耐水性的Pd-Co3O4催化界面用于甲烷完全氧化反应: 活性结构和反应路径研究

doi:10.1016/S1872-2067(25)64728-0

催化学报 ›› 2025, Vol. 74: 191-201.DOI: 10.1016/S1872-2067(25)64728-0

耐水性的Pd-Co₃O₄催化界面用于甲烷完全氧化反应: 活性结构和反应路径研究

许远杰^a, 侯润^a, 池坤翔^a, 刘波^a, 安泽民^a, 吴立志^a, 谭理^a, 宗绪鹏^b, 戴翼虎^c, 谢在来^a, 汤禹^a^,^*()

^a福州大学化学学院, 分子工程+研究院, 分子催化与原位表征研究所, 福建福州 350108
^b中国科学院大连化学物理研究所, 辽宁大连 116023
^c南京工业大学化学与分子工程学院, 江苏南京 211816

收稿日期:2024-12-15 接受日期:2025-04-11 出版日期:2025-07-18 发布日期:2025-07-20
通讯作者: *电子信箱: yu.tang@fzu.edu.cn (汤禹).
基金资助:
国家自然科学基金(22472030);国家自然科学基金(U22A20431);国家自然科学基金(22202047);国家自然科学基金(22172032);福建省自然科学基金(2024J01235);福建省自然科学基金(2022J05110)

A water-resistant and stable Pd-Co₃O₄ catalytic interface for complete methane oxidation with insights on active structures and reaction pathway

Yuanjie Xu^a, Run Hou^a, Kunxiang Chi^a, Bo Liu^a, Zemin An^a, Lizhi Wu^a, Li Tan^a, Xupeng Zong^b, Yihu Dai^c, Zailai Xie^a, Yu Tang^a^,^*()

^aInstitute of Molecular Engineering Plus, Institute of Molecule Catalysis and In-Situ/Operando Studies, College of Chemistry, Fuzhou University, Fuzhou 350108, Fujian, China
^bDalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^cInstitute of Advanced Synthesis, School of Chemistry and Molecular Engineering, Nanjing Tech University, Nanjing 211816, Jiangsu, China

Received:2024-12-15 Accepted:2025-04-11 Online:2025-07-18 Published:2025-07-20
Contact: *E-mail: yu.tang@fzu.edu.cn (Y. Tang).
Supported by:
National Natural Science Foundation of China(22472030);National Natural Science Foundation of China(U22A20431);National Natural Science Foundation of China(22202047);National Natural Science Foundation of China(22172032);Natural Science Foundation of Fujian Province(2024J01235);Natural Science Foundation of Fujian Province(2022J05110)

摘要/Abstract

摘要：

钯基催化剂因在甲烷燃烧反应中展现的高活性, 长期以来一直被视为甲烷燃烧的基准催化剂; 然而, 催化活性位点的真实相态仍是一个持续争论的话题. 此外, 甲烷燃烧过程中, 除了反应过程会产生水蒸气外, 反应气通常含有较高浓度的水蒸气, 这使得催化剂的耐水性成为甲烷燃烧反应催化剂面临的关键问题. 催化剂水中毒和长期稳定性等挑战需要得到解决, 以进一步提升催化剂性能. 尽管过去的数十年间, 针对低温甲烷燃烧已经进行了广泛的研究, 尤其是Pd与金属氧化物材料. 但是, 目前对于金属氧化物载体对Pd在催化过程中的状态影响仍不明确. 揭示金属氧化物对Pd在催化过程中的状态影响, 对催化机理的研究和催化剂的设计具有重要意义.

