铁镍纳米颗粒与单原子位点协同驱动非自由基类芬顿催化反应: 单线态氧和电子转移途径主导的高效水净化

doi:10.1016/S1872-2067(25)64881-9

催化学报 ›› 2026, Vol. 82: 187-200.DOI: 10.1016/S1872-2067(25)64881-9

铁镍纳米颗粒与单原子位点协同驱动非自由基类芬顿催化反应: 单线态氧和电子转移途径主导的高效水净化

韩贝^a^,^b, 靳宸^a^,^b, 罗翠红^a^,^b, 刘云焘^a^,^b, 戴志超^a, 孙运强^a, 甘自保^a, 王崇臣^a^,^c^,^*(), 郑秀文^a^,^b^,^*(), 胡尊富^a^,^*()

^a临沂大学化学与化学工程学院, 山东省先进生物材料与纳米医学高校重点实验室, 山东临沂 276000
^b齐鲁师范学院, 山东济南 250200
^c北京建筑大学未来新材料研究院, 建筑结构与环境修复功能材料北京市重点实验室, 城市雨水系统与水环境教育部重点实验室，北京 100044

收稿日期:2025-07-26 接受日期:2025-08-29 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: zhengxiuwen@lyu.edu.cn (郑秀文),huzunfu@lyu.edu.cn (胡尊富),wangchongchen@bucea.edu.cn (王崇臣).
基金资助:
国家自然科学基金(22371108);山东省泰山学者计划(tsqn202211242);山东省自然科学基金(ZR2023MB150);山东省自然科学基金(ZR2022MA026)

FeNi nanoparticles cooperate with single-atom sites to drive non-radical fenton-like catalysis: Dominant singlet oxygen and electron transfer pathways for efficient wastewater purification

Bei Han^a^,^b, Chen Jin^a^,^b, Cuihong Luo^a^,^b, Yuntao Liu^a^,^b, Zhichao Dai^a, Yunqiang Sun^a, Zibao Gan^a, Chong-Chen Wang^a^,^c^,^*(), Xiuwen Zheng^a^,^b^,^*(), Zunfu Hu^a^,^*()

^aKey Laboratory of Advanced Biomaterials and Nanomedicine in Universities of Shandong, College of Chemistry and Chemical Engineering, LinyiUniversity, Linyi 276000, Shandong, China
^bQilu Normal University, Jinan 250200, Shandong, China
^cInstitute of Advanced Materials, Beijing Key Laboratory of Functional Materials for Building Structure and Environment Remediation, Key Laboratory of Urban Stormwater System and Water Environment (Ministry of Education), Beijing University of Civil Engineering and Architecture, Beijing 100044, China

Received:2025-07-26 Accepted:2025-08-29 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: zhengxiuwen@lyu.edu.cn (X. Zheng),huzunfu@lyu.edu.cn (Z. Hu),wangchongchen@bucea.edu.cn (C.-C. Wang).
Supported by:
National Natural Science Foundation of China(22371108);Taishan Scholar Foundation of Shandong Province(tsqn202211242);Natural Science Foundation of Shandong Province(ZR 2023MB150);Natural Science Foundation of Shandong Province(ZR2022MA026)

摘要/Abstract

摘要：

近年来, 磺胺类抗生素的过度使用对水环境和人体构成潜在显著威胁, 而传统污水处理技术对于上述抗生素难以有效去除, 开发新型高效降解技术已成为研究人员关注的焦点. 基于过一硫酸盐(PMS)的类芬顿催化技术因其高效、易激活、成本低及宽pH范围适用性而广受关注. 凭借极高的原子利用率及独特的可控配位结构，单原子催化剂(SACs)已成为催化领域的重要研究方向. 进而, 优化SACs结构, 增强活性位点的催化活性及稳定性, 提高其类芬顿催化性能是当前单原子催化领域的研究热点之一. 利用金属颗粒调控单分散活性位点电子结构, 实现催化效能和稳定性提高是一种有效策略, 为SACs在抗生素等新污染物治理提供了可行路线.

