C-C键断裂抑制和中间体吸附增强共同促进乙二醇在银钯空心纳米立方体上的选择性电氧化

doi:10.1016/S1872-2067(26)65015-2

催化学报 ›› 2026, Vol. 86: 191-200.DOI: 10.1016/S1872-2067(26)65015-2

C-C键断裂抑制和中间体吸附增强共同促进乙二醇在银钯空心纳米立方体上的选择性电氧化

王子行^a, 仲伟^a, 李思齐^a, 孙斌^a, 蓝浩^a, 张晓雨^b^,^*(), 王新^b, 陈煜^a^,^*(), 艾轩^a^,^*()

^a 陕西师范大学材料科学与工程学院, 陕西省大分子科学重点实验室, 陕西西安 710062
^b 浙江万里学院碳中和研究所, 浙江宁波 315100

收稿日期:2025-10-13 接受日期:2025-11-28 出版日期:2026-07-05 发布日期:2026-06-12
通讯作者: ^*电子信箱: zxy@zwu.edu.cn (张晓雨),
ndchenyu@gmail.com (陈煜),
aixuan@snnu.edu.cn (艾轩).
基金资助:
国家自然科学基金青年项目(22309108);中国博士后科学基金(2023TQ0204);中国博士后科学基金(2025M770003);陕西省博士后科学基金(2024BSHSDZZ066);西安市科协青年人才基金(0959202513011);宁波市甬江人才引进计划(2024A-165-G);宁波市自然科学基金(2024J442);国家级大学生创新创业训练计划(S202510718212)

The C-C bond cleavage inhibition and intermediates adsorption enhancement co-boost the selective electrooxidation of ethylene glycol on silver-palladium hollow nanocubes

Zi-Hang Wang^a, Wei Zhong^a, Si-Qi Li^a, Bin Sun^a, Hao Lan^a, Xiao-Yu Zhang^b^,^*(), Xin Wang^b, Yu Chen^a^,^*(), Xuan Ai^a^,^*()

^a Key Laboratory of Macromolecular Science of Shaanxi Province, School of Materials Science and Engineering, Shaanxi Normal University, Xi’an 710062, Shaanxi, China
^b Institute of Carbon Neutrality, Zhejiang Wanli University, Ningbo 315100, Zhejiang, China

Received:2025-10-13 Accepted:2025-11-28 Online:2026-07-05 Published:2026-06-12
Supported by:
National Natural Science Foundation of China for the Youth(22309108);China Postdoctoral Science Foundation(2023TQ0204);China Postdoctoral Science Foundation(2025M770003);Shaanxi Province Postdoctoral Science Foundation(2024BSHSDZZ066);Young Talent Fund of Xi'an Association for Science and Technology(0959202513011);Ningbo Yongjiang Talent Introduction Program(2024A-165-G);Ningbo Natural Science Foundation(2024J442);National Training Program of Innovation and Entrepreneurship for Undergraduates(S202510718212)

摘要/Abstract

摘要：

乙二醇(EG)是一种来源广泛且价格低廉的平台分子, 可由木质纤维素生物质转化或废旧聚对苯二甲酸乙二醇酯塑料化学回收获得. 将EG选择性电氧化为具有高附加值的乙醇酸(GA), 是一条有望实现生物质资源与塑料固废的协同高值利用的路径. 此过程可与电解水产氢或二氧化碳电还原等过程耦合, 构建兼具能源输出和污染减排功能的电化学体系. 然而, EG电催化氧化过程中普遍存在C-C键易断裂、副产物复杂、目标产物选择性偏低以及贵金属催化剂利用效率不高等问题, 难以满足绿色高效电化学增值转化的需求.

针对上述问题, 本文提出通过合金界面电子结构调控和中空结构工程策略协同抑制C-C键断裂, 并强化中间体吸附的设计思路, 构筑银钯空心纳米立方体(AgPd hNCs)电催化剂. 以Ag纳米立方体为结构模板, 通过溶剂热辅助原位电化学置换实现Ag向Pd的部分取代和刻蚀, 获得内部中空、表面富含低配位活性位点的AgPd hNCs. 结构表征表明, Ag与Pd形成面心立方结构的均匀合金, 催化剂壳层由纳米颗粒自组装构成, 表面富集低配位活性位点, 且具有高电化学比表面积. X射线光电子能谱和X射线吸收精细结构谱结果揭示, AgPd合金引发电子重分布与几何畸变, 协同优化了Pd的d带中心. 在碱性EG电解液中, AgPd hNCs相较商用Pd黑表现出更负的EG电氧化起始电位和峰电位, 在0.90 V vs. RHE时实现96%的EG转化率、95.1%的GA选择性和93%的法拉第效率, 其质量活性约为Pd黑的2.8倍. 恒电位计时电流测试表明, AgPd hNCs具有良好的催化稳定性与抗毒化能力. 稳定性测试后的物理表征结果显示, 催化剂形貌与合金结构基本保持不变. 原位电化学光谱测试以及液相产物测试证实, GA为主要液相产物, C2路径占主导, 且C-C键断裂和CO₂生成受到有效抑制. 密度泛函理论计算表明, 与Pd(111)相比, AgPd(001)表面对EG及CH₂OH-CHO*等中间体具有更强吸附能力, 降低决速步能垒, 实现对C-C键断裂的抑制.

