原子钴掺杂AgFeO2对过一硫酸盐活化过程中Fe(Ⅲ)电子结构调控的定量关联

doi:10.1016/S1872-2067(25)64784-X

催化学报 ›› 2025, Vol. 77: 87-98.DOI: 10.1016/S1872-2067(25)64784-X

原子钴掺杂AgFeO₂对过一硫酸盐活化过程中Fe(Ⅲ)电子结构调控的定量关联

徐晨^a^,¹, 宋迪^a^,¹, 刘行刚^a, 邓芳^a^,^*(), 张永才^b, 朱明山^c^,^*(), 刘熙俊^d, 邹建平^a, 罗旭彪^a

^a南昌航空大学环境与化学工程学院, 江西省持久性污染物防控与资源再利用重点实验室, 江西南昌 330063
^b扬州大学化学化工学院, 江苏扬州 225009
^c暨南大学环境与气候学院, 广东广州 511443
^d广西大学资源环境与材料学院, 广西南宁 530004

收稿日期:2025-04-27 接受日期:2025-06-17 出版日期:2025-10-18 发布日期:2025-10-05
通讯作者: *电子信箱: dengfang40030@126.com (邓芳),zhumingshan@jnu.edu.cn (朱明山).
作者简介:¹共同第一作者.
基金资助:
国家自然科学基金(52470078);江西省主要学科学术和技术带头人(20213BCJL22053);江西省持久性污染物防控与资源再利用重点实验室(2023SSY02061);重金属污染物控制与资源化国家地方联合工程研究中心开放基金(ES202380056)

Quantitative correlation of Fe(III) electronic structure regulation in peroxymonosulfate activation via atomic cobalt doping AgFeO₂

Chen Xu^a^,¹, Di Song^a^,¹, Xinggang Liu^a, Fang Deng^a^,^*(), Yongcai Zhang^b, Mingshan Zhu^c^,^*(), Xijun Liu^d, Jianping Zou^a, Xubiao Luo^a

^aKey Laboratory of Jiangxi Province for Persistent Pollutants Prevention Control and Resource Reuse, Nanchang Hangkong University, Nanchang 330063, Jiangxi, China
^bSchool of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225009, Jiangsu, China
^cCollege of Environment and Climate, Jinan University, Guangzhou 511443, Guangdong, China
^dSchool of Resources, Environment and Materials, Guangxi University, Nanning 530004, Guangxi, China

Received:2025-04-27 Accepted:2025-06-17 Online:2025-10-18 Published:2025-10-05
Contact: *E-mail: dengfang40030@126.com (F. Deng), zhumingshan@jnu.edu.cn (M. Zhu).
About author:¹Contributed equally to this work.
Supported by:
National Natural Science Foundation of China(52470078);Jiangxi Academic and Technical Leader of Major Disciplines(20213BCJL22053);Key Laboratory of Jiangxi Province for Persistent Pollutants Prevention Control and Resource Reuse(2023SSY02061);National Local Joint Engineering Research Center of Heavy Metals Pollutants Control and Resource Utilization Open Fund(ES202380056)

摘要/Abstract

摘要：

水污染治理是当前面临的严峻挑战, 过一硫酸盐(PMS)高级氧化技术因其高效降解有机污染物能力而备受关注. 催化剂表面电子结构调控是提升PMS活化效率的关键策略, 然而电子结构调控如何定量影响PMS吸附、活化及催化性能的机制尚不明晰. 深入理解该机制对于设计高效的非均相类芬顿催化体系至关重要. 本研究聚焦于通过原子级掺杂精准调控催化剂的电子结构, 旨在揭示其与PMS活化性能的定量构效关系, 为高性能催化材料的设计提供理论依据.

