF-74 | 室温 | 20 h | 水 | Zn(CH3COO)2·2H2O | / | ||
MOF-303 | 120 | 6 h | 水 | AlCl3·6H2O | 179.5 | [ | |
机械化学法 | ZIF-8 | 室温 | 96 h | / | ZnO | / | [ |
ZIF-8 | 室温 | 2 h | 水 | Zn(CH3COO)2·2H2O | / | [ | |
MOF-74(Zn) | 室温 | 70 min | 水 | ZnO | / | [ | |
Fe-MIL-88A | 室温 | 10 min | / | FeCl3·6H2O | / | [ | |
HKUST-1 | 室温 | / | 乙醇 | Cu(OH)2 | 144000 | [ | |
ZIF-8 | 200 | / | / | [ZnCO3]2[Zn(OH)2]3 | 144000 | ||
Al-Fum | 室温 | / | / | Al2(SO4)3·18H2O | 27000 | ||
UiO-66 | 室温 | 90 min | 水 | 异丙醇锆 | / | [ | |
电化学法 | Fe-MIL-101 | 室温 | 14 h | DMF | FeCl2 | / | [ |
Fe-MIL-101-NH2 | 室温 | 8 h | DMF | FeCl2 | / | ||
Fe-MIL-100 | 室温 | 18 h | DMF | FeCl2 | / | ||
Fe-MIL-88B-NH2 | 室温 | 2 h | DMF | FeCl2 | / | ||
微波辅助法 | MOF-74 (Ni) | 125 | 60 min | DMF、乙醇、水 | Ni(NO3)2·6H2O | / | [ |
MOF-808 | 95 | 1 h | 水 | ZrOCl2·8H2O | / | [ | |
超声波辅助法 | CPO-27-Co | 70 | 75 min | DMF、水 | Co(NO3)2·6H2O | / | [ |
MIL-53(Fe) | / | 7 min | DMF | FeCl3·6H2O | / | [ | |
喷雾干燥法 | UiO-66 | 220 | / | DMF | 乙酰丙酮锆 | / | [ |
CID-1 | 220 | / | DMF | Zn(NO3)2·4H2O | / | ||
干凝胶转换法 | MIL-100(Fe) | 室温 | 30 min | 水 | Fe(NO3)3·9H2O | / | [ |
加速老化法 | Cd-MOF | 45 | 4天 | / | CdO | / | [ |
表1 部分MOF宏量制备工作主要参数
Table 1 Some key parameters related to the scale-up synthesis of MOFs
宏量制备方法 | 典型MOF | 温度/ ℃① | 时间① | 溶剂① | 金属源 | 时空产率/ (kg m-3 day-1)① | 参考文献 |
---|---|---|---|---|---|---|---|
水热法/溶剂热法 | UiO-66 | 120 | 24 h | DMF | ZrCl4 | / | [ |
HKUST-1 | 90 | 12 min | DMF、乙醇、水 | Cu(NO3)2·H2O | 5.8 | [ | |
MOF-5 | 120 | 12 min | DMF | Zn(NO3)2·6H2O | / | ||
IRMOF-3 | 120 | 12 min | DMF | Zn(NO3)2·6H2O | / | ||
UiO-66 | 140 | 15 min | DMF | ZrCl4 | / | ||
常温快速合成法/溶剂回流法 | UiO-66-(COOH)2 | 100 | 16 h | 水 | ZrCl4 | 96 | [ |
MIP-202(Zr) | 120 | 1 h | 水 | ZrCl4 | 7030 | [ | |
MOF-801(Zr) | 室温 | 5.5 h | 水 | ZrOCl2·8H2O | 168 | [ | |
NKMOF-8-Br | 室温 | 1 min | 乙腈 | CuI | / | [ | |
Cu-AD-SA | 80 | 24 h | DMF、水 | Cu(NO3)2·3H2O | 160 | [ | |
碱辅助法 | MOF-5 | 室温 | 24 h | DMF | Zn(NO3)2·6H2O | / | [ |
MIL-53(Al) | 室温 | 7天 | 水 | Al(NO3)3·9H2O | / | ||
MOF-74 | 室温 | 20 h | 水 | Zn(CH3COO)2·2H2O | / | ||
MOF-303 | 120 | 6 h | 水 | AlCl3·6H2O | 179.5 | [ | |
机械化学法 | ZIF-8 | 室温 | 96 h | / | ZnO | / | [ |
ZIF-8 | 室温 | 2 h | 水 | Zn(CH3COO)2·2H2O | / | [ | |
MOF-74(Zn) | 室温 | 70 min | 水 | ZnO | / | [ | |
Fe-MIL-88A | 室温 | 10 min | / | FeCl3·6H2O | / | [ | |
HKUST-1 | 室温 | / | 乙醇 | Cu(OH)2 | 144000 | [ | |
ZIF-8 | 200 | / | / | [ZnCO3]2[Zn(OH)2]3 | 144000 | ||
Al-Fum | 室温 | / | / | Al2(SO4)3·18H2O | 27000 | ||
UiO-66 | 室温 | 90 min | 水 | 异丙醇锆 | / | [ | |
电化学法 | Fe-MIL-101 | 室温 | 14 h | DMF | FeCl2 | / | [ |
Fe-MIL-101-NH2 | 室温 | 8 h | DMF | FeCl2 | / | ||
Fe-MIL-100 | 室温 | 18 h | DMF | FeCl2 | / | ||
Fe-MIL-88B-NH2 | 室温 | 2 h | DMF | FeCl2 | / | ||
微波辅助法 | MOF-74 (Ni) | 125 | 60 min | DMF、乙醇、水 | Ni(NO3)2·6H2O | / | [ |
MOF-808 | 95 | 1 h | 水 | ZrOCl2·8H2O | / | [ | |
超声波辅助法 | CPO-27-Co | 70 | 75 min | DMF、水 | Co(NO3)2·6H2O | / | [ |
MIL-53(Fe) | / | 7 min | DMF | FeCl3·6H2O | / | [ | |
喷雾干燥法 | UiO-66 | 220 | / | DMF | 乙酰丙酮锆 | / | [ |
CID-1 | 220 | / | DMF | Zn(NO3)2·4H2O | / | ||
干凝胶转换法 | MIL-100(Fe) | 室温 | 30 min | 水 | Fe(NO3)3·9H2O | / | [ |
加速老化法 | Cd-MOF | 45 | 4天 | / | CdO | / | [ |
图9 (a) 用于海水淡化的MOF-303膜,(b) 在α-Al2O3表面上生长的MOF-303膜横截面SEM图[75]
Fig. 9 (a) MOF-303 membrane for seawater desalination, (b) SEM image of the cross-section of MOF-303 membrane grown on α-Al2O3 surface[75]
图12 粉末和压片成型的(a) MIL-53(Al)(压片、碎片),(b) Cu3(BTC)2(压片、粉末)[84]
Fig. 12 Powder and pelletized (a) MIL-53(Al) (tablets, crushed tablets), (b) Cu3(BTC)2 (tablet, powder)[84]
图13 使用不同粘合剂制备的ZUL-300颗粒:(a) ZUL-300(左)和ZUL-300@HPC(右),(b) ZUL-300(左)和ZUL-300@PVB(右),(c) ZUL-300(左)和ZUL-300@PVA(右)[87]
Fig. 13 ZUL-300 pellets prepared with different binders: (a) ZUL-300 (left) and ZUL-300@HPC (right), (b) ZUL-300 (left) and ZUL-300@PVB (right), (c) ZUL-300 (left) and ZUL-300@PVA (right)[87]
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