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. 2024 Mar 29;29(7):1548.
doi: 10.3390/molecules29071548.

Aerobic Oxidative Desulfurization by Supported Polyoxometalate Ionic Liquid Hybrid Materials via Facile Ball Milling

Qian Wang  1   2 , Tianqi Huang  1 , Shuang Tong  1 , Chao Wang  1 , Hongping Li  1 , Ming Zhang  1
Affiliations

Aerobic Oxidative Desulfurization by Supported Polyoxometalate Ionic Liquid Hybrid Materials via Facile Ball Milling

Qian Wang et al. Molecules. .

Abstract

With the increasingly strict limitations on emission standards of vehicles, deep desulfurization in fuel is indispensable for social development worldwide. In this study, a series of hybrid materials based on SiO2-supported polyoxometalate ionic liquid were successfully prepared via a facile ball milling method and employed as catalysts in the aerobic oxidative desulfurization process. The composition and structure of prepared samples were studied by various techniques, including FT-IR, UV-vis DRS, wide-angle XRD, BET, XPS, and SEM images. The experimental results indicated that the synthesized polyoxometalate ionic liquids were successfully loaded on SiO2 with a highly uniform dispersion. The prepared catalyst (C16PMoV/10SiO2) exhibited good desulfurization activity on different sulfur compounds. Moreover, the oxidation product and active species in the ODS process were respectively investigated via GC-MS and ESR analysis, indicating that the catalyst can activate oxygen to superoxide radicals during the reaction to convert DBT to its corresponding sulfone in the fuel.

Keywords: aerobic oxidation desulfurization; ball milling; ionic liquid; polyoxometalate; solvent free.

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Conflict of interest statement

Author Qian Wang was employed by the company Hangzhou Zhensheng Technology Co., Ltd. The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest.

Figures

Figure 1
Figure 1
(A) FT-IR spectra, (B) Raman spectra, (C) XRD patterns and (D) UV-DRS spectra of different samples.
Figure 2
Figure 2
XPS analysis of C16PMoV: (A) survey, (B) Mo 3d, (C) V 2p and XPS spectra of C16PMoV/10SiO2: (D) full spectrum, (E) Mo 3d, (F) V 2p.
Figure 3
Figure 3
SEM images: (A) SiO2, (B) C16PMoV/10SiO2; EDS (C) of C16PMoV/10SiO2 and mapping images (D–F).
Figure 4
Figure 4
(A) Nitrogen adsorption-desorption isotherms and (B) pore size distributions of hybrid materials of different samples.
Figure 5
Figure 5
The effects of different factors: (A) different IL content, reaction conditions: m(catalysts) = 0.06 g, T = 120 °C, ν(air) = 100 mL/min; (B) catalyst mass, reaction conditions: T = 120 °C, ν(air) = 100 mL/min; (C) temperature, reaction conditions: m(catalyst) = 0.06 g, ν(air) = 100 mL/min; (D) sulfides, reaction conditions: m(catalysts) = 0.06 g, T = 120 °C, ν(air) = 100 mL/min.
Figure 6
Figure 6
Recycling performance and mass loss of catalysts in oxidative desulfurization. Reaction condition: m(catalyst) = 0.06 g, T = 120 °C, ν(air) = 100 mL/min.
Figure 7
Figure 7
GC-MS analysis of the oil phase (A) and the catalyst phase (B) during the reaction. Reaction condition: m(catalyst) = 0.06 g, T = 120 °C, ν(air) = 100 mL/min.
Figure 8
Figure 8
(A) The free radical capture experiment of catalyst C16PMoV/10SiO2; (B) ESR spectra of DMPO−•O2− generated in the oxidation reaction of DBT with C16PMoV/10SiO2. (a) With a catalyst; (b) without a catalyst.
See this image and copyright information in PMC

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