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Progress in Chemistry 2023, Vol. 35 Issue (12): 1752-1763 DOI: 10.7536/PC230415 Previous Articles   Next Articles

• Review •

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: Revised: Online: Published:
  • Contact: *e-mail: yangjiangfeng@tyut.edu.cn
  • Supported by:
    National Natural Science Foundation of China(21908153)
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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
Fig. 1 Metal that has been used to construct MOF. Orange: used; blue: unused[7]
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]
Fig. 2 Development of Ti-MOF (Orange: solvothermal synthesis; yellow: post-synthetic modification; green: in situ SBUs construction method)
Fig. 3 Structure of MIL-125[11]
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
Fig. 4 Synthesis of Cd-Ti-MOF-1[13]
Fig. 5 (a) Crystal structure of Cd-Ti-MOF-1. (b) Topology of ctm[13]
Fig. 6 Zn/Ti-oxo clusters of ZTOF-1 and ZTOF-2[13]
Fig. 7 Representative structures of ZTOF-1 and ZTOF-2[13]
Fig. 8 Structures of CTOF-1 and CTOF-2[47]
Fig. 9 The structure of MUV-10(Ca)[24]
Fig. 10 Stability of MUV-10(Ca) between pH 2 and 12[24]
Fig. 11 SEM images of MIL-173(Ti/Zr) samples of variable Ti content[48]
Fig. 12 The mechanism of UiO-66@TiO2 by PSM[56]
Fig. 13 Synthesis of MOF-5(Zn/Me) (Me=Ti, V, Cr, Mn, Fe)[57]
Fig. 14 Synthesis of Ti-MOF by HVMO[20]
Fig. 15 Heterometallic Ti-MOFs by Metal-exchange reactions[50]
Fig. 16 Synthesis process of PCN-22[19]
Fig. 17 7-connected Ti-oxo-clusters of PCN-22[13]
Fig. 18 Isoreticular MOF-901 and MOF-902[60]
Fig. 19 Diversity of Ti-oxo-clusters[61?~63]
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)
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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