Morphology evolution of acetic acid-modulated MIL-53(Fe) for efficient selective oxidation of H2S

doi:10.1016/S1872-2067(20)63625-7

Abstract

Abstract:

MIL-53(Fe) was synthesized using a “modulator approach” that utilizes acetic acid (HAc) as an additive to control the size and morphology of the resulting crystals. We demonstrate that after activation under vaccum at 100 °C, the MIL-53(Fe) functions well for H₂S selective oxidation. The introduction of acetic acid in the presence of benzene-1,4-dicarboxylic acid (H₂BDC) would result in a series of MIL-53(Fe) nanocrystals (denoted as MIL-53(Fe)-xH, x stands for the volume of added HAc with morphology evoluting from irregular particles to short hexagonal columns. The vacuum treatment facilitates the removal of acetate groups, thus generating Fe ³⁺ Lewis acid sites. Consequently, the resulted MIL-53(Fe)-xH exhibits good catalytic activity (98% H₂S conversion and 92% sulfur selectivity ) at moderate reaction temperatures (100-190 °C). The MIL-53(Fe)-5H is superior to the traditional iron-based catalysts, showing stable performance in a test period of 55 h.

Key words: Fe-metal-organic frameworks, Hydrogen sulfide, Selective oxidation, Controllable synthesis, Acetic acid, Modulation

Xiaoxiao Zheng, Sihui Qi, Yanning Cao, Lijuan Shen, Chaktong Au, Lilong Jiang. Morphology evolution of acetic acid-modulated MIL-53(Fe) for efficient selective oxidation of H₂S[J]. Chinese Journal of Catalysis, 2021, 42(2): 279-287.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(20)63625-7

https://www.cjcatal.com/EN/Y2021/V42/I2/279

Figures/Tables 10

Fig. 1. (A) Schematic of MIL-53(Fe)-xH preparation (Gray, C; Blue, O; Aqua, Fe3+; Light Orange, Fe3+ Lewis acid sites; Purple dotted line, missing linker defects); SEM images of (B) MIL-53(Fe), (C) MIL-53(Fe)-3H, (D) MIL-53(Fe)-5H, and (E) MIL-53(Fe)-10H.

Fig. 2. XRD patterns of MIL-53(Fe) and MIL-53(Fe)-xH (before vacuum treatment at 100 °C).

Fig. 3. DSC (red) and TG (black) curves of prepared samples: (A) MIL-53(Fe), (B) MIL-53(Fe)-3H, (C) MIL-53(Fe)-5H, and (D) MIL-53(Fe)-10H.

Fig. 4. (A) FT-IR spectra and (B) Raman spectra of MIL-53(Fe)-xH.

Fig. 5. XPS spectra of MIL-53(Fe)-xH: (A) survey; (B) C 1s; (C) O 1s; and (D) Fe 2p.

Fig. 6. Effect of reaction temperature on (A) conversion of H2S, (B) sulfur selectivity, and (C) sulfur yield over MIL-53(Fe), MIL-53(Fe)-xH and commercial Fe2O3.

Fig. 7. Time-on-stream behavior of Fe2O3, MIL-53(Fe), and MIL-53(Fe)-5H for H2S selective oxidation at 190 °C.

Fig. 8. Py-FT-IR spectra of (A) MIL-53(Fe), (B) MIL-53(Fe)-3H, (C) MIL-53(Fe)-5H, and (D) MIL-53(Fe)-10H after degassing at 30, 100, and 150 °C.

Fig. 9. Pyridine sorption peak area (at 1070 cm-1) and H2S conversion over MIL-53(Fe)-xH.

Fig. 10. Diagram of the selective conversion of H2S to sulfur over MIL-53(Fe)-xH.

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Morphology evolution of acetic acid-modulated MIL-53(Fe) for efficient selective oxidation of H₂S

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