高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类

doi:10.1016/S1872-2067(26)65097-8

催化学报 ›› 2026, Vol. 87: 70-86.DOI: 10.1016/S1872-2067(26)65097-8

高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类

Jiyeon Lee^a^,¹, Muhammad Irshad^a^,^e^,¹, Wonjoong Yoon^a, Jaehoon Kim^a^,^b^,^c^,^d^,^*()

^a 成均馆大学化学工程学院, 京畿道水原市, 韩国
^b 成均馆大学机械工程学院, 京畿道水原市, 韩国
^c 成均馆大学SKKU纳米技术高级研究所(SAINT), 京畿道水原市, 韩国
^d 成均馆大学低碳能源工程, 京畿道水原市, 韩国
^e 国家化学研究所无碳技术开发、示范和培训中心, 卢布尔雅那, 斯洛文尼亚

收稿日期:2025-11-27 接受日期:2026-01-20 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: jaehoonkim@skku.edu (J. Kim).
作者简介:¹共同第一作者.

High-pressure switch: Redirecting CO₂ hydrogenation from hydrocarbons to carboxylic acids and alcohols

Jiyeon Lee^a^,¹, Muhammad Irshad^a^,^e^,¹, Wonjoong Yoon^a, Jaehoon Kim^a^,^b^,^c^,^d^,^*()

^a School of Chemical Engineering, Sungkyunkwan University, 2066, Seobu-Ro, Jangan-Gu, Sueon, Gyeong Gi-Do 16419, Republic of Korea
^b School of Mechanical Engineering, Sungkyunkwan University, 2066, Seobu-Ro, Jangan-Gu, Suwon, Gyeong Gi-Do 16419, Republic of Korea
^c SKKU Advanced Institute of Nanotechnology (SAINT), Sungkyunkwan University, 2066, Seobu-Ro, Jangan-Gu, Suwon, Gyeong Gi-Do 16419, Republic of Korea
^d Low-carbon Energy Engineering, Sungkyunkwan University, 2066, Seobu-Ro, Jangan-Gu, Suwon, Gyeong Gi-Do 16419, Republic of Korea
^e Center for Development, Demonstration and Training for Carbon-Free Technologies, National Institute of Chemistry, Hajdrihova 19, SI-1000 Ljubljana, Slovenia

Received:2025-11-27 Accepted:2026-01-20 Online:2026-08-18 Published:2026-06-24
About author:¹Contributed equally to this work.

摘要/Abstract

摘要：

在二氧化碳(CO₂)催化转化制备高附加值化学品的研究中, 如何实现对反应路径与产物选择性的精准调控仍是多相催化领域的关键挑战. 本文以钾改性氧化铁(K-Fe₂O₃)为模型催化剂, 系统揭示了反应压力在CO₂加氢过程中对铁基催化剂物相演化及反应机理的决定性作用. 在0.1-10.0 MPa宽压力范围内的催化性能评价结果表明,低压至中等压力(< 3.5 MPa)下, 催化剂表面以Fe₅C₂为主, 该相能够有效促进费托合成(Fischer-Tropsch synthesis, FTS)型C-C偶联过程, 从而实现长链烃类的高选择性生成; 而在高压环境(≥ 7.0 MPa)下, Fe₅C₂逐渐转化为FeCO₃物相, 伴随Fe-O配位强度增强及表面碳酸盐物种积累. 综合X射线衍射(XRD)、穆斯堡尔谱、高分辨透射电子显微与元素分析(HR-TEM/EDX)、X射线吸收光谱(XAS)及X射线光电子能谱(XPS)等多维表征结果证实,K-Fe₂O₃存在显著的压力依赖性相变, FeCO₃在高压条件下成为主导相, 并对CO活化呈惰性. 原位漫反射红外傅里叶变换光谱(operando DRIFTS)和CO程序升温表面反应(CO-TPSR)实验进一步表明, FeCO₃能够稳定含COO中间体并抑制C-O键断裂, 从而阻断传统FTS链增长路径, 转而促进直接的COO插入反应, 实现产物选择性由烃类向含氧化合物(高级醇和羧酸)转变. 性能测试结果显示,中等压力下C₅⁺烃产率最高, 而高压下含氧化合物选择性显著提升, 验证了压力诱导的相变对产物分布的调控效应.

本研究不仅阐明了高压CO₂环境下铁基催化剂的结构重构机制, 还为调节CO₂加氢反应中的含氧化合物选择性提供了一种无需依赖贵金属或复杂催化剂构型的新策略. 为工业高压条件下CO₂定向转化制高值化学品提供了理论依据与技术参考.

关键词: CO₂加氢, 高压催化, Fe₅C₂-FeCO₃相变, 含氧化合物选择性, 钾促进铁催化剂

Abstract:

The selective conversion of CO₂ into value-added chemicals remains a critical challenge in heterogeneous catalysis. Here, we demonstrate that reaction pressure governs a decisive mechanistic switch in CO₂ hydrogenation over potassium-promoted iron catalysts. Catalytic tests conducted from 0.1 to 10.0 MPa reveal that moderate pressure (3.5 MPa) favors Fischer-Tropsch-type pathways, yielding long-chain hydrocarbons through Fe₅C₂-mediated C-C coupling. In contrast, elevated pressures (≥ 7.0 MPa) suppress hydrocarbon formation and promotes the production of long-chain oxygenates, including higher alcohols and carboxylic acids. Comprehensive structural characterization indicates a clear pressure-dependent phase transformation: Fe₅C₂ progressively diminishes and evolves into FeCO₃, accompanied by increased Fe-O and carbonate surface species. Operando diffuse reflectance infrared Fourier transform spectroscopy reveals that FeCO₃-rich surfaces stabilize COO-containing intermediates and inhibit C-O bond scission, favoring direct COO insertion rather than Fischer-Tropsch chain growth. CO-temperature programmed surface reaction further confirms that FeCO₃ is catalytically inert toward CO activation, explaining the reduced CO₂ conversion observed at high pressure. The combined results establish FeCO₃ as a pressure-generated phase that redirects CO₂ hydrogenation from hydrocarbon-selective to oxygenate-selective pathways. This work provides mechanistic insight into pressure-driven catalyst restructuring and offers a new strategy for tuning oxygenate selectivity in CO₂ hydrogenation.

