Abstract

The iron (III) benzene dicarboxylate metal-organic framework material (MIL-53(Fe)) was synthesized with either the solvent-thermal or hydrothermal method under different conditions. The influence of the type of solvents, molar ratio of precursors and solvent, temperature, and reaction time on the structure of MIL-53(Fe) was investigated. The material was characterized by using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), X-ray photoelectron spectroscopy (XPS), and N2 adsorption/desorption isotherm. The MIL-53(Fe) structure formed in N′, N-dimethylformamide (DMF) and methanol (MeOH) but not in water. In DMF, the molar ratio of precursors and solvent, temperature, and reaction time had a significant effect on the crystal structure of MIL-53(Fe). Under optimal conditions, MIL-53(Fe) has high crystallinity and a large specific surface area ( S BET = 88.2 m2/g). The obtained MIL-53(Fe) could serve as a potential heterogeneous catalyst to oxidize phenol (PhN), rhodamine B (RhB), and methylene blue (MtB) in the Fenton-like reaction system at the different solution pHs.

Highlights

  • Influence of Solvent Type. e influence of DMF, MeOH, and water on the formation of the crystal structure of iron (III) benzene dicarboxylate is evaluated from X-ray diffraction (XRD) data. e XRD patterns of the samples synthesized in DMF and MeOH exhibit diffraction peaks at 7.24, 8.92, 9.72, 10.15, and 12.50° (Figure 1(a)). ese peaks indicate that the metalorganic framework structure is formed in the reaction

  • The sample synthesized in MeOH has diffraction peaks with higher 2θ at 17, 25, and 27.6° (Figure 1(b)), and they are the typical diffraction peaks for BDC. is evidence indicates that a large amount of BDC does not react or only binds with iron (III) in the form of individual structures. e sample synthesized in water exhibits only the characteristic diffraction peaks of BDC without diffraction peaks at smaller angles (Figure 1(b))

  • E MIL-53(Fe) structure is formed via the bonds between iron (III)/iron oxide and the BDC anion, and the number of these bonds has a significant influence on the synthesis efficiency

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Summary

Introduction

Metal-organic frameworks (MOFs) are porous nanomaterials with large specific surface area and considerable pore volume [1,2,3,4,5,6,7,8,9,10,11]. ese materials have attracted a lot of attention from scientists due to their perfect structure and applicability in such fields as gas separation and storage [12,13,14,15,16,17], molecular sensors [18, 19], adsorption [1,2,3,4, 20,21,22], and catalysis [5,6,7,8, 23,24,25,26,27]. MIL-53(Fe) has attracted the attention of researchers due to its framework containing iron that acts as the structural nodes functioning as a new photocatalyst [5, 24] and a catalyst in the Fenton-like reaction system [6,7,8, 25]. E influence of solvent type, solvent content, temperature and time of reaction, and the molar ratio of precursors has been investigated to produce MIL-53(Fe) with high crystallinity and a large specific surface area. The obtained material is used as a catalyst in the Fenton-like reaction system to oxidize phenol (PhN), rhodamine B (RhB), and methylene blue (MtB). E concentration of PhN in the solution was determined with high-performance liquid chromatography (HPLC) on the UFLC Shimadzu (Japan) equipment. E RhB (or MtB) concentration in the supernatant was determined with the UV-Vis method on the Jasco V-770 (Japan) at λmax 554 nm for RhB (λmax 664 nm for MtB)

Results and Discussion
BDC Water
Initial solution pH
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