水系电催化氨氧化反应中MOFs活性位点的原位演变

doi:10.1016/S1872-2067(26)65042-5

催化学报 ›› 2026, Vol. 86: 171-180.DOI: 10.1016/S1872-2067(26)65042-5

水系电催化氨氧化反应中MOFs活性位点的原位演变

王超^a^,^b^,¹, 冯坤^c^,¹, 唐梁书语^a^,¹, 章伍军^d, 周沐宇^a, 李佳璐^a, 邵天雨^a, 沈炎宾^d^,^*(), 钟俊^c^,^*(), 苏韧^a^,^*()

^a 苏州大学能源与材料创新研究院(SIEMIS), 江苏苏州 215006, 中国
^b 河南科技大学化学化工学院, 河南洛阳 471023, 中国
^c 苏州大学功能纳米与软物质研究院(FUNSOM), 江苏省先进负碳技术重点实验室, 江苏苏州 215123, 中国
^d 中国科学院苏州纳米技术与纳米仿生研究所, 江苏苏州 215123, 中国
^e 奥胡斯大学跨学科纳米科学中心, 奥胡斯, 丹麦

收稿日期:2025-09-30 接受日期:2026-01-14 出版日期:2026-07-05 发布日期:2026-06-12
通讯作者: ^*电子信箱: suren@suda.edu.cn (苏韧),
作者简介:第一联系人：¹共同第一作者.
基金资助:
国家自然科学基金(22472112);国家重点研发计划(2020YFA0406103);苏州外籍院士工作站(SWY2022001)

In-situ developed active sites of MOFs in aqueous electrocatalytic ammoxidation

Chao Wang^a^,^b^,¹, Kun Feng^c^,¹, Liangshuyu Tang^a^,¹, Wujun Zhang^d, Muyu Zhou^a, Jialu Li^a, Tianyu Shao^a, Flemming Besenbacher^e, Yanbin Shen^d^,^*(), Jun Zhong^c^,^*(), Ren Su^a^,^*()

^a Soochow Institute for Energy and Materials InnovationS (SIEMIS), Soochow University, Suzhou 215006, Jiangsu, China
^b School of Chemistry and Chemical Engineering, Henan University of Science and Technology, Luoyang 471023, Henan, China
^c Institute of Functional Nano and Soft Materials Laboratory (FUNSOM), Jiangsu Key Laboratory of Advanced Negative Carbon Technologies, Soochow University, Suzhou 215123, Jiangsu, China
^d Suzhou Institute of Nano-Tech and Nano-Bionics (SINANO), Chinese Academy of Sciences, Suzhou 215123, Jiangsu, China
^e Interdisciplinary Nanoscience Center, Aarhus University, Gustav Wieds Vej 14, Aarhus, DK-8000, Denmark

Received:2025-09-30 Accepted:2026-01-14 Online:2026-07-05 Published:2026-06-12
About author:First author contact:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(22472112);National Key R&D Program of China(2020YFA0406103);Suzhou Foreign Academician Workstation(SWY2022001)

摘要/Abstract

摘要：

金属有机框架(MOFs)及其衍生物因具有高比表面积、可调孔道和丰富活性位点而广泛用于电催化反应, 如析氧、二氧化碳还原和氮还原等. 特别地, MOFs中金属节点与有机配体之间的构效关系, 可精准调控电催化剂与底物间的界面电荷转移, 使其在高附加值化学品的电合成中展现出巨大潜力. 然而, 在实际电合成环境中, 复杂的反应条件常引发MOFs结构重构甚至分解, 导致性能衰退. 传统催化剂保护策略(如包覆、掺杂或构建异质结构)虽然能够维持MOFs结构完整, 但过程繁琐, 可能覆盖活性位点, 影响反应中间体的接触, 从而降低催化效率与选择性. 近年来研究发现, MOFs在电化学过程中的动态重构可能形成优于原始结构的活性相, 显著提升反应动力学速率. 因此, 原位追踪MOFs在实际反应条件下的结构演化路径、识别真实活性中心, 对发展高效电催化合成技术具有关键意义.