本研究提出通过原子级钴掺杂调控AgFeO₂中Fe(III)阳离子的3d电子构型, 成功制备了AgFe_1-_xCo_xO₂ (x = 0, 0.05, 0.10, 0.15, 0.20)催化剂. 结合系统的表征(X射线衍射、X射线光电子能谱、电子顺磁共振、X射线吸收近边结构、扩展X射线吸收精细结构和磁性测量)和密度泛函理论计算(DFT), 深入研究了Co掺杂对Fe(III)电子结构(包括自旋态、有效磁矩μ_eff、e_g轨道填充)的调控作用. 研究发现, 随着Co掺杂量增加, 催化剂中Fe(III)的高自旋态比例、总有效磁矩和e_g轨道填充量均显著增加, Fe(III)的3d电子构型从AgFeO₂中的t₂_g⁴e_g¹转变为AgFe_0.80Co_0.20O₂中的t₂_g³e_g². 关键发现在于建立了催化剂电子结构参数与PMS吸附量及催化活性之间的定量关系: PMS吸附量和氧氟沙星(OFL)降解的拟一级动力学常数(k_obs)均与催化剂的总有效磁矩、高自旋Fe(III)比例以及e_g轨道填充量呈显著正相关, 而与低自旋Fe(III)比例呈负相关. DFT计算揭示了性能提升的微观机制: Co掺杂引起Fe(III)电子结构优化, 特别是Fe(III)的e_g轨道填充增加和dz²轨道占据减少导致PMS在Fe位点上的吸附能显著降低, 被吸附的PMS分子中S-O键长增加, 表明PMS在AgFe_0.80Co_0.20O₂表面的结合更强、更易活化; 同时, 费米能级附近的电子态密度增加, 电子传导性增强. 这些变化共同促进了PMS的吸附和后续的电子转移过程. 得益于电子结构的精细调控, 最优催化剂AgFe_0.80Co_0.20O₂展现出卓越的PMS活化性能. 在优化条件下, AgFe_0.80Co_0.20O₂催化剂30 min内对OFL的去除率高达98.4%, k_obs是未掺杂AgFeO₂的4倍以上, TOC去除率达75.7%. 机理研究表明, AgFe_0.80Co_0.20O₂/PMS体系中O₂^•‒和电子转移对OFL降解起主导作用, 而Co掺杂改变了AgFeO₂/PMS体系中高价金属氧物种主导的活性物种生成路径, 促进了表面电子转移. 电化学测试进一步证实了AgFe_0.80Co_0.20O₂具有更优异的电子转移能力. AgFe_0.80Co_0.20O₂催化剂表现出良好的抗干扰能力和循环稳定性. 该AgFe_0.80Co_0.20O₂/PMS体系成功应用于实际制药废水的处理, TOC和COD去除率分别达49.1%和71%, 显著提高了废水的可生化性. 在72 h的连续流实验中, 仅使用0.1 g催化剂的填充柱对OFL(10 mg L^-1)的去除率稳定在80%以上, 展现了巨大的实际应用潜力.

综上所述, 本研究通过原子级Co掺杂实现了AgFeO₂中Fe(III) 3d电子构型的精准调控, 建立了PMS吸附量及催化活性与Fe(III)电子结构参数的定量关系, 并从吸附能和电子转移角度阐明了性能提升的微观调控机制. AgFe_0.80Co_0.20O₂催化剂在实际制药废水处理和连续流实验中均表现出的优异性能和稳定性证实其在实际应用中的巨大潜力. 这项工作为理解电子结构调控对PMS活化的影响机制提供了新的见解, 为未来设计高效、稳定的非均相类芬顿催化体系提供了重要的理论指导和设计思路.

关键词: 3d电子构型, 多相催化, 过一硫酸盐活化, 电子转移, AgFeO₂

Abstract:

The influence of electronic structure on the performance of catalysts for peroxymonosulfate (PMS) activation remains ambiguous. In this study, the 3d electron configuration of Fe(III) in AgFeO₂ was atomically regulated using cobalt doping. The amount of PMS adsorbed and the catalytic performance were positively correlated with the total effective magnetic moment and the ratios of high-spin Fe(III) and e_g filling within the catalysts. These 3d electron regulations favor PMS adsorption and electron transfer owing to the lower PMS adsorption energy, increased electronic states near the Fermi level, and reduced dz² orbital occupancy. Benefiting from fine tailoring of the electron configuration, the AgFe_0.80Co_0.20O₂ catalyst exhibited outstanding catalytic PMS activation and favorable application potential, achieving efficient pharmaceutical wastewater treatment and more than 80% ofloxacin removal after 72 h of continuous-flow operation. Notably, this study offers a comprehensive understanding for the influence mechanism of electronic structure regulation on PMS activation, providing design guidance for the development of efficient heterogeneous Fenton-like catalytic systems.

Key words: 3d electron configuration, Heterogeneous catalysis, Peroxymonosulfate activation, Electron transfer, AgFeO₂

徐晨, 宋迪, 刘行刚, 邓芳, 张永才, 朱明山, 刘熙俊, 邹建平, 罗旭彪. 原子钴掺杂AgFeO₂对过一硫酸盐活化过程中Fe(Ⅲ)电子结构调控的定量关联[J]. 催化学报, 2025, 77: 87-98.

Chen Xu, Di Song, Xinggang Liu, Fang Deng, Yongcai Zhang, Mingshan Zhu, Xijun Liu, Jianping Zou, Xubiao Luo. Quantitative correlation of Fe(III) electronic structure regulation in peroxymonosulfate activation via atomic cobalt doping AgFeO₂[J]. Chinese Journal of Catalysis, 2025, 77: 87-98.

