A Post-Synthetic Method for the Construction of Titanium-Based Metal Organic Frameworks and Their Applications

doi:10.6023/A23020041

Acta Chimica Sinica ›› 2023, Vol. 81 ›› Issue (5): 548-558.DOI: 10.6023/A23020041 Previous Articles

Review

后合成法构筑钛基金属有机框架及其应用

齐学平, 王飞^*(), 张健

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:2023-02-20 发布日期:2023-03-28

作者简介:

齐学平, 中国科学院福建物质结构研究所无机化学专业在读硕士研究生, 师从王飞研究员. 目前主要研究方向为钛基金属有机框架材料的设计、合成及应用.

王飞, 中国科学院福建物质结构研究所研究员, 博士生导师. 2012年入选“中科院青年创新促进会”会员. 2014年获得卢嘉锡青年人才奖, 同年入选中国科学院福建物质结构研究所(海西研究院)“春苗”青年人才. 2019年获福建省自然科学二等奖(排名第二). 从事金属有机框架材料研究, 在钛基金属有机框架材料、手性金属有机框架材料、沸石型金属有机框架材料的设计合成及其在气体分离、催化/光电催化、手性识别拆分等领域取得系列进展, 已在Chem. Soc. Rev., Angew. Chem., Int. Ed., ACS Materials Lett., J. Mater. Chem A.及ACS Appl. Mater. Interfaces等期刊以第一和通讯作者发表论文100多篇.

张健, 中国科学院福建物质结构研究所研究员, 博士生导师. 现任中国科学院福建物质结构研究所副所长, 结构化学国家重点实验室副主任. 2014年获国家杰出青年基金资助. 主要研究方向为团簇和多孔催化材料. 目前作为课题负责人承担有国家杰出青年基金, 中国科学院“先导B”课题, 国家自然科学基金重点项目等多项研究课题. 已在系列国际知名期刊上发表论文300多篇, 论文被他人正面引用超过2万次, H因子82.

基金资助:
项目受国家自然科学基金(21971241)

A Post-Synthetic Method for the Construction of Titanium-Based Metal Organic Frameworks and Their Applications

Xueping Qi, Fei Wang(), Jian Zhang

State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002

Received:2023-02-20 Published:2023-03-28
Contact: *E-mail: wangfei04@fjirsm.ac.cn
Supported by:
National Natural Science Foundation of China(21971241)

Titanium-based metal organic frameworks (Ti-MOFs) have become a hot topic in current materials research due to their excellent photocatalytic activity. However, due to the extremely high reactivity and oxygenophilic properties of Ti ions, oxides and other competing by-products are easily formed during the reaction process, making the synthesis of Ti-MOFs extremely challenging. The research on Ti-MOFs was carried out simultaneously at the early stage of MOFs development, however, after more than two decades of development, only tens of Ti-MOFs have been reported, accounting for an extremely limited proportion of the tens of thousands of MOFs. In order to avoid or reduce the occurrence of titanium ion side reactions, Ti-MOFs are usually synthesized by introducing metal Ti ions into the framework of known MOFs to orientate the synthesis of Ti-MOFs, which is called post-synthetic method (PSM) and is also an effective method to construct Ti-MOF framework. The examples of PSM for constructing Ti-MOFs are systematically investigated and summarized in a timely manner. Firstly, based on the different ways and positions of titanium ion introduction, three routes are classified as ion exchange, ion insertion (introduction of titanium ion at the position of metal nodes or cluster units) and ligand modification (introduction of titanium ion at the position of organic ligands), and the Ti-MOFs constructed by each route are introduced by examples. Subsequently, the design and application of Ti-MOFs constructed by PSM and their composites are discussed. Finally, the current status of PSM-constructed Ti-MOFs is summarized and the future development direction is foreseen.

Key words: metal organic framework, post-synthetic method (PSM), titanium, photocatalysis

Cite this article

Xueping Qi, Fei Wang, Jian Zhang. A Post-Synthetic Method for the Construction of Titanium-Based Metal Organic Frameworks and Their Applications[J]. Acta Chimica Sinica, 2023, 81(5): 548-558.