综上, 本文构筑具有中空结构和可调电子结构的AgPd hNCs实现了EG向GA的高选择性电氧化, 揭示了合金界面抑制C-C键断裂并调控中间体吸附的构效关系, 为高性能贵金属电催化剂设计和生物质衍生多元醇电化学增值转化提供了有益借鉴.

关键词: 乙二醇氧化反应, 空心纳米立方体, 电子结构, 银钯合金, 选择性

Abstract:

Efficient electrooxidation of ethylene glycol (EG) to glycolic acid (GA) is highly desirable for biomass valorization and EG recycling, which remains challenging owing to side reactions involving C-C bond cleavage. Herein, the bimetallic AgPd hollow nanocubes (AgPd hNCs) are successfully prepared via a solvothermal-assisted Galvanic replacement strategy. Both theoretical calculations and experimental results indicate that the electronic interplay between the Pd atom and Ag atom hinders C-C bond breaking and enhances the adsorption of critical intermediates, resulting in high selectivity toward GA production. Benefiting from these features, AgPd hNCs achieve a Faradaic efficiency of 93% toward GA formation and a 2.8-fold increase in mass activity compared to Pd black. Moreover, the strong oxygen affinity of Ag promotes the removal of CO-like intermediates from the Pd surface, resulting in superior EG oxidation stability. This study highlights a generalizable Ag-based strategy to modulate bimetallic interfaces for selective oxidation reaction of specific functional groups, contributing to the rational design of electrocatalysts for biomass upgrading.

Key words: Ethylene glycol oxidation reaction, Hollow nanocubes, Electronic structure, Ag-Pd alloy, Selectivity

王子行, 仲伟, 李思齐, 孙斌, 蓝浩, 张晓雨, 王新, 陈煜, 艾轩. C-C键断裂抑制和中间体吸附增强共同促进乙二醇在银钯空心纳米立方体上的选择性电氧化[J]. 催化学报, 2026, 86: 191-200.

Zi-Hang Wang, Wei Zhong, Si-Qi Li, Bin Sun, Hao Lan, Xiao-Yu Zhang, Xin Wang, Yu Chen, Xuan Ai. The C-C bond cleavage inhibition and intermediates adsorption enhancement co-boost the selective electrooxidation of ethylene glycol on silver-palladium hollow nanocubes[J]. Chinese Journal of Catalysis, 2026, 86: 191-200.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65015-2

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图/表 5

Fig. 1. TEM image (a), element mapping (b), EDX linear scanning at the shell region (c), HAADF-STEM image (d), and magnified HAADF-STEM image (e) of AgPd hNCs.

Fig. 2. XRD pattern (a), Ag 3d XPS spectrum (b), and Pd 3d XPS spectrum (c) of AgPd hNCs. (d) Normalized Pd K-edge XANES for Pd foil, AgPd hNCs and PdO. (e) FT-EXAFS spectrum of AgPd hNCs, Pd foil and PdO. WT-EXAFS spectra of Pd in Pd foil (f), AgPd hNCs (g), and PdO (h).

Fig. 3. (a) CV curves of AgPd hNCs, Ag NCs and Pd black in N2-saturated 1.0 mol L−1 KOH solution at 0.05 V s−1. (b) CV curves of AgPd hNCs and Pd black in N2-saturated 1.0 mol L−1 EG + 1.0 mol L−1 KOH solutions at 0.05 V s−1. (c) A partial enlargement of Fig. 3(b). (d) CV curves of samples with different Ag/Pd ratios in N2-saturated 1.0 mol L−1 EG + 1.0 mol L−1 KOH solutions at 0.05 V s−1. (e) Nyquist plots of AgPd hNCs and Pd black. (f) CO stripping curves of AgPd hNCs and Pd black at 0.05 V s−1. (g) Chronoamperometric curves of AgPd hNCs and Pd black in N2-saturated 1.0 mol L−1 EG + 1.0 mol L−1 KOH solutions at 0.94 V vs. RHE.

Fig. 4. (a) 1H NMR analysis of the electrolytes after EGOR on AgPd hNCs. (b) Faradaic efficiency of AgPd hNCs and Pd black at different potentials. (c) In-situ Raman spectra of EGOR at AgPd hNCs with potential changes. (d) In-situ FTIR spectra of EGOR at AgPd hNCs with potential changes.

Fig. 5. (a) Schematic diagram of the reaction process. (b) Gibbs free energy diagrams of EGOR on the Ag(001), Pd(111), and AgPd(001). (c) Density of states of Pd(111) and AgPd(001). (d) Charge density difference of AgPd(001) and Pd(111) induced by the adsorption of *CH2OH-CHO. Deep pink, green, brown, red, and light pink spheres represent Pd, Ag, C, O, and H atoms, respectively.

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C-C键断裂抑制和中间体吸附增强共同促进乙二醇在银钯空心纳米立方体上的选择性电氧化

The C-C bond cleavage inhibition and intermediates adsorption enhancement co-boost the selective electrooxidation of ethylene glycol on silver-palladium hollow nanocubes

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