本文以Co-MOF为模型催化剂, 系统研究了电化学诱导催化剂重构机制及其在氨氧化反应中的活性位点演化机制. 首先, Co-MOF在碱性介质中通过电氧化重构转化为e-Co电催化剂. X-射线衍射、高分辨透射电镜、拉曼和X-射线光电子能谱等结果表明, Co-MOF在电化学处理过程中经历了钴金属-对苯二甲酸配体位点水解断裂, 有序框架结构不可逆坍塌, 形成高价态Co³⁺金属中心的过程, 最终生成具有晶态Co(OH)₂与非晶态CoO_x复合组分的e-Co电催化剂. 进一步地, 利用原位谱学技术分析了实际电化学条件下钴催化剂活性位点的形成过程和氨氧化反应路径. 原位X-射线吸收精细结构和原位拉曼光谱结果表明, 电氧化重构中生成的高价态钴物种作为关键活性位点参与氨氧化过程, 能够驱动氨分子活化氧化, 形成高活性Co-NH_3-_x物种; 高活性氨物种(NH_3-_x)与催化剂表面吸附的苯甲醛生成亚胺中间体; 高价态钴物种进一步促进亚胺中间体氧化脱氢, 实现苯甲腈产物的快速生成, 并从催化剂表面脱附. 同时, 钴活性位点被还原, 进入下一个催化循环. 在常温常压的水系电催化氨氧化体系中, e-Co展现出优异的苯甲腈合成性能, 在较低的槽电压(1.0 V)下, 苯甲腈产率达83%, 法拉第效率为72%, 并具备良好的循环稳定性. 该体系适用于多种官能团修饰的芳香醛和杂环醛, 还能够实现脂肪族腈类化合物的温和合成, 突破了传统合成路径对底物结构与反应条件的限制. 此外, 苯甲腈的高浓度合成和典型香料类腈类化合物的克级制备进一步验证了反应体系的放大应用潜力.

综上, 本工作利用原位表征技术揭示Co-MOF在电化学原位重构中的组分演变规律, 分析电催化氨氧化过程中金属活性位点的催化机制. 这为电催化氨氧化反应机理研究提供了重要实验依据, 也为可持续的腈合成提供了一种绿色高效的替代方案.

关键词: 异相电催化, 金属有机框架, 活性位点演变, 电化学合成, 电化学氨氧化, 钴电催化剂

Abstract:

Metal organic frameworks (MOFs) are frequently employed as electrocatalysts for chemical and energy conversions, owing to their tailored structure and electronic properties. However, the stability and evolution of MOFs under electrochemical conditions remain unclear, resulting in the identification of true active sites a challenging task, thus limiting the design of high-performance electrocatalysts. Here, we follow the development of a representative Co-MOF anode in electrolyte under bias by in-situ spectroscopies, and resolve the evolution of active species for efficient electrocatalytic ammoxidation of aldehydes. A rapid dissociation of Co-MOF occurs in KOH, forming a composite electrocatalyst (e-Co) that consists of crystalline cobalt hydroxide (Co(OH)₂) and amorphous cobalt oxide (CoO_x). The active Co²⁺ sites promote the dissociative adsorption of ammonia, forming Co³⁺-NH_3-_x sites to interact with aldehyde, yielding an imine intermediate and eventually generating nitrile via dehydrogenation. The evolved e-Co electrocatalyst exhibits a satisfactory yield (83%) and Faradaic efficiency (72%) for the synthesis of nitrile at an ultra-low cell voltage of 1.0 V in aqueous electrolyte under ambient air pressure. The e-Co electrocatalyst also displays a decent stability, a broad substrate scope, and a consistent catalytic performance at higher reactant concentrations, offering a sustainable solution for ammoxidation at a practical scale.