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Fig. & Tab. 13

Figure 1. PSM constructs important nodes of Ti-MOFs

Name	PSM	Ti source	Solvent	Ti percentage (max)	Condition	BET surface area/(m²•g^－1)	Ref.
UiO-66(Zr)	离子交换	TiCp₂Cl₂ TiCl₄(THF)₂ TiBr₄	DMF	w=12.0% w=37.9% w=1.4%	85 ℃, 120 h	1259 1365 1291	[43]
UiO-66(Zr/Ce)	离子交换	TiCl₄(THF)₂	DMF	x=20.2%	120 ℃, 96 h	1019	[47]
UiO-66(Zr)-NH₂,1(Zr)	离子交换	TiCl₄(THF)₂	DMF	x=28.4%	85 ℃, 120 h	—	[48]
Zr-NDC	离子交换	TiCl₄(THF)₂	DMF	x=26.7%	85 ℃, 120 h	1062.6	[49]
Zr-DNC-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=28.3%	85 ℃, 120 h	1026.7	[49]
UiO-66(Ce)	离子交换	TiCp₂Cl₂	DMF	—	100 ℃, 3 h	1032.9	[51]
(Ti/Ce)UiO-X@TiO₂ (X=H, Br, NO₂, NH₂, N)	离子交换	TiCp₂Cl₂	DMF	—	100 ℃, 3 h	—	[52]
PCN-224	离子交换	TiCp₂Cl₂	DMF	x=38.6%	120 ℃, 192 h	—	[53]
UiO-66(Zr)	离子交换	TiCp₂Cl₂	DMF	x≤60%	120 ℃, 8 h, microwave	965.8	[55]
MOF-5(Zn)	离子交换	TiCl₃(THF)₃	DMF	x=2%	room temperature, 7 d, stir	about 650	[57]
MIL-100(Sc)	离子交换	TiCl₃(THF)₃	DMF	x=88.0%	120 ℃, 24 h, N₂,	—	[58]
PCN-333(Sc)	离子交换	TiCl₃(THF)₃	DMF	x=48.8%	120 ℃, 24 h, N₂	—	[58]
MOF-74(Zn)	离子交换	TiCl₃(THF)₃	DMF	x=94.7%	120 ℃, 24 h, N₂	—	[58]
MOF-74(Mg)	离子交换	TiCl₃(THF)₃	DMF	x=37.9%	120 ℃, 24 h, N₂,	—	[58]
NU-1200(Zr)	离子插入	Ti(OⁱPr)₄	CH₂Cl₂	x=25%	60 ℃, 24 h	—	[59]
NU-1000(Zr)	离子插入	Ti(OⁱPr)₄	Heptane	w=5.16%	overnight, N₂	1930	[60]
NU-1008(Zr)	离子插入	Ti(OⁱPr)₄	Isopropanol	x=27.3%	80 ℃, 40 h	—	[61]
UiO-66(Zr)	离子插入	TiCl₄(THF)₂	DMF	X=21.3%~22.3%	90 ℃, 120 h	1200	[63]
2D UiO-67(Hf)-NS	离子插入	TiCl₄(THF)₂	DMF	x=14.58%	120 ℃, 120 h	—	[64]
H-UiO-66(Zr)	离子交换	TiCp₂Cl₂	DMF	x=3.83%	85 ℃, 120 h	1220	[65]
H-UiO-66(Zr/Ti)	离子插入	TiCp₂Cl₂ TiO(acac)₂ TiO(Bu)₄ Ti-Citrate	MeOH; H₂O	x=6.42% x=7.14% x=14.47% x=4.93%	65 ℃, 12 h, backflow	1031 1092 1588 859	[65]
IRMOF-3	配体修饰	Ti(OⁱPr)₄	CHCl₃	w=4.3%	25 ℃, 24 h, N₂	870	[69]
MIL-47-NH₂	配体修饰	TiO(acac)₂	Toluene	—	90 ℃, 40 h, Ar, stir	—	[71]
UiO-67-bpydc-MoO₂Cl₂	配体修饰和离子交换	TiCl₄(THF)₂	DMF	x=1.15%	120 ℃, 144 h	—	[74]
UiO-66(Zr)-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=57%	120 ℃, 384 h	787	[75]
MOF-525(Zr)	离子交换	TiCl₄(THF)₂	DMF	x=90%	85 ℃, 120 h	2780	[77]
UiO-67(Zr)-Ru	离子交换	TiCl₄(THF)₂	DMF	x=54.5%	120 ℃, 18 h	1694	[80]
UiO-66(Zr)-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=10.4%	120 ℃, 96 h	770	[93]
UiO-66(Zr)-NO₂	离子交换	TiCl₄(THF)₂	DMF	x=10.4%	120 ℃, 96 h	590	[93]

