CO2加氢反应诱导过程中In2O3催化剂结构演变的实验和理论研究

doi:10.1016/S1872-2067(25)64657-2

催化学报 ›› 2025, Vol. 72: 301-313.DOI: 10.1016/S1872-2067(25)64657-2

CO₂加氢反应诱导过程中In₂O₃催化剂结构演变的实验和理论研究

蔚张茜^a^,^b^,¹, 王明秀^a^,^b^,¹, 路昕楠^a^,^b^,^*(), 周紫璇^a^,^b, 唐梓祁^a^,^c, 常春然^e, 杨永^c, 李圣刚^a^,^b^,^c^,^d^,^*(), 高鹏^a^,^b^,^d^,^*()

^a中国科学院上海高等研究院, 低碳转化科学与工程中心, 上海 201210
^b中国科学院大学, 北京 100049
^c上海科技大学物质科学与技术学院, 上海 201210
^d中国科学院上海高等研究院院, 低碳催化与二氧化碳利用全国重点实验室, 上海 201210
^e西安交通大学化学工程学院, 陕西省能源化工过程强化重点实验室, 陕西西安 710049

收稿日期:2024-11-15 接受日期:2025-03-05 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: luxn@sari.ac.cn (路昕楠),lisg@sari.ac.cn (李圣刚),gaopeng@sari.ac.cn (高鹏).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2024YFB4006600)

An experimental and computational investigation on structural evolution of the In₂O₃ catalyst during the induction period of CO₂ hydrogenation

Zhangqian Wei^a^,^b^,¹, Mingxiu Wang^a^,^b^,¹, Xinnan Lu^a^,^b^,^*(), Zixuan Zhou^a^,^b, Ziqi Tang^a^,^c, Chunran Chang^e, Yong Yang^c, Shenggang Li^a^,^b^,^c^,^d^,^*(), Peng Gao^a^,^b^,^d^,^*()

^aCenter for Low-Carbon Conversion Science and Engineering, Shanghai Advanced Research Institute, Chinese Academy of Sciences, Shanghai 201210, China
^bUniversity of the Chinese Academy of Sciences, Beijing 100049, China
^cSchool of Physical Science and Technology, Shanghai Tech University, Shanghai 201210, China
^dState Key Laboratory of Low Carbon Catalysis and Carbon Dioxide Utilization, Shanghai Advanced Research Institute, Chinese Academy of Sciences, Shanghai 201210, China
^eShaanxi Key Laboratory of Energy Chemical Process Intensification, School of Chemical Engineering and Technology, Xi’an Jiaotong University, Xi’an 710049, Shaanxi, China

Received:2024-11-15 Accepted:2025-03-05 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: luxn@sari.ac.cn (X. Lu), lisg@sari.ac.cn (S. Li), gaopeng@sari.ac.cn (P. Gao).
About author:¹Contributed to this work equally.
Supported by:
National Key R&D Program of China(2024YFB4006600)

摘要/Abstract

摘要：

二氧化碳作为一种可广泛获取、廉价、无毒、无害的碳源, 能够在催化剂的辅助下与绿氢结合生产大宗化学品和甲醇等液体燃料. 甲醇合成是二氧化碳工业利用中最重要的可行方法之一, 该路线能够为生产绿色燃料和化学品提供平台, 拥有实现碳循环和回收的巨大潜力. 氧化铟(In₂O₃)作为一种高效催化二氧化碳加氢制甲醇的催化剂, 具有耐高温稳定性好等特点, 已经引起了极大的关注. 基于In₂O₃的二氧化碳加氢制甲醇催化剂已取得较大进展, 但仍存在转化率偏低、反应过程中存在逆水煤气变换反应生成一氧化碳副产物等问题. 了解结构-活性关系, 开发更高效的In₂O₃基催化剂, 亟需对实际反应条件下活性位点的演变有深入的了解. 本文旨在通过实验研究、密度泛函理论(DFT)计算和微动力学模拟相结合的方法, 捕捉活性位点在初始阶段的演变, 并将其与稳定阶段的催化剂结构进行比较.

本文通过沉积沉淀法制备了立方相In₂O₃纳米颗粒, 并评价了其催化二氧化碳加氢制备甲醇反应性能. 在反应开始的10 h内, 二氧化碳转化率逐渐升高, 甲醇选择性缓慢下降, 至20 h后达到平衡. 该催化剂的激活和诱导阶段存在In₂O₃纳米颗粒的烧结和在In₂O₃表面更多氧空位的生成. 进一步实验研究表明, 氢诱导使催化剂在活化阶段产生了额外的氧空位, 提高了In₂O₃催化剂的二氧化碳加氢性能. DFT计算和微观反应动力学模拟进一步表明, 在诱导期形成的氧空位覆盖率较高的表面或羟基化表面可以加快反应速率, 提高二氧化碳转化率. 然而, 它们主要促进一氧化碳生成而不是甲醇的形成, 因而导致甲醇选择性降低, 与实验结果一致.

综上, 本文深入探究了In₂O₃纳米催化剂上二氧化碳加氢过程的诱导阶段, 为显著提高In₂O₃基催化剂的二氧化碳反应活性并保持长期稳定性提供了有价值的见解.

