低二氧化铈含量兼具优异性能: 低温逆水煤气变换多组分CuFeCe/γ-Al2O3催化剂的原位光谱研究

doi:10.1016/S1872-2067(26)65221-7

催化学报 ›› 2026, Vol. 91: 176-191.DOI: 10.1016/S1872-2067(26)65221-7

低二氧化铈含量兼具优异性能: 低温逆水煤气变换多组分CuFeCe/γ-Al₂O₃催化剂的原位光谱研究

闵灯^a^,^b, Cisneros Sebastian^a^,^*(), Rabee Abdallah I. M.^c^,^d, Vuong Thanh Huyen^c, 肖家栋^e, 张耀远^f, 蔡鎔声^g, 石峰^a^,^*(), Rabeah Jabor^a^,^c^,^*()

^a 中国科学院兰州化学物理研究所, 低碳催化与二氧化碳利用全国重点实验室, 甘肃兰州 730000, 中国
^b 中国科学院大学, 北京 100049, 中国
^c 莱布尼茨催化研究所, 罗斯托克, 德国
^d 米尼亚大学理学院化学系, 米尼亚, 埃及
^e 中国科学院大学化学工程学院, 北京 101408, 中国
^f 北京理工大学化学与化工学院, 北京 100081, 中国
^g 中国科学院兰州化学物理研究所, 润滑材料全国重点实验室, 甘肃兰州 730000, 中国

收稿日期:2026-04-08 接受日期:2026-06-06 出版日期:2026-12-18 发布日期:2026-10-13
通讯作者: ^*电子信箱: jabor.rabeah@licp.cas.cn (J. Rabeah),
fshi@licp.cas.cn (石峰),
sebastian.cisneros@licp.cas.cn (S. Cisneros).
基金资助:
中国科学院战略性先导科技专项(XDB1500102);甘肃省科技计划(24ZD13FA002)

Low CeO₂ content with superior performance: In-situ spectroscopic insights into multicomponent CuFeCe/γ-Al₂O₃ catalysts for mild-temperature reverse water-gas shift

Deng Min^a^,^b, Sebastian Cisneros^a^,^*(), Abdallah I. M. Rabee^c^,^d, Thanh Huyen Vuong^c, Jiadong Xiao^e, Yaoyuan Zhang^f, Rongsheng Cai^g, Feng Shi^a^,^*(), Jabor Rabeah^a^,^c^,^*()

^a State Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization, Lanzhou Institute of Chemical Physics Chinese Academy of Sciences, Lanzhou 730000, Gansu, China
^b University of Chinese Academy of Sciences, Beijing 100049, China
^c Leibniz-Institut für Katalyse, Rostock 18059, Germany
^d Chemistry Department, Faculty of Science, Minia University, El-Minia 61519, Egypt
^e School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing 101408, China
^f Chemistry and Chemical Engineering, Beijing Institute of Technology, Beijing 100081, China
^g State Key Laboratory of Solid Lubrication, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, Gansu, China

Received:2026-04-08 Accepted:2026-06-06 Online:2026-12-18 Published:2026-10-13
Supported by:
Strategic Priority Research Program of the Chinese Academy of Science(XDB1500102);Project of Gansu Province-China(24ZD13FA002)

