配体保护的精确结构镍纳米团簇高效电催化甘油氧化制甲酸

doi:10.1016/S1872-2067(25)64779-6

催化学报 ›› 2025, Vol. 76: 185-197.DOI: 10.1016/S1872-2067(25)64779-6

配体保护的精确结构镍纳米团簇高效电催化甘油氧化制甲酸

杨丹^a^,¹^,^*(), 崔翔^a^,¹, 徐周^a^,¹, 颜前^a, 吴雅婷^a, 周春梅^a, 戴翼虎^a, 万晓月^a, 靳玉广^b, 杨艳辉^a^,^*()

^a南京工业大学化学与分子工程学院, 先进化学制造研究院, 江苏南京 211816, 中国
^b鄂尔多斯实验室, 内蒙古鄂尔多斯 017010, 中国
^cN. D. Zelinsky有机化学研究所, 莫斯科, 俄罗斯
^d莫斯科国立大学化学系, 莫斯科, 俄罗斯

收稿日期:2025-04-09 接受日期:2025-07-04 出版日期:2025-09-18 发布日期:2025-09-10
通讯作者: 杨丹,杨艳辉
作者简介:第一联系人：
¹共同第一作者.
基金资助:
江苏省自然科学基金(BK20230329);国家自然科学基金(22401147);国家自然科学基金(22361132540);国家自然科学基金(22178161);俄罗斯科学基金(23-73-30007)

Efficient electrocatalytic oxidation of glycerol toward formic acid over well-defined nickel nanoclusters capped by ligands

Dan Yang^a^,¹^,^*(), Xiang Cui^a^,¹, Zhou Xu^a^,¹, Qian Yan^a, Yating Wu^a, Chunmei Zhou^a, Yihu Dai^a, Xiaoyue Wan^a, Yuguang Jin^b, Leonid M. Kustov^c^,^d, Yanhui Yang^a^,^*()

^aInstitute of Advanced Synthesis, School of Chemistry and Molecular Engineering, Nanjing Tech University, Nanjing 211816, Jiangsu, China
^bOrdos Laboratory, Ordos 017010, Inner Mongolia, China
^cN. D. Zelinsky Institute of Organic Chemistry RAS, 47 Leninsky prosp., Moscow 119991, Russia
^dChemistry Department, Moscow State University, 1 Leninskie Gory, bldg. 3, Moscow 119992, Russia

Received:2025-04-09 Accepted:2025-07-04 Online:2025-09-18 Published:2025-09-10
Contact: Dan Yang, Yanhui Yang
About author:First author contact:
¹ Contributed equally to this work.
Supported by:
the Jiangsu Natural Science Foundation of China(BK20230329);the National Natural Science Foundation of China(22401147);the National Natural Science Foundation of China(22361132540);the National Natural Science Foundation of China(22178161);the Russian Science Foundation(23-73-30007)

摘要/Abstract

摘要：

甘油电催化氧化制甲酸是甘油转化利用最有前景的途径之一. 作为化石燃料的替代品, 生物柴油是一种清洁且可再生的能源. 然而, 其生产过程中大量副产的粗甘油制约了行业的发展. 将甘油转化为高附加值化学品对于推动生物柴油行业的可持续发展至关重要. 由可再生电力驱动的甘油选择性电催化氧化转化受到了研究者广泛关注, 其中氧化产物甲酸因其低毒性和高能量密度, 被认为是极具潜力的氢载体. 因此开发高效电催化剂实现甘油选择性氧化制甲酸意义重大.

与传统镍基催化剂相比, 配体保护的镍纳米团簇不仅具有结构明确的活性位点, 而且可以通过系统调节镍纳米团簇表面的配体覆盖度和电子结构, 实现对其催化性能的有效调控. 基于此, 本文可控合成了一系列结构明确的Ni_n(PET)₂_n纳米团簇(n = 4, 5, 6; SR = 苯乙硫醇, 正丁硫醇, 正己硫醇), 用于电催化甘油氧化制甲酸. 结果表明, 对镍纳米团簇表面进行一定的电化学预处理会有效提升其电催化活性, 其中Ni₆-PET-50CV电催化性能最佳: 甲酸选择性达到93%、甘油转化率达到86%, 显著优于传统NiO和Ni(OH)₂纳米颗粒催化剂. 这主要归因于其具有较低的电荷转移阻抗和较快的反应动力学. 结合原位红外、拉曼、紫外-可见光谱和X射线吸收精细结构测量, 重点研究了镍纳米团簇催化剂在电化学预处理和反应过程中结构的演变. 结果表明, 经过电化学预处理和电催化反应后, 镍纳米团簇没有团聚形成镍纳米颗粒以及NiOOH, 镍纳米团簇结构通过形成部分Ni-O键得以保持完整. 此外, 电化学动力学研究和原位红外光谱表明, 镍纳米团簇电催化甘油氧化的反应机制为连续氧化机制, 其中主要的反应步骤甘油→甘油醛→甘油酸的转化快速进行, 即使在低转化率下仍能高选择性生成甲酸.

综上, 配体保护的镍纳米团簇可高效将甘油电催化氧化为甲酸, 为研究镍纳米团簇在生物质衍生多羟基平台分子转化为高附加值羧酸中的应用提供了实践应用和理论参考.

