Fe(III)介导的无金属吡啶基COF自维持光芬顿系统: 界面电子转移驱动水净化

doi:10.1016/S1872-2067(25)64890-X

催化学报 ›› 2026, Vol. 82: 225-237.DOI: 10.1016/S1872-2067(25)64890-X

Fe(III)介导的无金属吡啶基COF自维持光芬顿系统: 界面电子转移驱动水净化

张如梦^a, 林沐珂^a, 焦奕木^a, 陈诚^b, 胡孟良^c, 周昊^a, 夏德华^a^,^*()

^a中山大学环境科学与工程学院, 广东省环境污染控制与修复技术重点实验室, 广东广州 510275
^b中国科学技术大学环境科学与工程系, 先进环境技术国家重点实验室, 安徽合肥 230026
^c中山大学材料学院, 广东深圳 518107

收稿日期:2025-08-19 接受日期:2025-09-15 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: xiadehua3@mail.sysu.edu.cn (夏德华).
基金资助:
国家自然科学基金(41603097);国家自然科学基金(21673086);国家自然科学基金(52070195);国家自然科学基金(32071322);国家自然科学基金(22476221);广东基础与应用基础研究基金(2022B1515020097)

Fe(III)-mediated self-sustaining photo-Fenton system on metal-free pyridine-COF: Interfacial electron transfer for water purification

Rumeng Zhang^a, Muke Lin^a, Yimu Jiao^a, Cheng Chen^b, Mengling Hu^c, Hao Zhou^a, Dehua Xia^a^,^*()

^aGuangdong Provincial Key Laboratory of Environmental Pollution Control and Remediation Technology, School of Environmental Science and Engineering, Sun Yat-Sen University, Guangzhou 510275, Guangdong, China
^bState Key Laboratory of Advanced Environmental Technology, Department of Environmental Science and Engineering, University of Science and Technology of China, Hefei 230026, Anhui, China
^cSchool of Materials, Sun Yat-Sen University, Shenzhen 518107, Guangdong, China

Received:2025-08-19 Accepted:2025-09-15 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: xiadehua3@mail.sysu.edu.cn (D. Xia).
Supported by:
National Natural Science Foundation of China(41603097);National Natural Science Foundation of China(21673086);National Natural Science Foundation of China(52070195);National Natural Science Foundation of China(32071322);National Natural Science Foundation of China(22476221);Guangdong Basic and Applied Basic Research Foundation(2022B1515020097)

摘要/Abstract

摘要：

高级氧化技术(AOPs)中的Fenton工艺是降解水体中难降解有机污染物的关键手段, 其通过羟基自由基(·OH)实现高效净化, 但传统Fenton系统存在两大核心瓶颈: 一是需依赖外源过氧化氢(H₂O₂)作为氧化剂, 增加运行成本且存在运输储存风险; 二是Fe(III)/Fe(II)循环效率低下, 易产生铁泥二次污染并限制pH适用范围. 虽有电芬顿、牺牲试剂添加等改进策略, 但往往伴随持续能耗输入、化学试剂残留或复杂工程问题, 难以满足规模化环境应用需求. 因此, 开发无金属、太阳能驱动的Fe(III)高效还原与H₂O₂原位生成一体化平台, 成为突破传统Fenton技术局限的核心方向.

本文通过溶剂热缩合反应, 合成无金属吡啶基共价有机框架TpBpy-COF, 构建了太阳能驱动的自维持光Fenton净水系统; 其富电子的双吡啶氮(μ-N,N)位点作为Fe(III)/Fe(II)还原氧化循环和2e^-氧还原反应的活性位点, 而缺电子的β-酮烯胺连接的苯单元驱动2e^-水氧化反应, 实现双路径原位产H₂O₂, 产率高达1300 μmol g^-1 h^-1且无需外源试剂. 该系统在模拟太阳光下, 60 min内对咖啡因、磺胺甲噁唑、对乙酰氨基酚等多种药物污染物降解率超80%, 30 min内可完全灭活大肠杆菌(10^6.5 CFU mL^-1), 且在河水、污水处理厂出水等实际水体中仍保持高降解效率, 循环使用6次后活性无显著衰减. 通过X射线光电子能谱证实反应中Fe(III)向Fe(II)的高效转化(60 min时Fe(II)占比显著提升), 原位红外吸收光谱追踪到H₂O₂生成的特征信号. 密度泛函理论计算揭示μ-N,N位点对Fe(III)的强吸附作用及电子转移机制, 证实该位点通过d-p轨道杂化降低Fe(III)还原能垒. 此设计突破了传统Fenton系统对Fe(II)引发剂的依赖, 实现无金属COF基平台集成双路径H₂O₂生成与自主Fe(III)/Fe(II)循环, 同时避免金属浸出问题, 且具备药物降解与致病菌灭活的多功能净水能力, 远超现有COF基Fenton体系的综合性能.