摘要/Abstract

摘要：

一氧化碳(CO)是合成高附加值化学品的关键前驱体, 通过逆水煤气变换反应(RWGSR)制备CO是实现碳中和目标的核心技术路径之一. 尽管高性能RWGSR催化剂的设计与合成已取得显著进展, 但其实际应用仍面临两大核心瓶颈: 一方面, 高活性贵金属(如铂)和稀土元素(如铈)成本高昂且全球供应链受限; 另一方面, 该吸热反应需在400 °C以上高温进行, 易导致活性位点烧结与失活. Cu基催化剂因成本低廉、初始活性高成为贵金属催化剂的主流替代方案, 但仍存在烧结和积碳问题. Fe掺杂可有效缓解积碳失活, 但对Cu烧结抑制效果有限; 将Cu负载于高比表面积γ-Al₂O₃载体可部分解决烧结问题, 然而Cu-Al₂O₃相互作用较弱, 无法长期稳定Cu纳米颗粒并维持对反应至关重要的Cu⁺/Cu⁰氧化还原对.
CeO₂作为一种多功能载体显示出独特优势, 其高还原性、储氧能力及氧迁移率可促进强的金属-载体相互作用, 并提升包括Cu在内的多种负载金属上的CO生成效率. 由于它在众多应用中的巨大需求, 已被归为关键原材料类别. 因此, 必须建立“低CeO₂负载量”催化剂的设计策略, 在保持高催化活性、选择性、稳定性的同时, 确保RWGSR过程的可持续性与经济性. 本文报道了一种多组分、低Ce负载量的CuFeCe/γ-Al₂O₃催化剂(实际负载量: Cu=0.84 wt%, Fe=0.46 wt%, Ce=4.5 wt%). 在380 °C该催化剂实现了约47 mmol·g_cat^-1 h^-1的CO生成速率, 选择性> 99%, 在相似条件下超越了以CeO₂为载体的催化剂性能. 利用原位漫反射红外光谱、原位电子顺磁共振及非原位X-射线光电子能谱, 证明了催化剂的优异活性源于Cu单位点与小尺寸的Cu⁰团簇的共存, 这些物种由FeOₓ团簇和邻近的氧空位(O_v)所稳定, 而氧空位则与高度分散于γ-Al₂O₃上的CeOₓ纳米颗粒(NPs)相关联. 邻近Ce³⁺的Cu单位点在Cu²⁺与Cu⁺之间快速氧化还原穿梭, 实现CO₂活化, 而Cu⁰团簇则促进H₂解离. 而且, 在Cu-Fe-Ce三种物种的界面处还存在通过桥连甲酸中间体的氢辅助反应路径, 实现CO的高效生成. 与单金属及双金属对照催化剂相比, 三金属催化剂的催化活性提升显著. 115 h长期稳定性测试显示, 催化剂具有可逆再活化特性, 表明其在动态操作条件下具有良好的耐用性. 本实验条件下基本可以排除Fe碳化物等含碳物相引发的不可逆结构重构. 总之, 通过系统改变催化剂组成发现, 最高的CO生成速率源自Cu-Fe-Ce相互作用位点所形成的独特微环境. 在反应条件下, 该微环境促进了额外活性位点与中间体(如氧空位和桥式甲酸盐)的生成.
对于未来的研究, 探索这一催化剂设计理念在高压条件下的应用将颇具意义, 因为高压环境涉及催化剂的结构重组及竞争反应. 例如, 高压RWGSR在热力学上相较于甲烷化反应极为不利, 而C-C偶联过程将导致活性位点上发生更严重的积碳. 这些问题对有效的工艺集成构成了挑战, 值得深入研究.

关键词: 逆水煤气变换反应, 二氧化碳, 低负载铈催化剂, 原位光谱表征, 氧空位, 桥式甲酸盐

Abstract:

CO is a key precursor for high-value-added chemicals, and its production via the reverse water-gas shift reaction is crucial for carbon-neutral processes. Herein, we report on a multicomponent low Ce-containing CuFeCe/γ-Al₂O₃ catalyst (actual loading Cu=0.84 wt%, Fe=0.46 wt% and Ce=4.5 wt%) which achieves CO formation rate of ca. 47 mmol g_cat^-1 h^-1 with > 99% selectivity at 380 °C, surpassing the performance of bulk CeO₂-based catalysts under similar conditions. Using in-situ diffuse reflectance infrared Fourier transform spectroscopy, in-situ electron paramagnetic resonance and ex-situ X-ray photoelectron spectroscopy, we demonstrate that the superior activity arises from the coexistence of Cu single sites and small Cu⁰ clusters, stabilized by FeO_x clusters and neighboring O-vacancies (O_v) associated with highly dispersed CeO_x nanoparticles on γ-Al₂O₃. Cu single sites vicinal to Ce³⁺ rapidly shuttle between Cu²⁺ and Cu⁺, activating CO₂ while Cu⁰ clusters facilitate H₂ dissociation. In addition to direct CO₂ activation, H-assistance pathway via a bridged formate intermediate contributes to CO formation, preferentially at the interfaces shared by Cu, Fe, and Ce species. Compared to monometallic and bimetallic analogs, the trimetallic catalyst exhibits markedly higher activity. Long-term tests (115 h) reveal reversible re-activation cycles, demonstrating the catalyst’s robustness under dynamic operating conditions.

Key words: Reverse water-gas shift reaction, Carbon dioxide, Low Ce-containing catalyst, In-situ spectroscopy characterization, Oxygen vacancies, Bridged formate

闵灯, Cisneros Sebastian, Rabee Abdallah I. M., Vuong Thanh Huyen, 肖家栋, 张耀远, 蔡鎔声, 石峰, Rabeah Jabor. 低二氧化铈含量兼具优异性能: 低温逆水煤气变换多组分CuFeCe/γ-Al₂O₃催化剂的原位光谱研究[J]. 催化学报, 2026, 91: 176-191.

Deng Min, Sebastian Cisneros, Abdallah I. M. Rabee, Thanh Huyen Vuong, Jiadong Xiao, Yaoyuan Zhang, Rongsheng Cai, Feng Shi, Jabor Rabeah. Low CeO₂ content with superior performance: In-situ spectroscopic insights into multicomponent CuFeCe/γ-Al₂O₃ catalysts for mild-temperature reverse water-gas shift[J]. Chinese Journal of Catalysis, 2026, 91: 176-191.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65221-7

https://www.cjcatal.com/CN/Y2026/V91/I12/176

图/表 12

Table 1 Structural properties of the distinct catalysts and bare γ-Al2O3 support.