本文以双金属有机框架化合物为模板成功制备了“竹节虫”形碳纳米管负载铁镍颗粒协同单分散活性位点催化剂((FeNi)_NPs,SAs-N-C). 与传统二维片状载体相比, 本研究中制备的碳纳米管能有效保护活性位点, 提高活性位点稳定性, 同时增强电荷传输效率. 利用扫描电镜、高分辨透射电镜和高角度环形暗场扫描透射电镜等表征手段对(FeNi)_NPs,SAs-N-C的结构进行了充分解析, 证实了碳纳米管及铁镍颗粒和单分散位点的共存. X射线光电子能谱、X射线吸收近边结构和扩展X射线吸收精细结构等表征结果进一步证明铁和镍呈现多种价态, 且铁/镍原子通过与氮原子配位形成了单分散位点(Fe-N₂/Ni-N₂). 系列降解实验结果表明, (FeNi)_NPs,SAs-N-C相较对照催化剂(MIL-88B(Fe), MIL-88B(Fe, Ni)及Fe_{NPs, SAs}-N-C)催化性能提高了16、17及7倍. 此外, 其PMS利用率、pH适应性及抗基质干扰性能也尤为突出. 为探究催化体系降解机理, 利用自由基猝灭实验、电子顺磁共振和电化学方法等方法对降解过程的活性物种进行了鉴别. 实验结果表明, 磺胺甲噁唑(SMZ)的降解主要以单线态氧(¹O₂)和电子转移的非自由基路径为主. 与此同时, 结合液相色谱-质谱联用技术确定了SMZ的降解路径. 借助毒性评估工具以及豆芽实验对降解过程中SMZ的中间产物进行毒性评估, 有力地证明了降解产物安全性. 通过密度泛函理论计算深入揭示了通过单线态氧和电子转移过程降解SMZ的机理, 阐明了镍掺杂优化后的(FeNi)_NPs,SAs-N-C催化剂增强与PMS相互作用的机制.

综上, 本工作构建了一种铁镍纳米粒子耦合单原子位点催化剂((FeNi)_NPs,SAs-N-C), 并通过实验与理论分析系统揭示了其颗粒与单分散位点间的协同机制. 本研究提出了一种可行的用于制备高效的纳米粒子与单原子位点协同催化剂的方法, 为开发创新性单原子催化剂用于废水净化提供了可行技术路线.

关键词: 类芬顿, 双金属催化剂, 纳米颗粒和单原子, 单线态氧(¹O₂), 电子转移

Abstract:

Heterogeneous Fenton-like systems provide sustainable water-purification solutions; however, improving their catalytic efficiency and recyclability remains challenging. We developed a facile strategy to prepare an FeNi nanoparticle (NPs)-coupled single-atom site catalyst ((FeNi)_NPs,SAs-N-C)), which exhibits a strong synergy between FeNi NPs and monodisperse Fe/Ni active sites. This catalyst effectively activates peroxymonosulfate (PMS) at low concentrations (0.2 mmol/L), generating abundant reactive oxygen species. Under the condition of continuous flow, the optimized system achieved over 99% sulfamethazine degradation within 3000 min, with a kinetic rate constant (k = 1.5758 min^-1) that is 16, 17, and 7 times higher than those of MIL-88B(Fe), MIL-88B(Fe,Ni) and Fe_NPs,SAs-N-C, respectively. Mechanistic studies showed that PMS activation occurs via a nonradical pathway dominated by singlet oxygen (¹O₂) and direct electron transfer, enhancing the resistance to interference from inorganic anions and natural organic matter. Density functional theory calculations showed that FeNi NPs donated electrons to affect the d-orbitals in Fe single-atom sites, enhancing their interaction with PMS to produce ¹O₂ and enable electron transfer. This study presents a viable method for creating efficient NPs coupled with single-atom site catalysts for environmental clean-up.

Key words: Fenton-like, Bimetallic catalyst, Nanoparticles and single atoms, Singlet oxygen (¹O₂), Electron transfer

韩贝, 靳宸, 罗翠红, 刘云焘, 戴志超, 孙运强, 甘自保, 王崇臣, 郑秀文, 胡尊富. 铁镍纳米颗粒与单原子位点协同驱动非自由基类芬顿催化反应: 单线态氧和电子转移途径主导的高效水净化[J]. 催化学报, 2026, 82: 187-200.

Bei Han, Chen Jin, Cuihong Luo, Yuntao Liu, Zhichao Dai, Yunqiang Sun, Zibao Gan, Chong-Chen Wang, Xiuwen Zheng, Zunfu Hu. FeNi nanoparticles cooperate with single-atom sites to drive non-radical fenton-like catalysis: Dominant singlet oxygen and electron transfer pathways for efficient wastewater purification[J]. Chinese Journal of Catalysis, 2026, 82: 187-200.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64881-9

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Fig. 1. (a) Schematic of (FeNi)NPs,SAs-N-C synthesis. (b) PXRD patterns of catalysts. (c) TEM image. (d) SEM image. (e) HRTEM image. (f,g) AC-HAADF-STEM images of the (FeNi)NPs,SAs-N-C (atomic Fe and Ni species circled by red). (h) EDS mapping images of (FeNi)NPs,SAs-N-C.

