Trifunctional strategy for the design and synthesis of a Ni-CeO2@SiO2 catalyst with remarkable low-temperature sintering and coking resistance for methane dry reforming

doi:10.1016/S1872-2067(21)63789-0

Abstract

Abstract:

In this study, a trifunctional strategy was developed to prepare a confined Ni-based catalyst (Ni-CeO₂@SiO₂) for dry reforming of methane (DRM) of two main greenhouse gases—CO₂ and CH₄. The Ni-CeO₂@SiO₂ catalyst was fabricated by utilizing the confinement effect of the SiO₂ shell and the synergistic interaction between Ni-Ce and the decoking effect of CeO₂. The catalysts were systematically characterized via X-ray diffraction, N₂ adsorption/desorption, transmission electron microscopy, energy dispersive X-ray spectroscopy, hydrogen temperature reduction and desorption set by program, oxygen temperature program desorption, Raman spectroscopy, thermogravimetric analysis, and in situ diffuse reflectance infrared Fourier transform spectroscopy measurements to reveal their physicochemical properties and reaction mechanism. The Ni-CeO₂@SiO₂ catalyst exhibited higher activity and stability than the catalyst synthesized via the traditional impregnation method. In addition, no carbon deposition was detected over Ni-CeO₂@SiO₂ after a 100 h durability test at 800 °C, and the average particle size of Ni nanoparticles (NPs) in the catalyst increased from 5.01 to 5.77 nm. Remarkably, Ni-CeO₂@SiO₂ also exhibited superior low-temperature stability; no coke deposition was observed when the catalyst was reacted at 600 °C for 20 h. The high coking and sintering resistance of this confined Ni-based DRM catalyst can be attributed to its trifunctional effect. The trifunctional strategy developed in this study could be used as a guideline to design other high-performance catalysts for CO₂ and CH₄ dry forming and accelerate their industrialization.

Key words: Methane dry forming, Low-temperature stability, Coke resistance, Trifunctional strategy, CO₂ utilization

Sixue Lin, Jing Wang, Yangyang Mi, Senyou Yang, Zheng Wang, Wenming Liu, Daishe Wu, Honggen Peng. Trifunctional strategy for the design and synthesis of a Ni-CeO₂@SiO₂ catalyst with remarkable low-temperature sintering and coking resistance for methane dry reforming[J]. Chinese Journal of Catalysis, 2021, 42(10): 1808-1820.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(21)63789-0

https://www.cjcatal.com/EN/Y2021/V42/I10/1808

Figures/Tables 12

Scheme 1. Illustration of the trifunctional strategy to design the confined Ni-CeO2 catalysts with high coking and sintering resistance.

Fig. 1. (a,b) TEM images of freshly reduced Ni-CeO2@SiO2 catalyst; (c) the particle size distribution of Ni-CeO2@SiO2 catalyst; HAADF-STEM (d) and EDX mapping (e-j) of the freshly reduced Ni-CeO2@SiO2 catalyst; (e) overlap images of Ni, Ce, Si and O species; (f) O mapping image; (g) Si mapping image; (h) Ce mapping image; (i) Ni mapping image; (j) Ni-Ce overlap image; (k) Line scan of freshly reduced Ni-CeO2@SiO2 catalyst.

Fig. 2. (a) H2-TPR profiles of the freshly calcined catalysts; (b) O2-TPD profiles of the freshly reduced Ni-CeO2@SiO2 and Ni-CeO2/SiO2 catalysts.

Fig. 3. Catalytic activities of Ni-CeO2@SiO2, Ni-CeO2/SiO2, Ni/SiO2 catalysts for DRM at different temperatures: (a) CH4 conversion; (b) CO2 conversion. Reaction conditions: WHSV = 18000 mL gcat-1 h-1, p = 1 atm, CH4:CO2 = 1:1.

Fig. 4. (a) Catalytic turnover frequencies (TOF) of CH4 and CO2; (b) Catalytic reaction rates of CH4 and CO2 calculated at 425 °C. Reaction conditions: WHSV = 90000 mL gcat-1 h-1, p = 1 atm, CH4:CO2 = 1:1.

Fig. 5. 100 h stability test of Ni-CeO2@SiO2. Reaction conditions: WHSV = 18000 mL gcat-1 h-1, p = 1 atm, CH4:CO2 = 1:1, temperature = 800 °C.

Fig. 6. TEM images and Ni particle size distributions of Ni-CeO2@SiO2 catalyst after 20 h of reaction at 800 °C (a,b), Ni-CeO2@SiO2 catalyst after 100 h of reaction at 800 °C (c,d), Ni-CeO2/SiO2 catalyst after 20 h of reaction at 800 °C (e); (f) XRD pattern of these catalysts after 20 and 100 h of reaction at 800 °C; (g) Raman spectra of all the spent catalysts; (h) TGA curves of all the spent catalysts.

Fig. 7. (a,b) 20 h stability test of Ni-CeO2@SiO2 catalyst: CH4 conversion and CO2 conversion. Reaction conditions: WHSV = 18000 mL gcat-1 h-1, p = 1 atm, CH4:CO2 = 1:1, temperature: 600 °C and H2/CO ratio of after 20 h reaction of the Ni-CeO2NW@SiO2 catalysts catalyst; (c,d) TEM images and Ni particle size distribution of the Ni-CeO2@SiO2 catalyst after 20 h of reaction at 600 °C; (e) TGA curves of the spent catalysts; (f) Raman spectra of the spent catalysts.

Fig. 8. Partial DRIFT spectra of CO2+CH4 adsorbed at different temperatures over Ni-CeO2@SiO2 with the wavelength 1770-2202 cm-1 (a) and 1770-1220 cm-1 (b). Reaction conditions: F(CH4) = F(CO2) = 10 mL min-1, F(N2) = 50 mL min-1.

Fig. 9. DRIFTS spectra of CO2-TPA at different temperatures over Ni-CeO2@SiO2. (b) is a 3D surface diagram explaining Fig. (a). Reaction conditions: F(CO2) = 10 mL min-1, F(N2) = 60 mL min-1.

Fig. 10. (a-c) In situ DRIFTS spectra of CH4-TPD at different temperatures over Ni-CeO2@SiO2. Reaction conditions: F(CH4) = 10 mL min-1, F(N2) = 60 mL min-1.

Scheme 2. The reaction mechanism of dry methane reforming on Ni-CeO2@SiO2 catalyst with triple functions.

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Trifunctional strategy for the design and synthesis of a Ni-CeO₂@SiO₂ catalyst with remarkable low-temperature sintering and coking resistance for methane dry reforming

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