Catalyst	Cu/wt% (1.0)^a	Ce/wt% (5.0)	Fe/wt% (0.5)	SSA/ m² g^-1	Average pore size/nm
Cu/γ-Al₂O₃	0.87	—	—	130	26.1
CuCe/γ-Al₂O₃	0.85	3.3	—	137	25.9
CuFe/γ-Al₂O₃	0.91	—	0.49	130	27.4
CuFeCe/γ-Al₂O₃	0.84	4.5	0.46	130	28.5
FeCe/γ-Al₂O₃	—	4.1	0.41	146	22.4
Fe/γ-Al₂O₃	—	—	0.48	—^b	—
γ-Al₂O₃	—	—	—	144	23.3

Fig. 1. Selected HAADF-STEM images of the catalysts before (a-c) and after (d-f) reaction. The dashed white circles enclose possible clusters of Cu species.

Fig. 2. Representative HAADF-STEM images of the fresh (a,c) and spent (b,d) Ce-containing catalysts indicating the presence of CeO2 (111), (200) and (311) planes.

Fig. 3. (a) CO rate (mass-normalized) over the catalysts after 12 h at the corresponding temperature (CO2 conversion < 20%). Reaction conditions: P=1 bar, CO2:H2=1:3, GHSV=36000 mL g-1 h-1. (b) Apparent activation energy for CO production over the catalysts in the range 340-380 °C. (c) Long-term stability at 380 °C over CuFeCe/γ-Al2O3. Red arrows indicate catalyst reactivation by oxidation (5% O2 in N2, 15 min) and re-reduction (50% H2 in N2, 15 min). Error bars represent the standard deviation of two independent experiments under identical conditions.

Fig. 7. (a-c) CO adsorption DRIFTS spectra obtained over the pre-reduced catalysts under 1% CO in He (25 mL min-1) during 15 min (purple spectra) and under 100% He (25 mL min-1) during 15 min (orange spectra). (d-f) CO adsorption DRIFT spectra computed after subtracting the spectrum collected after CO saturation from the spectra recorded under 100% He. All the spectra were recorded at RT.

Table 2 Kinetic parameters for the oxidation/reduction of Cu2+ sites over Cu/γ-Al2O3 and CuCe/γ-Al2O3 estimated by fitting the respective time evolution of the EPR second integrals of the spectra during distinct gas atmosphere switches.

Gas switch	Cu/γ-Al₂O₃		CuCe/γ-Al₂O₃		CuFeCe/γ-Al₂O₃
Gas switch	k₁₁/min^-1	k₂₁/min^-1	k₁₂/min^-1	k₂₂/min^-1	k₁₃/min^-1	k₂₃/min^-1
100% He → 50% H₂in He	0.63	0.014	0.49	0.017	—	—
50% H₂ in He → 15% CO₂ in He	0.35	0.016	0.15	0.025	0.71^a	0.048^a
15% CO₂ in He → 50% H₂ in He	0.38	0.011	0.40	0.010	—	—
50% H₂ in He → H₂ + CO₂ (3:1)	0.33	0.28	0.35	0.22	0.13^a	0.34^a

Fig. 4. (a) XPS spectra in the Cu 2p region of fresh Cu/γ-Al2O3, CuCe/γ-Al2O3, and CuFeCe/γ-Al2O3. (b) XPS spectra in the Ce 3d region of fresh CuCe/γ-Al2O3 and CuFeCe/γ-Al2O3. The percentages represent the atomic surface fractions estimated for the respective cations.

Fig. 5. (a-c) In-situ DRIFTS spectra recorded during 15 min at 350 °C over the distinct catalysts. RWGSR conditions: 25 mL min-1, 15% CO2, 45% H2 and balance He. The time separation between 2 consecutive spectra corresponds to 1 min.

Fig. 6. DRIFTS spectra recorded during 15 min at 350 °C over the distinct catalysts after switch from SS-RWGSR to 50% H2 in He (a-c), and after switch from SS-RWGSR to 100% He (d-f). The time separation between 2 consecutive spectra corresponds to 1 min.

Fig. 8. In-situ EPR spectra recorded during reduction in 50% H2 in He (a-c) and during gas switch from 50% H2 in He to 15% CO2 in He (d-f) over the distinct catalysts. All the spectra were recorded at 350 °C and flow rate of 25 mL min-1. The time separation between 2 consecutive spectra corresponds to 1 min.

Fig. 9. In-situ EPR spectra recorded at 350 °C during the switch from 15% CO2 in He to 50% H2 in He (a-c) and from 50% H2 in He to RWGSR conditions (d-f) over the distinct catalysts (flow rate of 25 mL min-1). The time separation between 2 consecutive spectra corresponds to 1 min.

Scheme 1. Proposed active sites and operative mechanisms for the RWGSR occurring on the CuFeCe/γ-Al2O3 catalyst.

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低二氧化铈含量兼具优异性能: 低温逆水煤气变换多组分CuFeCe/γ-Al₂O₃催化剂的原位光谱研究

Low CeO₂ content with superior performance: In-situ spectroscopic insights into multicomponent CuFeCe/γ-Al₂O₃ catalysts for mild-temperature reverse water-gas shift

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