关键词: 氧化铟, 二氧化碳加氢, 甲醇生产, 诱导和活化, 结构演化

Abstract:

As one of the most important industrially viable methods for carbon dioxide (CO₂) utilization, methanol synthesis serves as a platform for production of green fuels and commodity chemicals. For sustainable methanol synthesis, In₂O₃ is an ideal catalyst and has garnered significant attention. Herein, cubic In₂O₃ nanoparticles were prepared via the precipitation method and evaluated for CO₂ hydrogenation to produce methanol. During the initial 10 h of reaction, CO₂ conversion gradually increased, accompanied by a slow decrease of methanol selectivity, and the reaction reached equilibrium after 10-20 h on stream. This activation and induction stage may be attributed to the sintering of In₂O₃ nanoparticles and the creation of more oxygen vacancies on In₂O₃ surfaces. Further experimental studies demonstrate that hydrogen induction created additional oxygen vacancies during the catalyst activation stage, enhancing the performance of In₂O₃catalyst for CO₂ hydrogenation. Density functional theory calculations and microkinetic simulations further demonstrated that surfaces with higher oxygen vacancy coverages or hydroxylated surfaces formed during this induction period can enhance the reaction rate and increase the CO₂ conversion. However, they predominantly promote the formation of CO instead of methanol, leading to reduced methanol selectivity. These predictions align well with the above-mentioned experimental observations. Our work thus provides an in-depth analysis of the induction stage of the CO₂ hydrogenation process on In₂O₃ nano-catalyst, and offers valuable insights for significantly improving the CO₂ reactivity of In₂O₃-based catalysts while maintaining long-term stability.

Key words: In₂O₃, CO₂ hydrogenation, Methanol production, Induction and activation, Structural evolution

蔚张茜, 王明秀, 路昕楠, 周紫璇, 唐梓祁, 常春然, 杨永, 李圣刚, 高鹏. CO₂加氢反应诱导过程中In₂O₃催化剂结构演变的实验和理论研究[J]. 催化学报, 2025, 72: 301-313.

Zhangqian Wei, Mingxiu Wang, Xinnan Lu, Zixuan Zhou, Ziqi Tang, Chunran Chang, Yong Yang, Shenggang Li, Peng Gao. An experimental and computational investigation on structural evolution of the In₂O₃ catalyst during the induction period of CO₂ hydrogenation[J]. Chinese Journal of Catalysis, 2025, 72: 301-313.

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图/表 8

Fig. 1. Comparison of CO2 conversion (XCO2), methanol selectivity (SCH3OH) and methanol STY over In2O3 catalysts as a function of pressure (a), temperature (b), and time on stream (c). Reaction conditions: H2/CO2 = 3, GHSV = 7200 mL h?1 gcat?1, and (a) 300°C, 1-5 MPa, (b) 220-300 °C, 5 MPa, (c) 300 °C, 5 MPa.

Fig. 2. XRD patterns of In2O3 under different situations.

Fig. 3. TEM images of In2O3 under various conditions: fresh (a), 1 h (b), 5 h (c), 10 h (d), 20 h (e), and 40 h (f), where insets are the corresponding In2O3 particle size distributions.

Table 1 Texture properties of the In2O3 samples under various conditions.

Sample	Spent time (h)	S_BET ^a (m² g^-1)	Pore volume ^b (cm³ g^-1)	Pore width ^c (nm)
Fresh	0	129	0.25	7.8
1 h	1	28	0.22	31.2
5 h	5	35	0.23	31.0
10 h	10	37	0.22	31.1
20 h	20	30	0.19	31.3
40 h	40	28	0.23	30.9

Fig. 4. BET adsorption-desorption isotherms (a) and pore size distributions (b) of In2O3 under different situations. (c) CO2-TPD profiles for In2O3 under various conditions (CO2 was adsorbed without any pretreatment of the In2O3 samples). (d) H2-TPR profiles for In2O3 under various conditions.

Fig. 5. (a) Visible Raman spectra of the In2O3 catalysts under various conditions, where inset is the comparison of the relative amount of oxygen vacancies according to the I2/I1 ratio. (b) XPS spectra of O 1s for In2O3 under various situations with the percentages of the lattice and defect oxygen sites shown.

Fig. 6. (a) Top views of In2O3 (111)-one-VO, (111)-all-VO and (111)-33%-H model surfaces with the blue circle representing VO. (b,c) Pathways of methanol and CO formations with the energy barriers of the elementary steps (_D represents the defective surface with VO, _P represents the surface where the VO is filled by O, and * stands for the adsorption site).

Fig. 7. (a) Reaction rates predicted from microkinetic simulations. (b) Product selectivity predicted for the (111)-one-VO surface. (c) Product selectivities predicted for the (111)-all-VO, (111)-33%-H and (110)-33%-H surfaces, which are all similar. (d,e,f) DRC values from the microkinetic simulations for the (111)-one-VO, (111)-all-VO, and (111)-33%-H surfaces. Elementary reactions involved in the microkinetic simulations are shown in Table S5, and the energetics and harmonic frequencies for the studied surfaces are given in Tables S6-S9.

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CO₂加氢反应诱导过程中In₂O₃催化剂结构演变的实验和理论研究

An experimental and computational investigation on structural evolution of the In₂O₃ catalyst during the induction period of CO₂ hydrogenation

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