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化学进展 2023, Vol. 35 Issue (12): 1752-1763 DOI: 10.7536/PC230415 前一篇   后一篇

• 综述 •

钛基金属有机框架材料合成的研究进展

刘苏慧1,2, 张飞飞1,2, 王小青1,2, 刘普旭1,2, 杨江峰1,2,*()   

  1. 1 太原理工大学 化学工程与技术学院 太原 030024
    2 气体能源高效清洁利用山西省重点实验室 太原 030024
  • 收稿日期:2023-04-13 修回日期:2023-06-30 出版日期:2023-12-24 发布日期:2023-09-10
  • 作者简介:

    杨江峰 教授,博导,入选国家级青年人才项目;担任中国化工学会化工过程强化专业委员会青年委员,《低碳化学与化工》期刊青年编委。主要研究方向:非常规天然气及氢气的富集与提纯;基于温室气体减排的捕集与回收;无机多孔材料制备与气体吸附分离研究。在Adv. Mater., Angew. Chem. Int. Ed., Chem. Commun., AIChE J., IECR等刊物发表SCI收录论文百余篇,授权国家发明专利22件;获2019年度山西省自然科学一等奖(第一),2021年度中国石油和化学工业联合会技术发明一等奖(第二),2022年度山西省科技进步三等奖(第二)。

  • 基金资助:
    国家自然科学基金项目(21908153)
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Research Progress in Synthesis of Titanium-Based Organic Framework Materials

Suhui Liu1,2, Feifei Zhang1,2, Xiaoqing Wang1,2, Puxu Liu1,2, Jiangfeng Yang1,2,*()   

  1. 1 College of Chemical Engineering and Technology, Taiyuan University of Technology,Taiyuan 030024, China
    2 Shanxi Key Laboratory of Gas Energy Efficient and Clean Utilization,Taiyuan 030024, China
  • Received:2023-04-13 Revised:2023-06-30 Online:2023-12-24 Published:2023-09-10
  • Contact: *e-mail: yangjiangfeng@tyut.edu.cn
  • Supported by:
    National Natural Science Foundation of China(21908153)

钛基金属有机框架(Ti-MOF)作为一种高价金属MOF,具有优异的化学稳定性、特殊的光响应特性、低毒性等优点,但由于钛金属源具有很高的反应活性,给材料合成带来了一定的挑战。本文综述了近年来Ti-MOF在合成方面的研究进展,详细介绍了溶剂热直接合成法、后交换合成法、原位生成SBUs构筑法等方法,并对形成的拓扑类型和晶体结构进行了分析,总结了Ti-MOF的合成规律及各种方法的优缺点。指出调控金属源和配位环境是获得Ti-MOF最重要的策略,并从原位生成SBUs构筑Ti-MOF和构筑双金属Ti/M-MOF两个角度进行了展望。

关键词： 钛基金属有机框架, 合成, 溶剂热, 后交换

As a kind of metal-organic framework (MOF) with high valence, titanium-based metal-organic framework (Ti-MOF) has superior chemical stability, appealing photoresponsive properties, low toxicity and so on. However, due to the high reactivity of titanium sources, it brings certain challenges to the synthesis of materials. In this paper, the research progress of Ti-MOF synthesis in recent years is reviewed, and the solvothermal synthesis, post-synthetic modification and in situ SBUs construction methods are introduced in detail. The topological types and crystal structures formed are analyzed, and the synthesis rules of Ti-MOF and the advantages and disadvantages of various methods are summarized. It is pointed out that the control of the metal source and coordination environment is the most important strategy to obtain Ti-MOF, and the construction of Ti-MOF by in-situ formation of SBUs and heterometallic Ti/M-MOF are prospected.