本文聚焦甲烷完全氧化反应, 制备了Pd/Co₃O₄催化剂, 并以商用Pd/Al₂O₃催化剂为对照, 通过多种原位和非原位表征手段研究催化剂结构、性能及反应机制. 相比于商用Pd/Al₂O₃催化剂, Pd/Co₃O₄催化剂在350 °C甲烷完全氧化条件下连续运行100 h, 活性基本不变, 表现出优异的热稳定性. 同时, 在含水蒸汽的条件下, Pd/Co₃O₄表现出比Pd/Al₂O₃催化剂更优异的耐水性. 拉曼光谱和近常压X射线光电子能谱(NAP-XPS)结果表明, Pd/Co₃O₄具有更多的氧空位, 这有利于氧气的吸附和活化. H₂程序升温还原、O₂程序升温脱附和NAP-XPS结果表明, Pd的引入降低了Co₃O₄晶格氧的还原温度, 增强了界面处晶格氧的反应性和表面氧物种的迁移. Pd和Co₃O₄之间存在协同效应, 这种协同效应可以削弱Co-O键, 促进表面氧物种的迁移. 同时, 研究发现, 氧气更倾向于吸附在Co₃O₄的氧空位上并被活化, 从而参与甲烷完全氧化反应. 原位研究表明, 在催化过程中, Pd物种会发生快速相变, 这种快速相变有利于OH^-的脱附, 抑制Pd(OH)₂的形成. 稳态变温NAP-XPS实验发现, 催化剂在反应条件下通常保持在金属态, 这得益于Pd与Co₃O₄之间的电子金属载体相互作用. 该相互作用促进了Pd-O_v-Co催化界面的形成, 加速了氧分子和电子转移, 抑制了Pd(OH)₂的形成, 从而使催化剂具有优异的耐水性. 此外, 原位漫反射FTIR谱揭示了反应过程中, HCO₃^-倾向于转化为甲酸盐物种, 意味着催化剂对甲烷完全氧化反应的路径倾向于甲酸盐路径. 这项工作拓展了对Pd负载Co₃O₄催化剂的甲烷完全氧化界面协同效应的认识.

综上所述, 本文制备的Pd/Co₃O₄催化剂对甲烷完全氧化反应具有优异的热稳定性和耐水性. 结合原位和非原位表征技术, 阐明了催化剂活性位点结构和反应机制. 为工业上甲烷完全氧化催化剂的设计和制备提供了新思路.

关键词: 甲烷燃烧, 完全氧化, 钯基催化剂, 耐水性, 四氧化三钴, 氧气活化, 近常压-X射线光电子能谱

Abstract:

Palladium-based catalysts have long been considered the benchmark for methane combustion; however, the authentic phase of catalytic active sites remains a subject of ongoing debate. Additionally, challenges like water-poisoning and long-term stability need to be addressed to advance catalyst performance. Herein, we investigate Pd on Co₃O₄ nanorods as a highly effective catalyst for catalytic oxidation of methane, demonstrating long-term stability and water tolerance during a 100-h continuous operation at 350 °C. Comprehensive characterizations reveal the presence of an active Pd-oxygen vacancy (O_v)-cobalt interface in Pd/Co₃O₄, which effectively adsorbs molecular O₂. The absorbed oxygen species on this interface are activated and directly participate in methane combustion. Moreover, near-ambient pressure X-ray photoelectron spectroscopy demonstrates that Pd nanoparticles undergo a rapid phase transition and predominantly remain in the metallic state during the reaction. This behavior is attributed to the electronic metal-support interaction between Pd and Co₃O₄. Furthermore, in situ Fourier transformed infrared spectrum reveals that under reaction conditions, HCO₃* species are formed initially and subsequently transformed into formate species, indicating that the formate pathway is the dominant mechanism for CH₄ oxidation.

Key words: Methane combustion, Complete oxidation, Palladium catalyst, Water tolerance, Co₃O₄, Oxygen activation, Near-ambient pressure X-ray photoelectron spectroscopy

许远杰, 侯润, 池坤翔, 刘波, 安泽民, 吴立志, 谭理, 宗绪鹏, 戴翼虎, 谢在来, 汤禹. 耐水性的Pd-Co₃O₄催化界面用于甲烷完全氧化反应: 活性结构和反应路径研究[J]. 催化学报, 2025, 74: 191-201.