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Fig. 1. (a) Eads and S-O bond lengths of the adsorbed PMS molecules on AgFeO2 and AgFe0.80Co0.20O2 surface. (b) DOS diagrams of AgFeO2 and AgFe0.80Co0.20O2. (c) PDOS for Fe-3d orbitals in AgFeO2 and AgFe0.80Co0.20O2. (d) PDOS of the Fe eg orbital in AgFeO2 and AgFe0.80Co0.20O2. (e) Schematic sketch of the spin-state-dependent PMS activation process.

Fig. 2. SEM (a), TEM (b) and HRTEM (c) images of AgFe0.80Co0.20O2. (d) EDS mappings of AgFe0.80Co0.20O2.

Fig. 3. XRD patterns (a) and FT-IR spectra (b) of AgFeO2 and AgFe1-xCoxO2. Ag 3d (c), Fe 2p (d), O 1s (e), and Co 2p (f) XPS spectra of AgFeO2 and AgFe0.80Co0.20O2.

Fig. 4. (a) Fe K-edge normalized XANES spectra. (b) FT-EXAFS spectra of AgFeO2, AgFe0.80Co0.20O2 and standard samples. (c) The FT-EXAFS K-space fitting curve of AgFeO2. (d) The FT-EXAFS K-space fitting curve of AgFe1-xCoxO2. (e) EPR spectra of AgFeO2 and AgFe0.80Co0.20O2. (f) Temperature-dependent magnetic susceptibilities of different catalysts. (g) The quantitative changes of μeff,Fe, high spin state, low spin state and eg filling for AgFe1-xCoxO2 with different Co-doping amount. (h) Schematic illustration of strong interaction and eg occupancy of FeOh and CoOh in AgFe0.80Co0.20O2.

Fig. 5. (a) OFL removal efficiency in different AgFe1-xCoxO2/PMS systems. (b) The kobs change with different Co-doping ratio. (c) The TOC removal ratio of OFL solution in AgFe1-xCoxO2/PMS systems with different Co-doping amount. (d) The quantitative correlation of kobs with high spin and low-spin proportion, eg filling and μeff,Fe.

Fig. 6. (a) Quenching experiment of reactive species in AgFe0.80Co0.20O2/PMS. (b) EPR spectra of DMPO-O2?? in AgFeO2/PMS and AgFe0.80Co0.20O2/PMS system. (c) PMS adsorption and consumption in AgFe1-xCoxO2/PMS. (d) Quantitative correlation of PMS adsorption with high spin and low-spin proportion, eg filling and μeff,Fe. (e) Correlation between lnkobs and PMS adsorption quantity. Catalysts: 1 g L-1, C[PMS]: 0.5 mmol L-1, C[MeOH]: 100 mmol L-1, C[BQ] = C[DMSO]: 1 mmol L-1, C[NaN3] = C[IPA] = C[KI]: 10 mmol L-1, C0[OFL]: 15 mg L-1, initial solution pH = 7.0, and T = 25 ± 2 °C.

Fig. 7. (a) I-t curves. (b) LSV curves obtained under different conditions. (c) EIS Nyquist plots in different systems. (d) CV curves of AgFeO2 and AgFe0.80Co0.20O2.

Fig. 8. (a) Influence of various anions on OFL degradation in the AgFe0.80Co0.20O2/PMS system. (b) OFL removal efficiency in different actual water samples. Catalysts: 1 g L-1, C0[OFL]: 15 mg L-1, C[PMS]: 0.5 mmol L-1, and T = 25 ± 2 °C. (c) Consecutive use of AgFe0.80Co0.20O2. (d) Fe 2p XPS spectrum of the recovered AgFe0.80Co0.20O2.

Fig. 9. (a) COD and TOC removal of actual pharmaceutical wastewater by the AgFe0.80Co0.20O2/PMS system. (b) Enhanced biodegradability of pharmaceutical wastewater by the AgFe0.80Co0.20O2/PMS system. (c) The photo of continuous flow reactor. (d) OFL removal by catalyst packed column. catalyst loading = 0.1 g, C0[OFL]: 10 mg L-1, C[PMS]: 0.5 mmol L-1, flow rate = 14 mL h-1).

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原子钴掺杂AgFeO₂对过一硫酸盐活化过程中Fe(Ⅲ)电子结构调控的定量关联

Quantitative correlation of Fe(III) electronic structure regulation in peroxymonosulfate activation via atomic cobalt doping AgFeO₂

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