CeAlO3镶嵌镍纳米颗粒抗积碳甲烷干重整催化剂

doi:10.1016/S1872-2067(26)65063-2

催化学报 ›› 2026, Vol. 87: 363-375.DOI: 10.1016/S1872-2067(26)65063-2

CeAlO₃镶嵌镍纳米颗粒抗积碳甲烷干重整催化剂

马忠臣^a, 尹美怡^a, 徐润^b, 张荣俊^b, 兰天^a, 顾文丽^a, 陈国庆^a, 路勇^a^,^c^,^*()

^a 华东师范大学化学与分子工程学院, 石油化工分子转化与反应工程全国重点实验室, 上海市绿色化学与化工过程绿色化重点实验室, 上海 200062
^b 中石化石油化工科学研究院有限公司, 北京 100083
^c 崇明生态研究院, 上海 202151

收稿日期:2025-11-19 接受日期:2025-12-22 出版日期:2026-08-18 发布日期:2026-06-24
通讯作者: ^*电子信箱: ylu@chem.ecnu.edu.cn (路勇).
基金资助:
国家自然科学基金(22572054);国家自然科学基金(22272053);国家自然科学基金(22072043);国家重点研发计划(2023YFA1507903);国家重点研发计划(2023YFB3810602);中石化石油化工科学研究院有限公司部分经费资助

Coking-resistant CeAlO₃-Socketed Nickel Nanocatalysts for dry reforming of methane

Zhongchen Ma^a, Meiyi Yin^a, Run Xu^b, Rongjun Zhang^b, Tian Lan^a, Wenli Gu^a, Guoqing Chen^a, Yong Lu^a^,^c^,^*()

^a State Key Laboratory of Petroleum Molecular & Process Engineering, Shanghai Key Laboratory of Green Chemistry and Chemical Processes, School of Chemistry and Molecular Engineering, East China Normal University, Shanghai 200062, China
^b SINOPEC Research Institute of Petroleum Processing Co., Ltd., Beijing 100083, China
^c Institute of Eco-Chongming (IEC), Shanghai 202151, China

Received:2025-11-19 Accepted:2025-12-22 Online:2026-08-18 Published:2026-06-24
Supported by:
National Natural Science Foundation of China(22572054);National Natural Science Foundation of China(22272053);National Natural Science Foundation of China(22072043);National Key Research and Development Program of China(2023YFA1507903);National Key Research and Development Program of China(2023YFB3810602);support partially provided by the SINOPEC Research Institute of Petroleum Processing Co., Ltd.

摘要/Abstract

摘要：

推进碳基能源化工体系的绿色可持续发展, 是当前国家“双碳”战略实施的必然要求. 从绿色碳科学分子视角看, CH₄和CO₂能源化工利用的开发和应用, 是一项赋能“碳减排”、服务“碳中和”的重要路径. 将CO₂与CH₄通过重整反应(DRM, 甲烷干重整)制成合成气并经下游催化技术转化可同时实现天然气(主要成分为CH₄)和CO₂的化工利用, 是规模化消纳CO₂、助力“碳减排”的极具工业化潜力的关键技术. 作为最具工业应用潜力的镍基催化剂, 其抗积碳、抗烧结性能依然面临严峻挑战, 这极大制约了DRM过程的商业化开发.