Yuanjie Xu, Run Hou, Kunxiang Chi, Bo Liu, Zemin An, Lizhi Wu, Li Tan, Xupeng Zong, Yihu Dai, Zailai Xie, Yu Tang. A water-resistant and stable Pd-Co₃O₄ catalytic interface for complete methane oxidation with insights on active structures and reaction pathway[J]. Chinese Journal of Catalysis, 2025, 74: 191-201.

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图/表 8

Fig. 1. Catalytic performance of the catalysts. (a) Temperature dependence of CH4 conversion over Co3O4, Pd/Co3O4, and Pd/Al2O3 for COM reaction. (b) Arrhenius plots of Co3O4, Pd/Co3O4, and Pd/Al2O3 for COM reaction. (c) Catalytic performance of Co3O4, Pd/Co3O4, and Pd/Al2O3 for COM reaction at 350 °C against time on stream. Conditions: 50 mg catalysts, a mixture of 20 mL/min 10 vol% CH4/Ar and 10 mL/min pure O2. (d) Long-term performance of Pd/Co3O4 and Pd/Al2O3 for complete oxidation of methane under wet feed conditions at 350 °C. The feed contains 2000 ppm CH4, 1%O2, and 3% H2O balanced with Ar (50 mL/min).

Fig. 2. XRD patterns of fresh catalyst of Co3O4 spent Co3O4 catalyst after complete oxidation of methane, fresh catalyst of Pd/Co3O4, and spent Pd/Co3O4 catalyst after complete oxidation of methane. Scan rate of 1°/min with 0.01 step in the 2θ range from 20° to 70°.

Fig. 3. STEM images of Pd/Co3O4 after catalytic combustion of methane.

Fig. 4. (a) DRIFTS-CO spectra of Co3O4, fresh catalyst of Pd/Co3O4, and spent Pd/Co3O4 catalyst after complete oxidation of methane. Conditions: all the samples were pretreated at 200 °C under Ar for 1h, and tested CO adsorption at room temperature. (b) Raman spectra of fresh catalyst of Co3O4, spent Co3O4 catalyst after complete oxidation of methane, fresh catalyst of Pd/Co3O4, and spent Pd/Co3O4 catalyst after complete oxidation of methane.

Fig. 5. Redox properties of Co3O4 and Pd/Co3O4 catalysts. (a) H2-TPR profile; (b) CH4-TPR profile; (c) O2-TPD profile.

Table 1 The H2 consumption of the as-prepared catalysts.

Samples	Peak 1 (mmol/g)	Peak 2 (mmol/g)
Co₃O₄	3.16	11.51
Pd/Co₃O₄	2.39	4.49

Fig. 6. NAP-XPS studies of Pd/Co3O4 under COM reactions. (a) Photoemission feature of Co 2p and Pd 3d of Pd/Co3O4 under various gas-phase conditions at 250 °C. Data were collected across four sequential stages by altering the gas composition. (I) 1 Torr O2; (II) 0.2 Torr CH4; (III) 1 Torr O2; (IV) 0.2 Torr CH4. (b) Pd chemical states deconvoluted from NAP-XPS experiment. (c) NAP-XPS studies of Pd/Co3O4 catalyst for the steady state spectra of Pd 3d under the COM reactant gases at different temperatures.

Fig. 7. (a) In situ DRIFTS studies of Pd/Co3O4 under steady state complete oxidation of methane at 200 °C as the function of time. (b) Schematic diagram of complete oxidation of methane on Pd/Co3O4 catalyst.

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耐水性的Pd-Co₃O₄催化界面用于甲烷完全氧化反应: 活性结构和反应路径研究

A water-resistant and stable Pd-Co₃O₄ catalytic interface for complete methane oxidation with insights on active structures and reaction pathway

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