Key words: CO₂ hydrogenation, High-pressure catalysis, Fe₅C₂-FeCO₃ phase transformation, Oxygenate selectivity, Potassium-promoted iron catalysts

Jiyeon Lee, Muhammad Irshad, Wonjoong Yoon, Jaehoon Kim. 高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类[J]. 催化学报, 2026, 87: 70-86.

Jiyeon Lee, Muhammad Irshad, Wonjoong Yoon, Jaehoon Kim. High-pressure switch: Redirecting CO₂ hydrogenation from hydrocarbons to carboxylic acids and alcohols[J]. Chinese Journal of Catalysis, 2026, 87: 70-86.

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Fig. 1. (a) Catalytic performance of K-Fe2O3 during 100 h of on-stream CO2 hydrogenation at various reaction pressures. (b) Distribution of oxygenated products as a function of pressure. (c) STY of total oxygenates (carboxylic acids and alcohols) at different reaction pressures. (d) Digital photographs of liquid-phase products collected at each pressure. (e) Oxygenate distribution as a function of time under selected reaction conditions. (f) Catalytic performance at various reaction temperatures. Calcination at 600 °C with a ramp rate of 1.6 °C min?1 for 6 h under static air; Reduction at 450 °C and 3.5 MPa under H2 flow (50 mL min?1) for 12 h; CO2 hydrogenation at 330 °C, 0.1-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 2. (a) XRD patterns of the calcined, reduced, and spent K-Fe2O3 catalysts obtained after CO2 hydrogenation at different reaction pressures. (b) Enlarged view of selected XRD regions from Fig. 2a highlighting the evolution of iron phases with pressure. Calcination at 600 °C with a ramp rate of 1.6 °C min?1 for 6 h under static air; Reduction at 450 °C and 3.5 MPa under H2 flow (50 mL min?1) for 12 h; CO2 hydrogenation at 330 °C, 0.1-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 3. (a-c) Spectral phase compositions derived from the 57Fe Mössbauer spectra of the spent catalysts obtained after CO2 hydrogenation at reaction pressures corresponding to KFe35 (3.5 MPa), KFe70 (7.0 MPa), and KFe100 (10.0 MPa), respectively. (d) Quantitative phase fractions of Fe-containing species extracted from the Mössbauer spectra as a function of reaction pressure. CO2 hydrogenation at 330 °C, 0.1-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 4. SEM and HR-TEM images of the spent K-Fe2O3 catalysts after 100 h of CO2 hydrogenation at reaction pressures corresponding to KFe35 (a,d), KFe70 (b,e), and KFe100 (c,f). High-angle Annular Dark-Field-STEM images and their corresponding EDX elemental maps of KFe35 (g), KFe70 (h), and KFe100 (f). (j) Schematic illustration of the structural transformation of the catalyst with increasing reaction pressure, showing the transition from Fe5C2-rich to FeCO3-rich states. CO2 hydrogenation at 330 °C, 0.1-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 5. (a) Normalized Fe K-edge XANES spectra of the spent catalysts compared with reference materials (dotted lines). (b) k3-weighted Fourier transforms of the normalized Fe K-edge EXAFS spectra, highlighting the evolution of local Fe coordination environments. CO2 hydrogenation at 330 °C, 0.1-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 6. XPS spectra of the calcined, reduced, and spent K-Fe2O3 catalysts in the regions corresponding to Fe 2p (a), O 1s (b), and K 2p and C 1s (c). Calcination at 600 °C with a ramp rate of 1.6 °C min?1 for 6 h under static air; Reduction at 450 °C and 3.5 MPa under H2 flow (50 mL min?1) for 12 h; CO2 hydrogenation at 330 °C, 3.5-10.0 MPa, H2/CO2 = 3, and GHSV = 6000 mL g?1 h?1 for 100 h.

Fig. 7. CO-TPSR activity test for FeCO3. (a) TCD signal obtained during H2-assisted CO-TPSR. (b-d) QMS profiles corresponding to gaseous species desorbed or evolved from the catalyst surface during CO-TPSR.

Fig. 8. CO2-DRIFTS spectra of the spent KFe35 (a) and KFe100 (b) catalysts recorded under CO2 adsorption and subsequent H2 exposure. QMS profiles of desorbed or evolved gaseous species during the operando DRIFTS experiments for KFe35 (c,d) and KFe100 (e,f), highlighting differences in surface reactivity under identical conditions.

Fig. 9. Plausible reaction mechanisms for CO2 conversion over the K-Fe2O3 catalyst under different reaction pressures, illustrating the transition from Fe5C2-driven Fischer-Tropsch chain growth at mild pressure to FeCO3-mediated COO-insertion pathways at elevated pressure.

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高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类

High-pressure switch: Redirecting CO₂ hydrogenation from hydrocarbons to carboxylic acids and alcohols

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高压开关: 将二氧化碳加氢产物从碳氢化合物转向羧酸和醇类

High-pressure switch: Redirecting CO2 hydrogenation from hydrocarbons to carboxylic acids and alcohols

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High-pressure switch: Redirecting CO₂ hydrogenation from hydrocarbons to carboxylic acids and alcohols