基于此, 本研究提出了一种限域结构耦合界面氧化-还原工程的催化剂构筑策略, 旨在为Ni基催化剂的易积碳和易烧结问题提供解决方案. 具体而言, 通过H₂还原诱导Ni颗粒从Ce₁Al_0.95Ni_0.05O_x复合氧化物中析出, 并同步结晶生成CeAlO₃, 可控构建出CeAlO₃镶嵌Ni纳米颗粒的限域耦合特定界面的独特结构. 尤其是, 通过改变还原温度(700‒900 °C)实现了系列Ni颗粒析出程度可控且Ni-CeAlO₃界面量可调的Ce₁Al_0.95Ni_0.05O_x-T催化剂的制备. 对所制得催化剂进行了扫描电镜、透射电镜、分散度、催化活性、失活率及转换频率等分析表征, 结合理论计算, 深入研究了还原温度对界面结构以及催化活性和稳定性的影响. 结果表明, 经750 °C还原制得的催化剂, Ni纳米颗粒(3-4 nm)均匀嵌入到CeAlO₃载体中, 形成了丰富的Ni-CeAlO₃界面结构. 所得Ce₁Al_0.95Ni_0.05O_x-750催化剂在常压、700 °C, 15 L g_cat⁻¹ h⁻¹, CH₄/CO₂ = 1/1(无稀释)的反应条件下, 连续运行500 h无失活且无积碳生成. 研究表明, Ni-CeAlO₃界面活性位相对于Ni颗粒表面位点, 对甲烷的活化能力有所削弱但同时对CO₂的活化能力得到了明显增强. 在此基础上, 借助原位红外漫反射光谱和¹³C同位素标记实验研究, 揭示了Ni-CeAlO₃界面氧化-还原催化循环机理: 在反应气氛中CO₂优先在Ni-CeAlO₃界面位点上活化, 生成CO与活性氧物种(O*); 随后, 界面的O*以CH₃O*中间体的形式参与CH₄的活化并进一步转化生成CO和H₂, 完成界面氧化-还原催化循环. 这种串行反应机制实现了CO₂和CH₄分子的计量转化, 从本质上抑制了传统甲烷裂解机理上由于O*供给以及传递速率不足引起的积碳, 赋予催化剂突出的抗积碳性能.

综上, 本文针对Ni基DRM催化剂易积碳和易烧结的问题, 发展了限域结构耦合界面氧化-还原工程的催化剂构筑策略, 研制出兼具抗积碳和抗烧结性能的Ni基催化剂, 阐明了基于CO₂优先活化提供活性氧物种(O*)接力活化转化CH₄的串行反应新机理. 本研究为设计具有工业应用前景的高效镍基DRM催化剂提供了新思路和可行技术方案.

关键词: 甲烷干重整, 抗积碳, 镍基催化剂, 界面催化, CeAlO₃

Abstract:

Nickel-based catalysts are regarded as the most promising candidates for industrial dry reforming of methane (DRM), yet severe coking and metal sintering impede their commercial viability. Herein, we report a CeAlO₃-socketed Ni nanocatalyst with extensive Ni-CeAlO₃ interfaces, demonstrating coke-free stability with no deactivation over 500 h test at 700 °C for a feed of CH₄/CO₂ = 1/1 (undiluted). The socket-structured catalyst was obtained via H₂-reduction-triggered Ni exsolution and simultaneous formation of CeAlO₃ from a Ce₁Al_0.95Ni_0.05O_x composite oxide. A socketed structure featuring extensive Ni-CeAlO₃ interface was achieved upon reduction at 750 °C, which essentially modulated the catalytic activation kinetics of both CO₂ and CH₄. In-situ diffused reflectance infrared Fourier transformed spectroscopy and isotope-labeling experiments were performed to gain insight into the interfacial catalysis, revealing that CO₂ was preferentially activated at the Ni-CeAlO₃ interface to form CO and O*, and CH₄ was subsequently oxidized by O* to form H₂ and another CO through formation of CH₃O* intermediates. Such tandem reaction pathway led to stoichiometric conversion of CO₂ and CH₄ molecules thereby imparting our catalyst to high coking resistance. Our findings shed light on the rational design of a valid Ni-based DRM catalyst with substantial potential for industrial application.

Key words: Dry reforming of methane, Coking resistance, Nickel catalyst, Interface catalysis, CeAlO₃

马忠臣, 尹美怡, 徐润, 张荣俊, 兰天, 顾文丽, 陈国庆, 路勇. CeAlO₃镶嵌镍纳米颗粒抗积碳甲烷干重整催化剂[J]. 催化学报, 2026, 87: 363-375.

