后合成法构筑钛基金属有机框架及其应用

doi:10.6023/A23020041

化学学报 ›› 2023, Vol. 81 ›› Issue (5): 548-558.DOI: 10.6023/A23020041 上一篇

综述

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

Qi Xueping, Wang Fei(), Zhang Jian

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)

文章分享

摘要/Abstract

钛基金属有机框架(Ti-MOFs)因其优异的光催化活性成为当前材料研究领域的热点. 但由于Ti离子极高的反应活性和亲氧属性, 在反应过程中极易形成氧化物和其它竞争性的副产物, 使得Ti-MOFs的合成极具挑战性. 在MOFs发展的初期, 关于Ti-MOFs的研究便同步开展, 然而经过二十多年的发展, 已报道的Ti-MOFs只有数十种, 在上万种的MOFs中占比极其有限. 为了避免或减少钛离子副反应的发生, 通常在已知MOFs框架中引入金属Ti离子, 来定向合成Ti-MOFs, 该方法被称为后合成法(PSM), 也是构筑Ti-MOF框架的一种有效方法. 对PSM构筑Ti-MOFs的实例进行了系统的调研和总结. 首先, 依据钛离子引入方式和位置的不同, 分为离子交换、离子插入(金属节点或簇单元位置引入钛离子)和配体修饰(有机配体位置引入钛离子)三种途径, 并通过实例介绍了每种途径构筑的Ti-MOFs. 随后, 对PSM构筑的Ti-MOFs及其复合材料的设计与应用进行讨论. 最后, 对PSM构筑Ti-MOFs的现状进行总结并展望了未来的发展方向.

关键词: 金属有机框架, 后合成法, 钛, 光催化

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

引用此文

齐学平, 王飞, 张健. 后合成法构筑钛基金属有机框架及其应用[J]. 化学学报, 2023, 81(5): 548-558.

Qi Xueping, Wang Fei, Zhang Jian. 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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图/表 13

图1. PSM构筑Ti-MOFs重要节点

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]

表1. 部分主要PSM构筑Ti-MOFs及合成条件

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

表1. 部分主要PSM构筑Ti-MOFs及合成条件

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

图2. 通过PSE合成混合配体MOF1(Zr), 以得到混合金属MOFs 1(Zr/Ti), UiO-66(Zr/Ti)-NH2

图3. 生物相容性的PCN-224(Zr/Ti)敷料作为光驱抗菌剂用于治疗细菌感染, 由于Ti掺入诱导ROS生成增加, PCN-224(Zr/Ti)杀菌活性增强

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

图4. 从模板MOFs设计Ti-MOFs逐步HVMO程序示意图 (a) MIL-100(Sc)和PCN-333(Sc)与Ti(III)金属交换, 然后在空气中金属节点氧化[PCN-333(Sc)和MIL-100(Sc)具有相同拓扑但结构不同]; (b) MOF-74(Zn)和MOF-74(Mg)的过程类似

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

图5. 不同Ti负载条件下Zr6节点上的转换路线注意, 当负载3Ti/Zr6时, 所提出的结构可能同时存在

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

图6. UiO-66中支撑在节点(A), 节点(B)和支柱(C)上的TiIV离子结构(这些离子周围的配体是不清楚的, 因此被省略)

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

图7. Ti功能化的H-UiO-66(Zr/Ti)制备示意图

图8. UiO-67-bpydc-MoO2Cl2-Ti合成过程示意图

图9. 基于对该过程产生Ti(III)和O2的观察, 可见光激发Ti/Zr-MOF- 525电子转移和CO2光还原过程机理

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.

图10. 构建UZT/CFMX异质结构示意图

图11. U(VI)在缺陷Zr-MOFs上的光催化还原示意图

图12. (a)合成UiO-66(Zr)-NH2和均苯三甲酰氯(TMC)功能化UiO-66(Zr)-NH2纳米颗粒的反应步骤和(b)以金属有机框架(MOFs)和TMC(UiO-66(Zr)-NH2)为例, 通过共价键制备TFN膜示意图

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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