Contents

1 Introduction

2 Synthesis of Ti-MOF

2.1 Solvothermal synthesis

2.2 Post-synthetic modification

2.3 In situ SBUs construction methods

3 Conclusion and outlook

Key words: titanium-based MOFs, synthesis, solvothermal synthesis, post-synthetic modification
()
图1 已被用作构建MOF的金属。橙色:已被使用;蓝色:未被使用[7]
Fig. 1 Metal that has been used to construct MOF. Orange: used; blue: unused[7]
表1 Ti-MOF的应用范围[11]
Table 1 Application fields of Ti-MOF[11]
MOF Ti-oxo-cluster Bandgap energy (eV) Application
MIL-125 Ti8O8(OH)4(CO2)16 3.60 Alcohol oxidation[18]
MIL-125-NH2 Ti8O8(OH)4(CO2)16 2.60 CO2 photoreduction, water splitting
H2 production[21]
NTU-9 TiO6 1.72 Dye degradation[17]
PCN-22 Ti7O6(CO2)12 1.93 Alcohol oxidation[19]
MOF-901 Ti6O6(CO2)6 2.65 Polymerization[22]
ZSTU-3 (Ti6O12)n 2.20 H2 production[23]
MUV-10 Ti2Ca2(O)2(H2O)4(CO2)8 3.10 H2 production[24]
MUV-101 [TiM2(O)
(O2C)6X3]
(M=Mg, Fe,
Co, Ni;)		 — Hydrolysis of nerve agent simulants[25]
FIR-125 Ti8O8(OH)4(CO2)16 2.95 CO2 photoreduction[26]
图2 Ti-MOF发展历程(橙色:溶剂热直接合成法;黄色:后交换合成法;绿色:原位生成SBUs构筑法)
Fig. 2 Development of Ti-MOF (Orange: solvothermal synthesis; yellow: post-synthetic modification; green: in situ SBUs construction method)
图3 MIL-125的结构图[11]
Fig. 3 Structure of MIL-125[11]
表2 基于溶剂热法合成的Ti-MOF
Table 2 Ti-MOF synthesized by solvothermal synthesis
Ti-MOF Ti sources Organic linker Solvent environment ref
MTM-1 Ti(OiPr)4 Isonicotinic acid ACN 32
MIL-125 Ti(OiPr)4 Terephthalic acid DMF、Dry CH3OH 18
NH2-MIL-125 Ti(OiPr)4 2-Aminoterephthalic acid DMF、Dry CH3OH 21
MIP-207 Ti(OiPr)4 Trimesic acid Ac2O、CH3COOH 33
IEF Ti(OiPr)4 Squaric acid IPA、CH3COOH 34
NTU-9 Ti(OiPr)4 2,5-Dihydroxyterephthalic acid CH3COOH 17
MIL-167 Ti(OiPr)4 2,5-Dihydroxyterephthalic acid DEF、CH3OH 35
COK-69 Cp2TiCl2 Trans-1,4-cyclohexanedicarboxybic acid DMF、CH3COOH 36
Ti-MIL-101 TiCl3 Terephthalic acid DMF、C2H5OH 37,38
MIL-177 Ti(OiPr)4 3,3',5,5'-Tetracarboxydiphenylmethane CH3OH 39
ZSTU-1 Ti(OiPr)4 4,4',4″-Nitrilotribenzoic acid DryDMF 23
ZSTU-2 Ti(OiPr)4 1,3,5-Tris(4-Carboxyphenyl)benzene DryDMF 23
ZSTU-3 Ti(OiPr)4 4',4‴,4'''''-Nitrilotris([1,1'-biphenyl]-4-carboxylic acid) DryDMF 23
Ti-(Ti-TBP) TiCl4·2THF Tetra(4-carboxyphenyl)porphine DMF、CH3COOH 40
MUV-11 Ti(OiPr)4 Benzene-1,4-dihydroxamic acid DMF、CH3COOH 41
ACM-1 Ti(OiPr)4 4,4',4″,4‴-(1,9-dihydropyrene-1,3,6,8-tetrayl)tetrabenzoic acid DEF-C6H5Cl(1∶1)、
C2H5COOH		 42
图4 Cd-Ti-MOF-1的合成方法[13]
Fig. 4 Synthesis of Cd-Ti-MOF-1[13]
图5 (a) Cd-Ti-MOF-1的晶体结构; (b) ctm拓扑结构[13]
Fig. 5 (a) Crystal structure of Cd-Ti-MOF-1. (b) Topology of ctm[13]
图6 ZTOF-1和ZTOF-2中的Zn/Ti-oxo簇[13]
Fig. 6 Zn/Ti-oxo clusters of ZTOF-1 and ZTOF-2[13]
图7 ZTOF-1和ZTOF-2的代表性结构[13]
Fig. 7 Representative structures of ZTOF-1 and ZTOF-2[13]
图8 CTOF-1和CTOF-2的结构[47]
Fig. 8 Structures of CTOF-1 and CTOF-2[47]
图9 MUV-10(Ca)的配位结构[24]
Fig. 9 The structure of MUV-10(Ca)[24]
图10 MUV-10(Ca)在pH=2~12的稳定性[24]
Fig. 10 Stability of MUV-10(Ca) between pH 2 and 12[24]
图11 不同Ti含量的MIL-173(Zr/Ti)的SEM[48]
Fig. 11 SEM images of MIL-173(Ti/Zr) samples of variable Ti content[48]
图12 PSM法制备UiO-66@TiO2的机理示意图[56]
Fig. 12 The mechanism of UiO-66@TiO2 by PSM[56]
图13 PSM策略制备的MOF-5(Zn/Me)(其中Me=Ti、V、Cr、Mn、Fe)[57]
