A triple-bed Na-FeAlOx/Zn-HZSM-5@SiO2 catalyst for the stable and direct generation of aromatics via CO2 hydrogenation

doi:10.1016/S1872-2067(25)64821-2

Abstract

Abstract:

The direct synthesis of aromatic compounds from the reduction of CO₂ remains challenging due to harsh operating conditions, low aromatic yields, and catalyst deactivation. A comprehensive understanding of the distance-induced optimal activity is therefore essential for achieving a rational spatial arrangement of multifunctional active sites for the hydrogenation of CO₂ to generate aromatic compounds. In this study, a triple-bed catalyst system is reported, which directly converts CO₂ into aromatic compounds with low CO emission levels. At a CO₂ conversion of 50.3%, the hydrocarbon pool contained 73.6% aromatic compounds while maintaining a moderately low CO selectivity of 13.9%. The BTEX (benzene, toluene, xylene, and ethylbenzene) selectivity within the aromatic products reached 67.8% and remained stable over 125 h, with only a slight decline being observed beyond this time. Compared to the mortar- and granular-mixed configurations, the triple-bed system exhibited a superior catalytic stability, likely due to the suppression of Na-induced poisoning on the zeolite acid sites. Additionally, the close contact between Fe and the zeolite structure altered the Fe phase evolution process for the chain extension reaction, while also significantly degrading the structural integrity of the zeolite. Under 370 °C and 3.5 MPa conditions, the zeolite crystallinity in the mortar-mixed 11% Na-promoted FeAlO_x/Zn-HZSM-5@SiO₂ catalyst dropped below 12%, whereas the double- and triple-bed configurations retained crystallinities of ~65%, which likely contributed to the improved catalyst longevity. These results indicate that the triple-bed configuration provides a promising route for enhancing the stability and efficiency of the direct hydrogenation reaction to generate aromatic compounds from CO₂.

Key words: CO₂ hydrogenation, Aromatic compounds, Proximity, Deactivation, Triple-bed catalyst

Wonjoong Yoon, Malayil Gopalan Sibi, Jaehoon Kim. A triple-bed Na-FeAlO_x/Zn-HZSM-5@SiO₂ catalyst for the stable and direct generation of aromatics via CO₂ hydrogenation[J]. Chinese Journal of Catalysis, 2026, 80: 330-346.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(25)64821-2

https://www.cjcatal.com/EN/Y2026/V80/I1/330

Figures/Tables 9

Table 1 Textural properties of the zeolite supports and composite catalysts determined from their N2 adsorption-desorption isotherms.

Catalyst	BET surface area ^a (m² g⁻¹)	Total pore volume ^b (cm³ g^-1)	Micropore volume ^c (cm³ g⁻¹)	Mesopore volume ^c (cm³ g⁻¹)	Average pore diameter (nm)
HZSM-5(12.5)	402.2	0.210	0.180	0.031	2.0
Zn-HZSM-5(12.5)	318.8	0.154	0.141	0.013	1.9
Reduced ZnZS	367.9	0.206	0.165	0.041	2.2
Spent TBM (250 h)	221.2	0.168	0.159	0.009	3.1
Spent TBB (250 h)	281.3	0.181	0.170	0.011	2.6

Fig. 1. (a) Hydrogenation of CO2 and the resulting hydrocarbon selectivity. (b) Detailed liquid hydrocarbon distribution over the 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (MM, Na11-FA?ZnZS), granular-mixed (GM, Na11-FA|ZnZS), dual-bed (DB, Na11-FA||ZnZS ), and triple-bed (TB, Na11-FA|||ZnZS) configurations. (c) Schematic representation of the various catalyst configurations. Pretreatment conditions: 450 °C, 3.5 MPa, H2 flow rate = 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 25 h. Note: The visual difference between the middle and bottom ZnZS layers in the TB configuration is due to limitations in the visualization setup using a glass TPD cell. Both layers contain identical ZnZS catalyst (0.5?g each) and were uniformly loaded in the actual stainless-steel reactor.

Fig. 2. Hydrogenation of CO2, hydrocarbon selectivity, and stability over the 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (Na11-FA?ZnZS) (a,b), granular-mixed (Na11-FA|ZnZS) (c,d), dual-bed (Na11-FA||ZnZS) (e,f), and triple-bed (Na11-FA|||ZnZS) (g,h) configurations. Pretreatment conditions: 450 °C, 3.5 MPa, H2 flow rate = 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, and 4000 mL g?1 h?1. Non-Aro C5+ = non-aromatic C5+ compounds. Aro = aromatic compounds.

Fig. 3. (a) XRD patterns of the reduced and spent 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (Na11-FA?ZnZS), granular-mixed (Na11-FA|ZnZS), dual-bed (Na11-FA||ZnZS), and triple-bed (Na11-FA|||ZnZS) configurations. Layer-position abbreviations used herein: DBT/DBB denote the top/bottom layers of the dual-bed (DB) configuration, and TBT/TBM/TBB denote the top/middle/bottom layers of the triple-bed (TB) configuration. Enlarged XRD patterns in the metal oxide region (b), carbide region (c), and zeolitic region (d,e). Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

Fig. 4. High-resolution XPS spectra in the C 1s region (a), Fe 2p region (b), and Na 1s region (c) for the spent 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (Na11-FA?ZnZS), granular-mixed (Na11-FA|ZnZS), dual-bed (Na11-FA||ZnZS), and triple-bed (Na11-FA|||ZnZS) configurations. Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

Fig. 5. NH3-TPD (a) and pyridine-DRIFT profiles (b) of the reduced 11%Na-FeAlOx (Na11-FA), Zn-HZSM-5(12.5)@SiO2 (ZnZS), and 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (Na11-FA?ZnZS) and granular-mixed (Na11-FA|ZnZS) configurations, along with those of the spent Na11-FA/ZnZS catalyst in the bottom bed of dual-bed (Na11-FA||ZnZS) configuration, and in the middle and bottom beds of the triple-bed (Na11-FA|||ZnZS) configuration. Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

Fig. 6. HR-TEM and HAADF images of the spent Na11-FA (250 h) (a), Na11-FA?ZnZS (150 h) (b), Na11-FA|ZnZS (150 h) (c), top bed Na11-FA||ZnZS (150 h) (d), and top bed Na11-FA|||ZnZS (250 h) (e) catalysts. Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

Fig. 7. HR-TEM and HAADF images of the spent bottom beds of the Na11-FA||ZnZS (150 h) (a) and Na11-FA|||ZnZS (250 h) (b) catalysts. Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

Fig. 8. TGA profiles of the spent 11%Na-FeAlOx (Na11-FA) (a) and 11%Na-FeAlOx/Zn-HZSM-5(12.5)@SiO2 (Na11-FA/ZnZS) catalysts in the mortar-mixed (Na11-FA?ZnZS) (b), granular-mixed (Na11-FA|ZnZS) (c), top bed of the dual-bed (Na11-FA||ZnZS) (d), bottom bed of the Na11-FA||ZnZS (e), top bed of the triple-bed (Na11-FA|||ZnZS) (f), middle bed of the Na11-FA|||ZnZS (g), and bottom bed configurations for the Na11-FA|||ZnZS (h) catalysts. Pretreatment conditions: 450 °C, 3.5 MPa, H2 50 mL min?1, 10 h. Reaction conditions: 370 °C, 3.5 MPa, H2/CO2 = 3:1, 4000 mL g?1 h?1, 150-250 h.

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A triple-bed Na-FeAlO_x/Zn-HZSM-5@SiO₂ catalyst for the stable and direct generation of aromatics via CO₂ hydrogenation

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