Zhongchen Ma, Meiyi Yin, Run Xu, Rongjun Zhang, Tian Lan, Wenli Gu, Guoqing Chen, Yong Lu. Coking-resistant CeAlO₃-Socketed Nickel Nanocatalysts for dry reforming of methane[J]. Chinese Journal of Catalysis, 2026, 87: 363-375.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65063-2

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图/表 5

Fig. 1. Reduction induced Ni exsolution from Ce1Al0.95Ni0.05Ox composite oxide. (a) XRD patterns and local enlarged patterns of Ce1Al0.95Ni0.05Ox and Ce1Al0.95Ni0.05Ox-T catalysts (T, reduction temperature). (b) Crystallite sizes of CeAlO3 in the Ce1Al0.95Ni0.05Ox-T catalysts, derived from XRD patterns. (c) TEM images of representative Ce1Al0.95Ni0.05Ox-T catalysts. (d) Schematic illustration of the exsolution degree of nickel nanoparticles against reduction temperatures, based on TEM images. (e) SEM images of the Ce1Al0.95Ni0.05Ox-T catalysts.

Fig. 2. Structural characterization of exsolved Ni nanoparticles. (a) XRD patterns and local enlarged patterns of fresh and reduced catalysts. (b) H2 pulse chemisorption-MS profiles of the Ce1Al0.95Ni0.05Ox-750 and Ni/CeAlO3-750 catalysts. (c) TEM image of the Ni/CeAlO3-750 catalyst. (d) AC-STEM image of the Ce1Al0.95Ni0.05Ox-750 catalyst and EDS line mapping images (inset) across the region outlined by red dashed line. (e) Ball-and-stick model of the Ni-CeAlO3 interface. (f) Schematic illustration of the particle-substrate interface for deposited and exsolved Ni nanoparticles.

Fig. 3. Catalytic performance of Ce1Al0.95Ni0.05Ox-T and Ni/CeAlO3-750 catalysts for the DRM reaction and characterization of the used catalysts. (a) CH4 and CO2 conversions during 100-h DRM reaction test. XRD patterns and local enlarged patterns (b), TG profiles (c), and O2-TPO-MS profiles (d) of the used catalysts. (e) 500-h DRM reaction stability test of the Ce1Al0.95Ni0.05Ox-750 catalyst. Reaction conditions: 700 °C, CH4/CO2 = 1/1, GHSV = 15 L gcat−1 h−1, and 1 bar.

Fig. 4. Insights into CH4 and CO2 activations at the Ni-CeAlO3 interface. CH4-TPSR-MS (a), CO2-TPSR-MS (b), and CO2/CH4-TPSR-MS (c) profiles for the Ce1Al0.95Ni0.05Ox-750 and Ni/CeAlO3-750 catalysts.

Fig. 5. Interfacial catalysis for DRM reaction. (a) 13CO2/CH4-TPSR-MS profiles for Ce1Al0.95Ni0.05Ox-750 in a flow of 13CO2/CH4/He (1/1/8) at 30 mL min−1. (b) 13CO2/CH4-constant temperature pulse reaction over Ni/CeAlO3-750 and Ce1Al0.95Ni0.05Ox-750 catalysts at 750 °C, with each pulse of 0.5 mL of 13CO2/CH4/He (1/1/8) carried by He at 20 mL min−1. In-situ DRIFT spectra collected over Ce1Al0.95Ni0.05Ox-750 catalyst under static-state CO2/CH4/He (1/1/8) atmosphere at 700 °C (c,d), and under continuous CO2/He (1/9) flow at 20 mL min−1 first for 15 min at 700 °C followed by He purging for 15 min, and then exposed to continuous flow of CH4/He (1/9) at 20 mL min−1 for another 15 min at 700 °C (e,f).

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CeAlO₃镶嵌镍纳米颗粒抗积碳甲烷干重整催化剂

Coking-resistant CeAlO₃-Socketed Nickel Nanocatalysts for dry reforming of methane

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