Fig. 13 Synthesis of MOF-5(Zn/Me) (Me=Ti, V, Cr, Mn, Fe)[57]
图14 HVMO方法制备的Ti-MOF [20]
Fig. 14 Synthesis of Ti-MOF by HVMO[20]
图15 金属交换策略制备的双金属Ti-MOF[50]
Fig. 15 Heterometallic Ti-MOFs by Metal-exchange reactions[50]
图16 PCN-22合成过程[19]
Fig. 16 Synthesis process of PCN-22[19]
图17 PCN-22的7-连接钛簇[13]
Fig. 17 7-connected Ti-oxo-clusters of PCN-22[13]
图18 等网状的MOF-901和MOF-902[60]
Fig. 18 Isoreticular MOF-901 and MOF-902[60]
图19 Ti-oxo-clusters的多样性[61?~63]
Fig. 19 Diversity of Ti-oxo-clusters[61?~63]
表3 基于原位生成SBUs构筑法的Ti-MOF
Table 3 Ti-MOF synthesized by in situ SBUs construction methods
Ti-MOF Ti sources Organic linker Solvent environment ref
PCN-22
Ti6O6(OiPr)6(abz)6		 Ti(iPrO)4 4-Aminobenzoic acid IPA 19
PCN-22 Ti6O6(OiPr)6(abz)6 Tetrakis(4-carboxyphenyl)porphyrin DEF、C6H5COOH、
DGIST-1
(Ti6O6(OiPr)6(t-BA)6)		 Ti(iPrO)4 4-Aminobenzoic acid IPA 65
DGIST-1 Ti6O6(OiPr)6(t-BA)6 Tetrakis(4-carboxyphenyl)porphyrin DEF、C6H5COOH
MIP-208
Ti8AF cluster		 Ti(iPrO)4 Ac2O CH3COOH 66
MIP-208 Ti8AF cluster 5-Aminoisophthalic acid Ac2O、C2H5COOH、CH3OH
Ti3-BPBC
(Ti6O6(OiPr)6(abz)6)		 Ti(iPrO)4 4-Aminobenzoic acid IPA 67
Ti3-BPBC Ti6O6(OiPr)6(abz)6 Biphenyl-4,4'-dicarboxylic acid DMF、C2H5COOH
MIL-100(Ti)
Ti6O6(4-tbbz)6(OiPr)6		 Ti(iPrO)4 4-tert-butylbenzoic acid IPA-THF (3∶1) 68
MIL-100(Ti) Ti6 Trimesic acid ACN-THF(3∶1)
表4 三种合成方法的对比
Table 4 Comparison of three synthesis methods
Method Advantage and disadvantage Common synthesis condition
Solvothermal synthesis Ti-MOF Ad: The available ligands are diverse, and the synthesized structures are rich with few restrictions.
Dis: High reaction activity, easy hydrolysis, and the majority of synthesized sample powders.		 Ti sources: organic Ti sources
Solvent environment: organic solvent
pH controller:acetic acid
Heterometallic Ti/M-MOF Ad: Properly reduce the reactivity of Ti and synthesize materials with heterometallic advantages.
Dis: The high polarizing power of Ti4+ prevents a direct reaction with other metals that would likely result in poor control over their distribution in the final material for the formation of segregated phases.		 Ti sources:organic sources
Solvent environment:organic solvent
Post-synthetic modification M-MOF transform into Ti/M-MOF
by PSM		 Ad: Capable of functionalizing the introduction of specific Ti ions into existing MOFs.
Dis: 1. Titanium sources are prone to severe hydrolysis and are dangerous to operate.
2. Easy to be MOF@metal oxide rather than Ti/M-MOF		 Ti sources:TiCl3、TiCl4 etc.
Synthetic environment:Inert
gas environment
Ti/M1-MOF transform into Ti/M2-MOF by PSM Ad: Heterometallic Ti-MOF that cannot be obtained under high-temperature solvothermal conditions can be synthesized.
Dis: Ti/M1-MOF is relatively rare, and not all bimetallic MOFs are suitable for this strategy.
In situ SBUs construction methods Ad: It is another effective method to control the hydrolysis Condensation reaction reaction of Ti.
Dis: The addition of reaction steps has made the stability of titanium clusters another factor limiting the reaction.		 Ti sources:Ti6O6(OiPr)6(abz)6
Solvent environment:organic solvent
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