The smallest Ni species triggering selective hydrogenation of CO2 to methane: Ni dimer embedded in MFI and enhancement of MnOx

doi:10.1016/S1872-2067(26)65095-4

Abstract

Abstract:

Ni-based catalysts have shown significant potential in CO₂ methanation, but the high catalytic performance is usually obtained at quite high Ni loading, as small particles just transform CO₂ into CO via reverse water gas shift reaction. Thus, a scientifically and practically important work is clarification of the structure of the smallest active Ni species and the catalytic activity of structurally different Ni species. Here, MnO_x-modulated metallic nickel dimers (MnO_x-Ni₂) were embedded in silicalite-1 framework at a Ni loading of ~0.86%. It’s CO₂ conversion, CH₄ selectivity and CH₄ space time yield (STY) surprisingly reach ~76%, ~98% and ~450 mol·mol_Ni^-1·h^-1 at 400 °C, 0.5 MPa and 12000 mL·g^-1·h^-1. Such a catalytic performance can be well maintained at least within 200 h. In-situ spectroscopy, density functional theory (DFT) calculation and ab initio molecular dynamics simulation results confirm that Ni dimer (Ni₂) is the smallest Ni cluster triggering the CO₂ methanation and the CH₄ formation activity is linearly increased with the Ni₂ content. Introduction of MnO_x not only increases the number of Ni₂ species, but also improves its intrinsic activity in CO₂ methanation, as MnO_x enhances the electronic density of Ni species and facilitates NiO reduction to MnO_x-Ni₂ species. This species shows higher H₂ dissociation activity than single atom Ni (Ni₁), pure Ni₂ and large Ni nanoparticles (NPs). In addition, it exhibits much stronger CO adsorption and lower energy barrier of CO* intermediate hydrogenation to CH₄. In-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), isotope-labeled in-situ DRIFTS, on line mass spectroscopy (MS), Proton transfer reaction time of flight PTR TOF-MS and DFT calculation results reveal that CO₂ hydrogenation to methane on MnO_x-Ni₂@MFI mainly follows the HCOO* and CO* intermediates route.

Key words: Zeolite, Confined encapsulation, Ni-based catalyst, Nickel dimers, CO₂ hydrogenation, Reaction mechanism

Sen Wang, Shiying Li, Rui Geng, Bo Zhou, Pengfei Wang, Zhangfeng Qin, Mei Dong, Jianguo Wang, Unni Olsbye, Weibin Fan. The smallest Ni species triggering selective hydrogenation of CO₂ to methane: Ni dimer embedded in MFI and enhancement of MnO_x[J]. Chinese Journal of Catalysis, 2026, 87: 113-125.

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https://www.cjcatal.com/EN/Y2026/V87/I8/113

Figures/Tables 5

Fig. 1. Catalytic performance of (x)Ni@MFI and (x)Ni-MnOx(y)@MFI in CO2 methanation. (a,b) Catalytic results of (0.9)Ni@MFI, (0.9)Ni-MnOx(y)@MFI and MnOx@MFI for CO2 hydrogenation to methane. (A) (0.9)Ni@MFI; (B) (0.9)Ni-MnOx(18.0)@MFI; (C) (0.9)Ni-MnOx(9.0)@MFI; (D) (0.9)Ni-MnOx(4.5)@MFI; (E) (0.9)Ni-MnOx(2.0)@MFI; (F) (0.9)Ni-MnOx(1.1)@MFI; (G) MnOx@MFI. Reaction conditions: 400 °C, 1 atm, 12000 mL·g-1·h-1, and H2/CO2 molar ratio of 4/1. (c) The CH4 STYs obtained on (0.9)Ni-MnOx(2.0)@MFI and reported typical Ni-based catalysts. (1) Ni3Fe2/ZrO2 (1 atm); (2) Ni-MCM-41 (1 atm); (3) Ni/a-TiO2-NH3 (1 atm); (4) Ni-sepiolite (1 atm); (5) Ni-La2O3/Na-Beta (1 atm); (6) Ni@NaX (0.5 MPa); (7) Ni/CeO2 (1 atm); (8) Ni/SiO2 (1 atm); (9) Ni-CeO2/Al2O3 (1 atm); (10) Ni@MGC (1 atm); (11) Ni/LaMgOx-ZSM-5 (1 atm); (12) Ni/SSZ-13 (1 atm); (13) NiMn/Al2O3 (1 atm); (14) Ni/CeO2 (1 atm); (15) LaNi1?xCoxO3 (1 atm); (16) Ni-CeO2/MCM-41 (1 atm); (17) Ni-CeO2-Y2O3 (1 atm); (18) LaNiOx (1 atm). (d) Catalytic stability test result of (0.9)Ni-MnOx(2.0)@MFI in CO2 hydrogenation to methane. Reaction conditions: 400 °C, 5 atm, 12000 mL·g-1·h-1 and H2/CO2 molar ratio of 4/1.

