为解决Fe基MOFs（Fe-MOFs）在类芬顿反应中Fe³⁺/Fe²⁺氧化还原循环慢，材料界面电子转移速度低和Fe-MOFs中Fe³⁺的电子密度高的问题，基于氧化还原偶联反应的原理，采用一步溶剂热法合成了Fe-Cu双金属硝基功能化MOFs材料（NMIL-88B-Cu-1），对其进行表征分析，应用于非均相类芬顿反应降解水体中的刚果红（Congo red，CR），研究了不同材料、H₂O₂用量、pH、CR的浓度、干扰离子对CR降解的影响及材料稳定性与催化降解的机理。结论如下：Fe³⁺和Cu²⁺的摩尔分数均为50%时，能够在α-Fe₂O₃上组装形成六角棒状结构的介孔型NMIL-88B-Cu-1。在CR的浓度为10 mg/L，pH在3~7范围内，NMIL-88B-Cu-1使用量为0.1 g/L，H₂O₂浓度为0.5 mol/L时，反应15 min，能够实现对CR快速高效地降解，CR的降解率达98%，NMIL-88B-Cu-1对CR的降解速率分别是NO₂-MIL-88B的1.95倍和MIL-88B的2.24倍。在循环4次实验后，CR的降解率达92%，Fe³⁺/Fe²⁺的含量比值仅降低了5%，且其晶型结构保持一致，证明了其具有较高的循环稳定性。体系中SO {}_{\mathrm{4}}^{\mathrm{2}-}和NO {}_{\mathrm{3}}^{-}不影响CR的降解，而Cl^-和H₂PO {}_{\mathrm{4}}^{-}抑制了CR的降解。机理分析表明，硝基功能化的材料中心Fe³⁺的电子密度低，Cu²⁺的引入构建了Fe-Cu双金属MOFs材料，通过Fe与Cu之间的氧化还原偶联反应和Fe-Cu的协同作用，有效促进了Fe²⁺形成，加速了NMIL-88B材料界面e^-转移，产生的·OH能够将CR氧化降解为CO₂和H₂O等无机小分子物质。

To solve the problems in Fenton-like reactions， such as slow Fe³⁺/Fe²⁺ redox cycle， low electron transfer rate at the material interface， and high electron density of Fe³⁺ in Fe-MOFs， Fe-Cu bimetallic nitro-functionalized MOFs material （NMIL-88B-Cu-1） is synthesized by a one-step solvothermal method based on the principle of redox coupling reaction. The material is characterized and applied to effectively degrade Congo red （CR） in a Fenton-like process. The effects of different materials， H₂O₂ dosage， pH， CR concentration， and coexisting ions on the degradation of CR are investigated. The stability of materials is verified， and the catalytic degradation mechanism is proposed. The results show that when the molar percentage of Fe³⁺ and Cu²⁺ are both 50%， NMIL-88B-Cu-1 with hexagonal rod structure and mesoporous can be assembled on α-Fe₂O₃. When CR is 10 mg/L， pH value is 3-7， NMIL-88B-Cu-1 catalyst is 0.1 g/L， and H₂O₂ is 0.5 mol/L， CR can be rapidly and efficiently degraded in 15 min. The degradation efficiency of CR is 98%， which is 1.95 times that of NO₂-MIL-88B and 2.24 times that of MIL-88B， respectively. The CR degradation efficiency could still reach 92% after 4 cycles， the content ratio of Fe³⁺/Fe²⁺ is only reduced by 5%， and its crystal structure remains the same， exhibiting the high cycle stability of NMIL-88B-Cu-1. In the system SO {}_{\mathrm{4}}^{\mathrm{2}-} and NO {}_{\mathrm{3}}^{-} do not affect the degradation of CR， while Cl^- and H₂PO {}_{\mathrm{4}}^{-} with a concentration of 0.09 mo/L show an inhibitory effect on the degradation of CR. The analysis of the mechanism shows that the electron density of Fe³⁺ in the center of the nitro-functionalized material is low， and the introduction of Cu²⁺ constructs Fe-Cu bimetallic MOFs materials. The redox coupling reaction between Fe and Cu and the synergistic effect of Fe-Cu promote the formation of Fe²⁺ effectively， and accelerate the e^- transfer at the interface of NMIL-88B. The generated ·OH can oxidize and degrade CR into inorganic small molecules such as CO₂ and H₂O.