综上, 本研究通过精准调控TpBpy-COF的电子结构与活性位点空间分布, 构建了高效稳定的无金属自维持光Fenton系统, 不仅解决了传统Fenton技术的核心瓶颈, 也为共价有机框架材料在太阳能驱动高级氧化过程中的应用提供了新范式, 对推动环境友好型净水技术的规模化发展具有重要理论与实际意义.

关键词: 无金属芬顿催化, 共价有机框架, 自维持氧化还原循环, 高级氧化技术, H₂O₂原位生成, 水净化

Abstract:

Sluggish Fe(III)/Fe(II) cycling and inefficient two-electron H₂O₂ production severely limit the practicality of conventional photocatalytic Fenton systems. In this study, we present a metal-free pyridine-based covalent organic framework (TpBpy-COF) that enables a highly efficient and self-sustaining photo-Fenton process. The system is designed to integrate dual-path H₂O₂ production—through oxygen reduction reaction (ORR) and water oxidation reaction (WOR), along with interfacial Fe(III) reduction. Electron-rich dual-pyridinic nitrogen (μ-N,N) bridging sites facilitate Fe(III)/Fe(II) redox cycling and direct 2e^- ORR, while β-ketoenamine-linked benzene units promote 2e^- WOR, working synergistically to enable continuous in situ H₂O₂ generation. This cooperative mechanism leads to outstanding water purification performance, including rapid degradation of pharmaceuticals (e.g., caffeine), complete microbial inactivation, and robust stability across diverse real water matrices. In-situ spectroscopy and density functional theory calculations elucidate the atomic-scale synergy: pyridinic-N sites selectively reduce Fe(III) and activate O₂, while β-ketoenamine-linked benzene units oxidize water via spatially decoupled charge transfer, collectively enabling autonomous Fenton cycles. This work pioneers a self-sustained Fenton paradigm through a metal-free COF architecture that synergizes dual-path H₂O₂ generation and autonomous Fe(III)/Fe(II) cycling, offering a solar-driven platform for eco-adaptive water purification with negligible reliance on exogenous reagents or energy inputs.

Key words: Metal-free Fenton catalysis, Covalent organic frameworks, Self-sustaining redox cycling, Advanced oxidation processes, In-situ H₂O₂ production, Water purification

张如梦, 林沐珂, 焦奕木, 陈诚, 胡孟良, 周昊, 夏德华. Fe(III)介导的无金属吡啶基COF自维持光芬顿系统: 界面电子转移驱动水净化[J]. 催化学报, 2026, 82: 225-237.

Rumeng Zhang, Muke Lin, Yimu Jiao, Cheng Chen, Mengling Hu, Hao Zhou, Dehua Xia. Fe(III)-mediated self-sustaining photo-Fenton system on metal-free pyridine-COF: Interfacial electron transfer for water purification[J]. Chinese Journal of Catalysis, 2026, 82: 225-237.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64890-X

https://www.cjcatal.com/CN/Y2026/V82/I3/225

图/表 5

Fig. 1. Synthesis and comprehensive characterization of TpBpy-COF. (a) Schematic illustration of the synthesis of TpBpy-COF. (b) Atomic structure model of TpBpy-COF. (c) Experimental PXRD pattern with simulated AA-stacking configuration. (d) SEM image of TpBpy-COF. (e) TEM image. (f) HRTEM image. (g) HAADF-STEM image and corresponding elemental maps. (h) N2 adsorption-desorption isotherms and corresponding pore size distribution. (i,j) FTIR and Raman spectrum of TpBpy-COF. (k) High-resolution XPS spectra of C 1s and N 1s. (l) UV-vis DRS with Tauc plot inset (bandgap determination). (m) Mott-Schottky plot (flat-band potential analysis). (n) Transient photocurrent of TpBpy-COF (inset: KPFM potential mapping). (o) Surface potential from KPFM image of TpBpy-COF (inset: average surface potential selection area).