Fig. 2. Catalysts characterization of Ni-MnOx(x)@MFI catalyst. (a,b) In-situ XRD patterns of (0.9)Ni-MnOx(2.0)@MFI after reduction at 590 °C for 2 h in H2 atmosphere and further catalyzing CO2 hydrogenation at 400 °C for 6 h at 0.1 MPa and H2/CO2 molar ratio of 4/1. (c?e) TEM images of (0.9)Ni-MnOx(2.0)@MFI. High resolution aberration-corrected HAADF-STEM image (f) and corresponding color-enhanced contrast HAADF-STEM images (h,i) (the green-colored bright spots represent the highly dispersed NiOx and MnOx within silicalite-1 framework), and iDPC-STEM image (g) of (0.9)Ni-MnOx(2.0)@MFI. (j) STEM-EDX elemental mappings of Si, O, Ni and Mn in (0.9)Ni-MnOx(2.0)@MFI.

Fig. 3. Electronic structure and coordination state of Ni species. Ni-K edge XANES (a) and EXAFS (b) spectra of (0.9)Ni@MFI and (0.9)Ni-MnOx(2.0)@MFI after in-situ H2 reduction at 590 °C for 2 h, and reference samples of NiO and Ni foil. (c) The percentage of Ni species and the CN of Ni-Ni of reduced (x)Ni@MFI catalysts. (d) The dependence of CH4 formation rate (mol·h?1) derived from its space time yield on the Ni dimer amount of reduced (x)Ni@MFI catalysts. PDOS results for Ni, Mn, O and Si atoms of Ni-MnOx@MFI (e), and for Ni, O and Si atoms of Ni@MFI (f). (g) CDD result of Ni-MnOx@MFI. The accumulation and depletion charge regions are shown in yellow and cyan, respectively. Temperature and energy fluctuations (h) as well as the variation of Ni-Ni bonding distance of MnOx-Ni2 sites (i) in AIMD simulations at 873 K for a duration of ~10000 fs. (j) Radial distribution function (g(r)) and integrated g(r) for Ni-Ni bond of MnOx-Ni2 sites.

Fig. 4. Reaction mechanism of Ni@MFI and Ni-MnOx(x)@MFI catalysts in CO2 methanation. (a?c) Temperature-dependent in-situ DRIFTS of (0.9)Ni-MnOx(2.0)@MFI for CO2 hydrogenation. The arrow represents the increase in reaction temperature. Time-dependent in-situ DRIFTS of (0.9)Ni-MnOx(2.0)@MFI (d) and Ni@MFI (e) for CO2 hydrogenation at 180 °C. (f) Dependence of in-situ DRIFTS peak intensity of formate species on the reaction time at 180 °C on (0.9)Ni-MnOx(2.0)@MFI and (0.9)Ni@MFI. (g) On-line MS of the effluents during CO2 hydrogenation of (0.9)Ni-MnOx(2.0)@MFI. (h,i) Temperature-dependent in-situ PTR TOF-MS for CO2 hydrogenation on (0.9)Ni-MnOx(2.0)@MFI.

Fig. 5. DFT calculations and AIMD simulations. Reaction scheme for CO2 methanation (a) and free energy profiles of various elemental steps for CO2 hydrogenation to methane on Ni2 and MnOx-Ni2 sites (b). The free energy surface of CO* adsorption on Ni1 (c), Ni2 (d) and MnOx-Ni2 (e) sites obtained from metadynamics (MTD) calculations.

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The smallest Ni species triggering selective hydrogenation of CO₂ to methane: Ni dimer embedded in MFI and enhancement of MnO_x

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