Fig. 2. (a) XPS spectra of N 1s. (b) Fe K-edge XANES. (c) Ni K-edge XANES. (d) Fe K-edge FT-EXAFS spectra. (e) Ni K-edge FT-EXAFS spectra. (f) Fe K-edge EXAFS fitting curves. (g) Ni K-edge EXAFS fitting curves. (h,i) WT of (FeNi)NPs,SAs-N-C.

Fig. 3. Catalytic degradation of SMZ (a) and the corresponding reaction rate constants and removal efficiency (b) in various reaction systems. (c) Summary of experimental data for optimizing reaction conditions. (d) Effect of various anions and organics on SMZ removal by (FeNi)NPs,SAs-N-C+PMS system. (e) Effects of HA, SA and BSA on SMZ degradation in the FeNPs,SAs-N-C+PMS and (FeNi)NPs,SAs-N-C+PMS systems. (f) Cyclic experiment for the (FeNi)NPs,SAs-N-C+PMS system. (g) SMZ degradation in simulated wastewater prepared using different water environments with the (FeNi)NPs,SAs-N-C+PMS system. (h) Removal of various pollutants by the (FeNi)NPs,SAs-N-C+PMS system. (i) k values for degradation with different catalyst systems.

Fig. 4. (a) SMZ removal rate constants of various quenching systems. (b) Oxidation of trans-stilbene in the reactions of (FeNi)NPs,SAs-N-C+PMS and (c) FeNPs,SAs-N-C+PMS systems. (d) UV-vis spectra of DPBF in the MIL-88B(Fe)+PMS, MIL-88B(Fe,Ni)+PMS, FeNPs,SAs-N-C+PMS and (FeNi)NPs,SAs-N-C+PMS systems. (e) SMZ oxidation via a premixture of (FeNi)NPs,SAs-N-C and PMS at estimated time intervals. (f) ESR spectra for 1O2, ?OH, SO4?- and ?O2-. (g) Contributions of various ROS for SMZ degradation in the (FeNi)NPs,SAs-N-C+PMS and FeNPs,SAs-N-C+PMS systems.

Fig. 5. (a) Scheme of GOS with catalyst. (b) LSV of (FeNi)NPs,SAs-N-C electrodes under different conditions. (c) EIS spectra of MIL-88B(Fe), MIL-88B(Fe,Ni), FeNPs,SAs-N-C and (FeNi)NPs,SAs-N-C. (d) I-t curves. (e) Radar chart of SMZ degradation/PMS usage rate, COD and 1O2 yield of these catalysts. (f) Toxicity evaluation of intermediates. (g) Toxicity levels of the (FeNi)NPs,SAs-N-C+PMS system. Evaluation of SMZ removal using fresh (FeNi)NPs,SAs-N-C+PMS (h) and regenerated (FeNi)NPs,SAs-N-C+PMS (i) systems.

Fig. 6. (a) Front and side views of FeNPs,SAs-N-C and (FeNi)NPs,SAs-N-C. Blue, green, gray and gold spheres represent Fe, Ni, N and C atoms, respectively. (b) Eads, lO-O and Bader charges of PMS adsorbed on the FeNPs,SAs-N-C and (FeNi)NPs,SAs-N-C. Blue represent electron accumulation and yellow represent electron depletion. (c) Bader charges of FeNPs,SAs-N-C and (FeNi)NPs,SAs-N-C. Blue represent electron accumulation and yellow represent electron depletion. (d) Free energy profiles of 1O2 and FeIVNx=O in different systems. (e) PDOS of Fe atoms and N atoms and the d-band center of Fe sites in FeNPs,SAs-N-C and (FeNi)NPs,SAs-N-C. (f) Adsorption configuration and corresponding adsorption energy of FeIVN4=O on the amido gen sites (-NH2) of SMZ and FeIVN2=O on imino (-NH) sites of SMZ. (g) Schematic illustration of different attack pathways of SMZ at FeIVN4=O and FeIVN2=O sites.

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铁镍纳米颗粒与单原子位点协同驱动非自由基类芬顿催化反应: 单线态氧和电子转移途径主导的高效水净化

FeNi nanoparticles cooperate with single-atom sites to drive non-radical fenton-like catalysis: Dominant singlet oxygen and electron transfer pathways for efficient wastewater purification

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