CO2 hydrogenation selectivity shift over In-Co binary oxides catalysts: Catalytic mechanism and structure-property relationship

doi:10.1016/S1872-2067(21)63870-6

Abstract

Abstract:

The hydrogenation of CO₂ into methanol has attracted much attention and In₂O₃ is a promising catalyst. Introducing metal elements into In₂O₃ (M/In₂O₃) is one of the main strategies to improve its performance. However, its mechanism and active sites remain unclear and need to be further elucidated. Here, the noble-metal-free In_x-Co_y oxides catalysts were prepared. Much-improved performance and obvious product selectivity shift were observed. The optimized catalyst (In₁-Co₄) (9.7 mmol g_cat^-1 h^-1) showed five times methanol yields than pure In₂O₃ (2.2 mmol g_cat^-1 h^-1) (P = 4.0 MPa, T = 300 °C, GHSV = 24000 cm³_STP g_cat^-1 h^-1, H₂:CO₂ = 3). And the cobalt-catalyzed CO₂ methanation activity was suppressed, although cobalt was most of the metal element. To unravel this selectivity shift, detailed catalysts performance evaluation, together with several in-situ and ex-situ characterizations, were employed on cobalt and In-Co for comparative study. The results indicated CO₂ hydrogenation on cobalt and In-Co catalyst both followed the formate pathway, and In-Co reconstructed and generated a surface In₂O₃-enriched core-shell-like structure under a reductive atmosphere. The enriched In₂O₃ at the surface significantly enhanced CO₂ adsorption capacity and well stabilized the intermediates of CO₂ hydrogenation. CO₂ and carbon-containing intermediates adsorbed much stronger on In-Co than cobalt led to a feasible surface C/H ratio, thus allowing the *CH₃O to desorb to produce CH₃OH instead of being over-hydrogenated to CH₄.

Key words: Indium oxide, Cobalt, CO₂ hydrogenation, Methanol synthesis, Core-shell structure, Surface C/H ratio

Longtai Li, Bin Yang, Biao Gao, Yifu Wang, Lingxia Zhang, Tatsumi Ishihara, Wei Qi, Limin Guo. CO₂ hydrogenation selectivity shift over In-Co binary oxides catalysts: Catalytic mechanism and structure-property relationship[J]. Chinese Journal of Catalysis, 2022, 43(3): 862-876.

Figures/Tables 14

Table 1 Physicochemical properties of as-prepared catalysts.

Catalyst	Indium element molar proportion (%) ^a	BET surface area (m² g^-1)	Crystallite size (nm)^b
Catalyst	Indium element molar proportion (%) ^a	BET surface area (m² g^-1)	Co₃O₄	In₂O₃
Co₃O₄	0	42.89	16.6	—
In₁-Co₁₉	4.8	52.15	12.3	—
In₁-Co₉	8.9	58.75	11.2	—
In₁-Co₄	19.5	71.88	5.7	—
In₁-Co₁	51.1	29.39	13.6	15.1
In₂O₃	100	28.61	—	18

Fig. 1. Morphological and structural characterizations of as-prepared catalysts. XRD patterns (a) and Raman spectra (b) of as-prepared Inx-Coy catalysts with different In/Co molar ratios versus the referential In2O3 and Co3O4 catalysts; TEM image (c) and high-resolution TEM image (d) of as-prepared In1-Co4; (e) HAADF-STEM image and corresponding EDS elemental mappings of as-prepared In1-Co4.

Fig. 2. Catalytic performances of the catalysts. (a) CO2 conversion, product selectivity; (b) CH3OH and CH4 yield of catalysts of Inx-Coy catalysts with different In/Co molar ratios versus the referential In2O3 and Co3O4 catalysts; (c) product selectivity of In1-Co4 by co-precipitation and physical-mixed methods; (d) product selectivity, CO2 conversion of In1-Co4 catalyst with different GHSV; (e,f) the comparison of catalytic performance between In1-Co4 and Co3O4 at different pressures or H2/CO2 feeding ratio conditions. Typical reaction conditions: P = 4.0 MPa, T = 300 °C, GHSV = 24000 cm3STP gcat-1 h-1, H2/CO2 = 3 (unless otherwise specified), all catalysts were reduced under 20% H2/Ar at 300 °C for 2 h before reaction.

Fig. 3. Comparative structural characterizations of as-prepared and reduced catalysts. (a) XRD patterns; (b) XPS spectroscopy with core level Co 2p, Raman spectra (c) of as-prepared and reduced In1-Co4 catalyst; (d) H2-TPR of as-prepared catalysts.

Fig. 4. Morphological and structural characterizations of the reduced catalysts. TEM image (a) and high-resolution TEM image (b) of the reduced In1-Co4; (c) EDS line scan profile of reduced In1-Co4.