关键词: 镍纳米团簇, 精确结构, 电催化, 甘油氧化, 甲酸

Abstract:

The electrocatalytic oxidation of glycerol toward formic acid is one of the most promising pathways for transformation and utilization of glycerol. Herein, a series of well-defined Ni_n(SR)₂_n nanoclusters (n = 4, 5, 6; denoted as Ni NCs) were prepared for the electrocatalytic glycerol oxidation toward formic acid, in which Ni₆-PET-50CV afforded the most excellent electrocatalytic performance with a high formic acid selectivity of 93% and a high glycerol conversion of 86%. This was attributed to the lowest charge transfer impedance and the most rapid reaction kinetics. Combined electrochemical measurements and X-ray absorption fine structure measurements revealed that the structures of Ni NCs remained intact after CV scanning pretreatment and electrocatalysis via forming the Ni-O bond. Additionally, the kinetic studies and in-situ Fourier transformed infrared suggested a sequential oxidation mechanism, in which the main reaction steps of glycerol → glyceraldehyde → glyceric acid were very rapid to produce a high selectivity of formic acid even though the low glycerol conversion. This work presents an opportunity to study Ni NCs for the efficient electrocatalytic oxidation of biomass-derived polyhydroxyl platform molecules to produce value-added carboxylic acids.

Key words: Nickel nanocluster, Well-defined structure, Electrocatalysis, Glycerol oxidation, Formic acid

杨丹, 崔翔, 徐周, 颜前, 吴雅婷, 周春梅, 戴翼虎, 万晓月, 靳玉广, 杨艳辉. 配体保护的精确结构镍纳米团簇高效电催化甘油氧化制甲酸[J]. 催化学报, 2025, 76: 185-197.

Dan Yang, Xiang Cui, Zhou Xu, Qian Yan, Yating Wu, Chunmei Zhou, Yihu Dai, Xiaoyue Wan, Yuguang Jin, Leonid M. Kustov, Yanhui Yang. Efficient electrocatalytic oxidation of glycerol toward formic acid over well-defined nickel nanoclusters capped by ligands[J]. Chinese Journal of Catalysis, 2025, 76: 185-197.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64779-6

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图/表 9

Fig. 1. (a) Crystal structures of Ni4, Ni5, and Ni6, all hydrogen atoms are omitted for clarity. (b) MALDI mass spectra of Ni NCs. (c) UV-vis spectra of Ni NCs. Ni K-edge XANES spectra (d) and FT-EXAFS spectra (e) for Ni6-PET NCs after 0, 20, 50 CV pretreatment at 0.7-2.3 V vs. RHE in 0.1 mol L-1 KOH. Ni foil and NiO are showed for comparison. Color labels: green = Ni; yellow = S; grey = C.

Fig. 2. Electrocatalytic performance of GLY oxidation over the Nix NCs. (a) The LSV curves of Ni6-PET NCs pretreated by different scanning segments in 0.1 mol L-1 KOH with 0.01 mol L-1 GLY. (b) Catalytic performance of different Ni6-PET NCs at 1.40 V vs. RHE. (c) LSV curves of Ni4-PET, Ni5-PETand Ni6-PET NCs pretreated by scanning 50 segments CV curves in 0.1 mol L-1 KOH solution with and without 0.01 mol L-1 GLY. (d) Catalytic performance of pretreated Nix-50CV NCs under different applied potentials, others mainly included small amounts of GLYC, LA and GLYO.

Fig. 3. (a) Schematic diagram of Ni6 structure with different organic ligands. (b) UV-vis spectra of Ni6-PET, Ni6-C4, and Ni6-C8 NCs. (c) LSV curves of Ni6-PET, Ni6-C4, and Ni6-C8 NCs pretreated by scanning 50 segments CV curves in 0.1 mol L-1 KOH solution with and without 0.01 mol L-1 GLY. (d) Catalytic performance of pretreated Nix-50CV NCs at 1.50 V vs. RHE, 40 °C for 8 h, others mainly included small amounts of GLYC, LA and GLYO.

Fig. 4. (a,c) Capacitive current densities of Nix-PET-nCV NCs in GLY oxidation as a function of scan rate. (b,d) ECSA normalized LSV curves of Nix-PET-nCV NCs.

Fig. 5. Structural evolutions of the Ni6-PET NCs pretreated by different CV scanning segments. (a) In-situ ATR-IR spectra of ligand changes; (b) UV-vis spectra; (c) Ni 2p; (d) S 2p XPS spectra.

Fig. 6. In-situ XANES spectra (a) and EXAFS spectra (b) for the Ni6-PET NCs after 50CV, 150CV and 350CV pretreatment. Time-resolved in-situ XANES spectra (c) and EXAFS spectra (d) for the Ni6-PET-50CV catalyzing GLY oxidation.

Fig. 7. Nyquist plots of Ni6-PET pretreated by different CV scanning segments (a), Ni4, Ni5, and Ni6 NCs pretreated by 50 scanning segments (b), different ligand capped Ni6 NCs pretreated by 50 scanning segments at an applied bias voltage (c). (d) Nyquist plots of Ni6-PET-50CV NCs at the applied potentials.

Fig. 8. In-situ ATR FT-IR spectra of Ni6-PET-0CV (a), Ni6-PET-20CV (b), Ni6-PET-50CV (c), and Ni6-PET-100CV (d) catalyzing the GLY electrooxidation

Fig. 9. The Tafel plots for GLY oxidation of Ni6-PET-nCV (a) and Ni NCs (b) with different sizes and ligands. (c) Kinetic profiles of Ni4-PET, Ni5-PET and Ni6-PET catalysts in GLY oxidation. Selectivity-conversion correlation of GLY oxidation over (d) Ni4-PET, (e) Ni4-PET, and (f) Ni6-PET catalysts. Reaction condition: 1.45 V vs. RHE, 25 °C, Ni NCs catalysts were pretreated by the 50 CV scanning.

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配体保护的精确结构镍纳米团簇高效电催化甘油氧化制甲酸

Efficient electrocatalytic oxidation of glycerol toward formic acid over well-defined nickel nanoclusters capped by ligands

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