Name	PSM	Ti source	Solvent	Ti percentage (max)	Condition	BET surface area/(m²•g^－1)	Ref.
UiO-66(Zr)	离子交换	TiCp₂Cl₂ TiCl₄(THF)₂ TiBr₄	DMF	w=12.0% w=37.9% w=1.4%	85 ℃, 120 h	1259 1365 1291	[43]
UiO-66(Zr/Ce)	离子交换	TiCl₄(THF)₂	DMF	x=20.2%	120 ℃, 96 h	1019	[47]
UiO-66(Zr)-NH₂,1(Zr)	离子交换	TiCl₄(THF)₂	DMF	x=28.4%	85 ℃, 120 h	—	[48]
Zr-NDC	离子交换	TiCl₄(THF)₂	DMF	x=26.7%	85 ℃, 120 h	1062.6	[49]
Zr-DNC-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=28.3%	85 ℃, 120 h	1026.7	[49]
UiO-66(Ce)	离子交换	TiCp₂Cl₂	DMF	—	100 ℃, 3 h	1032.9	[51]
(Ti/Ce)UiO-X@TiO₂ (X=H, Br, NO₂, NH₂, N)	离子交换	TiCp₂Cl₂	DMF	—	100 ℃, 3 h	—	[52]
PCN-224	离子交换	TiCp₂Cl₂	DMF	x=38.6%	120 ℃, 192 h	—	[53]
UiO-66(Zr)	离子交换	TiCp₂Cl₂	DMF	x≤60%	120 ℃, 8 h, microwave	965.8	[55]
MOF-5(Zn)	离子交换	TiCl₃(THF)₃	DMF	x=2%	room temperature, 7 d, stir	about 650	[57]
MIL-100(Sc)	离子交换	TiCl₃(THF)₃	DMF	x=88.0%	120 ℃, 24 h, N₂,	—	[58]
PCN-333(Sc)	离子交换	TiCl₃(THF)₃	DMF	x=48.8%	120 ℃, 24 h, N₂	—	[58]
MOF-74(Zn)	离子交换	TiCl₃(THF)₃	DMF	x=94.7%	120 ℃, 24 h, N₂	—	[58]
MOF-74(Mg)	离子交换	TiCl₃(THF)₃	DMF	x=37.9%	120 ℃, 24 h, N₂,	—	[58]
NU-1200(Zr)	离子插入	Ti(OⁱPr)₄	CH₂Cl₂	x=25%	60 ℃, 24 h	—	[59]
NU-1000(Zr)	离子插入	Ti(OⁱPr)₄	Heptane	w=5.16%	overnight, N₂	1930	[60]
NU-1008(Zr)	离子插入	Ti(OⁱPr)₄	Isopropanol	x=27.3%	80 ℃, 40 h	—	[61]
UiO-66(Zr)	离子插入	TiCl₄(THF)₂	DMF	X=21.3%~22.3%	90 ℃, 120 h	1200	[63]
2D UiO-67(Hf)-NS	离子插入	TiCl₄(THF)₂	DMF	x=14.58%	120 ℃, 120 h	—	[64]
H-UiO-66(Zr)	离子交换	TiCp₂Cl₂	DMF	x=3.83%	85 ℃, 120 h	1220	[65]
H-UiO-66(Zr/Ti)	离子插入	TiCp₂Cl₂ TiO(acac)₂ TiO(Bu)₄ Ti-Citrate	MeOH; H₂O	x=6.42% x=7.14% x=14.47% x=4.93%	65 ℃, 12 h, backflow	1031 1092 1588 859	[65]
IRMOF-3	配体修饰	Ti(OⁱPr)₄	CHCl₃	w=4.3%	25 ℃, 24 h, N₂	870	[69]
MIL-47-NH₂	配体修饰	TiO(acac)₂	Toluene	—	90 ℃, 40 h, Ar, stir	—	[71]
UiO-67-bpydc-MoO₂Cl₂	配体修饰和离子交换	TiCl₄(THF)₂	DMF	x=1.15%	120 ℃, 144 h	—	[74]
UiO-66(Zr)-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=57%	120 ℃, 384 h	787	[75]
MOF-525(Zr)	离子交换	TiCl₄(THF)₂	DMF	x=90%	85 ℃, 120 h	2780	[77]
UiO-67(Zr)-Ru	离子交换	TiCl₄(THF)₂	DMF	x=54.5%	120 ℃, 18 h	1694	[80]
UiO-66(Zr)-NH₂	离子交换	TiCl₄(THF)₂	DMF	x=10.4%	120 ℃, 96 h	770	[93]
UiO-66(Zr)-NO₂	离子交换	TiCl₄(THF)₂	DMF	x=10.4%	120 ℃, 96 h	590	[93]