Fig. 5. CO2 adsorption ability over different catalysts. (a) CO2-TPD profiles of reduced catalysts; (b) CO2 adsorption DRIFTS spectra of different catalysts at 25 °C; (c) CO2 adsorption DRIFTS spectra of In1-Co4 at different temperatures.

Table 2 Infrared band assignments of the surface species on catalysts.

Surface species	Wavenumber (cm^-1)	assignment	Ref.
CO₂	2358	ν(C=O)	[51]
CH₄	3018	ν(C-H)	[51]
Carbonate *CO₃	1330	ν_s(OCO)	[24,47,48]
Carbonate *CO₃	1583	ν_as(OCO)	[24,47,48]
Bicarbonate *HCO₃	1236	ν_s(OCO)	[24,47,48]
	1429	δ(CH)	[24,47,48]
	1626, 1656	ν_as(OCO)	[24,47,48]
Formate *HCOO	1347-1355	ν_s(OCO)	[24,48,50]
	1382	δ(CH)	[24,48,50]
	1578-1581, 1642-1645	ν_as(OCO)	[24,48,50]
	2867-2875	ν(CH)	[24,48,50]
	2735, 2957-2964	δ(CH) + ν (OCO)	[24,48,50]
Methoxyl *CH₃O	1045-1049	ν(CH) of terminal *CH₃O	[24,48,51]
Methoxyl *CH₃O	2820-2827, 2935-2942	ν(CH₃)	[24,48,51]
*CO	2077	adsorbed linear CO species	[24,47,48]
Gaseous HCOOH	1083	δ(CH)	[52,53]
	1214	ν(CO)	[52,53]
	1789	ν(C=O)	[52,53]
	2939-2943	ν(CH) + δ(CH)	[52,53]
Adsorbed HCOOH	1119	ν(CO)	[52,53]
Adsorbed HCOOH	1749	ν(C=O)	[52,53]

Fig. 6. Dependence of CO2 conversion rate towards H2 partial pressure and CO2 partial pressure over reduced Co3O4 (a) and In1-Co4 (b). Reaction conditions: P = 4.0 MPa, T = 300 °C, H2/CO2 = 3, more details are in the supplementary materials.

Fig. 7. In-situ DRIFTS spectra of the CO2 + H2 reaction after CO2 adsorption on reduced Co3O4 (a) and In1-Co4 (b). Reaction conditions: P = 0.1 MPa, T = 250 °C, 5 mL/min CO2 + 15 mL/min H2, all catalysts were reduced under 20% H2/Ar at 300 °C for 2 h before reaction.

Fig. 8. HCOOH/CH3OH adsorption DRIFTS spectra on reduced Co3O4 and In1-Co4. HCOOH adsorption DRIFTS spectra on reduced Co3O4 (a) and In1-Co4 (b) at different temperatures. CH3OH adsorption DRIFTS spectra on reduced Co3O4 (c) and In1-Co4 (d) at different temperatures. All spectra were collected after introducing HCOOH/CH3OH for 30 min to ensure adsorption saturation; all catalysts were reduced under 20% H2/Ar at 300 °C for 2 h before the adsorption process.

Fig. 9. In-situ DRIFTS spectra of H2 reaction after CH3OH saturated adsorbed on reduced In1-Co4 and Co3O4. Reaction conditions: P = 0.1 MPa, T = 250 °C, methanol was first bubbled in for 30 min then the gas was switched to 15 mL/min H2 for further reaction; all catalysts were reduced under 20% H2/Ar at 300 °C for 2 h before the adsorption process.

Scheme 1. CO2 hydrogenation pathways on reduced Co3O4 and Inx-Coy catalysts.

Table 3 Performance comparison of different In-Co catalysts.

Catalyst	P (MPa)	T (°C)	H₂/CO₂ ratio	GHSV (cm³_STP g_cat^-1 h^-1)	In/Co ratio	CO₂ Conversion (%)	Methanol Selectivity (%)	rate_MeOH (g g_cat^-1 h^-1)	Ref.
In@Co-2	5	300	4	27500	1	17	80	0.86	[12]
MOF-derived In₂O₃@Co₃O₄	5	300	4	16500	3/4	20.5	65	0.65	[37]
50% In₂O₃/Co/C-N	2	300	3	3000	—	9.5	88.4	0.08	[36]
In₁-Co₄	4	300	3	24000	1/4	8.9	46.5	0.31	this work
In₁-Co₉	4	300	3	24000	1/9	8.2	43.5	0.30	this work

Scheme 2. Schematic adsorption-selectivity relationship for reduced Co3O4 and Inx-Coy catalysts in CO2 hydrogenation reactions.

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CO₂ hydrogenation selectivity shift over In-Co binary oxides catalysts: Catalytic mechanism and structure-property relationship

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