Key words: Heterogeneous electrocatalysis, Metal organic frameworks, Active sites evolution, Electrochemical synthesis, Electrochemical ammoxidation, Cobalt electrocatalyst

王超, 冯坤, 唐梁书语, 章伍军, 周沐宇, 李佳璐, 邵天雨, 沈炎宾, 钟俊, 苏韧. 水系电催化氨氧化反应中MOFs活性位点的原位演变[J]. 催化学报, 2026, 86: 171-180.

Chao Wang, Kun Feng, Liangshuyu Tang, Wujun Zhang, Muyu Zhou, Jialu Li, Tianyu Shao, Flemming Besenbacher, Yanbin Shen, Jun Zhong, Ren Su. In-situ developed active sites of MOFs in aqueous electrocatalytic ammoxidation[J]. Chinese Journal of Catalysis, 2026, 86: 171-180.

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Fig. 1. The fresh and transformed electrocatalysts. HRTEM (a,b), Raman (c), and XPS (d) spectra of the as-synthesized Co-MOF and e-Co. The e-Co is produced from treating Co-MOF in 0.1 mol·L−1 KOH for 30 min at 1.2 V. XANES (e) and EXAFS (f) spectra at Co K-edge for Co-MOF, e-Co, and standard materials.

Fig. 2. Evolution of the electrocatalyst. (a) The activation process of the Co-MOF and the appearance of the Co catalyst during electrochemical ammoxidation of benzaldehyde. In-situ Co K-edge XANES (b), EXAFS (c) and Raman (d) spectra in 0.1 mol·L−1 KOH upon dosing ammonia (2.6 mol·L−1) and benzaldehyde (10 mmol·L−1) under bias (1.4 V vs. RHE). The time interval is 3 min for Raman.

Fig. 3. Electrocatalytic ammoxidation. (a) Catalytic performance in comparison with other electrodes. (b) Time-course of ammoxidation using the developed e-Co under a cell voltage of 1.2 V. (c) Effect of NH3·H2O concentration on the ammoxidation. (d) Stability of e-Co for the synthesis of benzonitrile under optimum conditions. (e) Five-dimensional evaluation of the e-Co system in comparison with reported electrocatalytic ammoxidation systems. Reaction conditions: two-electrode system, benzaldehyde (0.24 mmol) and desired quantity of NH3∙H2O in 12.0 mL electrolyte (0.1 mol·L−1 KOH/MeCN, v/v = 11:5).

Fig. 4. Reaction mechanisms. (a) Multi-potential i-t curves of e-Co in 0.1 mol·L−1 KOH and under ammoxidation conditions. (b) LSV of Co-MOF and e-Co with a mixture of hemiaminal and imine intermediate in a 0.1 mol·L−1 Bu4NPF6/MeCN solution. (c) Evolution of the Co-active site and the promotional mechanism for electrocatalytic ammoxidation.

Table 1 Substrates scope. Electrosynthesis of nitriles catalyzed by e-Co a.

Fig. 5. Scalability and Expandability. (a) Effect of starting concentrations of benzaldehyde for the synthesis of benzonitrile using e-Co electrocatalyst. Reaction conditions: desired quantity of benzaldehyde, 2.4 mL NH3·H2O (aq.), and 9.6 mL 0.1 mol·L−1 KOH/MeCN, e-Co as anode, NS as cathode, 1.2 V. (b) Gram-scale synthesis of nitriles using e-Co with a geometric surface area of 7.5 cm2. Reaction conditions: 10 mmol 3a, 20 mL NH3∙H2O (aq.), and 80 mL KOH/MeCN, 1.4 V for 96 h. 9 mmol 3v, 3w or 3ab, 18 mL NH3∙H2O (aq.) and 72 mL KOH/MeCN, 1.6 V for 120 h.

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水系电催化氨氧化反应中MOFs活性位点的原位演变

In-situ developed active sites of MOFs in aqueous electrocatalytic ammoxidation

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