Fig. 2. Degradation performance and mechanistic study of TpBpy-COF/Fe(III) photo-self-Fenton system. (a b) CAF removal efficiency under different control conditions within 60 min. Pseudo-first-order kinetics of CAF degradation as a function of TpBpy-COF dosage (c) and Fe(III) concentration (95% CI) (d). (e) Light-intensity-dependent rate constant (k) for CAF degradation. (f) High-valent iron species probed by PMSO oxidation to PMSO2 (30 μmol L-1). (g) EPR spectra of ·OH, O2?-, and 1O2 in the system. (h) ROS contribution to CAF degradation and the impact of different atmospheres (O2, N2). (i) CAF removal efficiency in diverse real water matrices. Error bars represent standard deviation from triplicate test.

Fig. 3. Dual-pathway mechanism for photocatalytic in situ H2O2 generation. (a) H2O2 production performance of TpBpy-COF under visible light irradiation (inset: comparative yields under light and dark conditions). (b) Quenching effects on H2O2 yield with EDTA-2Na (20 mmol L-1) and KBrO3 (0.1 mol L-1). (c) Quenching effects with CHCl3 (20 m mol L-1) and TBA (10%). (d) In-situ ATR-SEIRAS spectra for the photocatalytic system of TpBpy-COF. (e) Calculated free-energy diagram for ORR pathways with different sites. (f) Gibbs free-energy diagram for 2e- WOR-H2O2 and 4e- WOR-H2O2 pathway. (g,h) Optimized O2 adsorption configurations at two distinct active sites. (i) H2O adsorption configuration. (j) Dual-pathway (ORR/WOR) H2O2 generation mechanism via O2 and H2O activation on TpBpy-COF (isosurface ±0.0013 e ?-3, yellow/blue: electron depletion/accumulation).

Fig. 4. Fe(III)/Fe(II) cycling promotion and interfacial reaction mechanisms. Fe species in TpBpy-COF/Fe(III) system at different initial concentrations: 40 μmol L-1 (a) and 80 μmol L-1 (b). XPS Fe 2p spectra of used TpBpy-COF catalyst: after 5 min (c) and 60 min (d) reaction. (e) CV curves under different conditions. (f) Open-circuit potential profiles with sequential additions of reagents. ([Na2SO4]0 = 0.5 mol L-1, [Fe(III)]add = 1.0 mmol L-1, [CAF]add = 10.0 mg L-1). (g) Comparative activation barriers for Fe(III) reduction at different sites. (h) Projected density of states (PDOS) of Fe(III)-adsorbed TpBpy-COF systems. (i) Fe(III) activation mechanism showing charge transfer, N-Fe coordination, and 2D ELF (yellow/blue: electron depletion/accumulation regions, isosurface = ±0.0016 e ?-3).

Fig. 5. Multifunctionality and stability of TpBpy-COF/Fe(III) photo-self-Fenton system. (a) Temporal evolution of pollutant concentrations (CAF, SMX, PCM, NPX, CBZ). (b) Pseudo-first-order kinetics of pollutant degradation with observed rate constants (kobs). (c) Recyclability test for CAF degradation over six cycles. (d) Antimicrobial activity against E. coli (inset: colony-forming unit comparisons pre-/post-treatment). (e) Photocatalytic self-Fenton flow reactor and schematic diagram. (f) Underlying mechanisms governing the elevated oxidative capability in the TpBpy-COF/Fe(III) system.

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Fe(III)介导的无金属吡啶基COF自维持光芬顿系统: 界面电子转移驱动水净化

Fe(III)-mediated self-sustaining photo-Fenton system on metal-free pyridine-COF: Interfacial electron transfer for water purification

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