Table 1. Some major PSM for constructing Ti-MOFs and synthesis conditions

Figure 3. Enhanced bactericidal activity of PCN-224(Zr/Ti) due to the increased ROS generation induced by Ti incorporation when biocompatible PCN-224(Zr/Ti)-based dressing was applied as a light driven antibacterial agent for curing bacterial infection Reproduced with permission from ref. [53]. Copyright 2020 Wiley

Figure 4. Schematic illustration of the stepwise HVMO procedure for the design of Ti-MOFs from the template MOFs (a) MIL-100(Sc) and PCN-333(Sc) metal metathesis with Ti(III), followed by metal node oxidation in the air (PCN-333(Sc) and MIL-100(Sc) have same topology but different structures); (b) similar process for MOF-74(Zn) and MOF-74(Mg). Reproduced with permission from ref. [58]. Copyright 2016 Royal Society of Chemistry

Figure 5. Proposed transformation route on Zr6 node with different Ti loading Noted, when the loading is 3Ti/Zr6, all proposed structures might exist at the same time. Reproduced with permission from ref. [61]. Copyright 2022 American Chemical Society

Figure 6. Proposed structures for TiIV ions supported on the nodes (A), as the nodes (B), and on the struts (C) of UiO-66 (the ligands surrounding these ions are unidentified and thus are omitted) Reproduced with permission from ref. [63]. Copyright 2015 Royal Society of Chemistry

Figure 9. Proposed mechanism of electron transfer and CO2 photoreduction processes within Ti/Zr-MOF-525 excited by visible-light illumination based on the observation of Ti(III) and O2 generated in the process Reproduced with permission from ref. [77]. Copyright 2020 Wiley.

Figure 12. (a) Reaction sequence for the synthesis of UiO-66(Zr)-NH2 and trimesoyl chloride (TMC)-functionalized UiO-66(Zr)-NH2 nanoparticles and (b) schematic diagram for the fabrication of TFN membranes via the covalent bonding between metal organic frameworks (MOFs) using TMC (UiO-66(Zr)-NH2 as an example of MOF) Reproduced with permission from ref. [89]. Copyright 2020 Elsevier

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后合成法构筑钛基金属有机框架及其应用

A Post-Synthetic Method for the Construction of Titanium-Based Metal Organic Frameworks and Their Applications

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