金属有机骨架MIL-100(Fe)高的铁氧簇含量、大的比表面积、合适的光响应能级，使其可作为理想的非均相光芬顿催化剂，但MIL-100(Fe)的应用容易受光吸收能力弱、电荷分离效率低和粉体回收困难的限制。本论文提出基于单分散的Ag/Fe3O4（AF）核壳纳米颗粒，分别采用连续离子层吸附反应（SILAR）和水热法，简便快速构建可磁分离、高光芬顿活性AgCl/Fe3O4@MIL-100(Fe)（ACFM）和Ag/Fe3O4@MIL-100(Fe)（AFM）的新方法。在此基础上，通过巧妙调控水热反应中Fe3+用量，可控制备了MIL-100(Fe)比例更高、光芬顿性能更优的F/Ag/Fe3O4@MIL-100(Fe)和中空Fe3O4@MIL-100(Fe)催化剂（F/AFM和HFM）。主要研究内容和结果如下：

（1）通过SILAR一步合成AgCl和MIL-100(Fe)，构建了可磁分离ACFM异质结。此合成方法过程简单，ACFM中MIL-100(Fe)含量可控。由于AgCl和MIL-100(Fe)异质结界面有效的电荷分离，制备的ACFM-15具有优异的光芬顿活性，在30 min光芬顿反应后对RhB的降解率达92.9%，高于sFM-15的光芬顿活性。

（2）通过AF与H3btc的直接水热反应，制备了可磁分离的单分散AFM核壳结构。此方法可有效避免Ag纳米颗粒的聚集，通过H3btc的用量调控MIL-100(Fe)的负载量。得益于Ag纳米颗粒对光吸收和电荷分离的增强作用，所制备的AFM-2具有优异的光芬顿性能，30 min光芬顿反应后可降解88.5%的RhB，远高于hFM的光芬顿活性。

（3）在AF与H3btc的水热反应中引入Fe3+，并通过调控Fe3+用量合成了F/AFM和HFM两种结构。Fe3+的引入增加了催化剂中MIL-100(Fe)的沉积量和比表面积，所制备的F/AFM-1和F/AFM-2在30 min光芬顿反应后对RhB的降解率分别为97.1%和95.9%，均优于AFM-2。

Metal-organic framework MIL-100(Fe) has high iron-oxygen cluster content, large specific surface area and suitable energy level to response light, which make it great potential as a heterogeneous photo-Fenton catalyst. However, the application of MIL-100(Fe) is easily limited by its weak light absorption, insufficient charge separation efficiency and difficulty in recycling. In this thesis, we presented the simple and rapid construction of magnetically separable AgCl/Fe₃O₄@MIL-100(Fe) (ACFM) and Ag/Fe₃O₄@MIL-100(Fe) (AFM) with high photo-Fenton activity based on monodispersed Ag/Fe₃O₄ (AF) core-shell nanoparticles by using successive ionic layer adsorption and reaction (SILAR) and hydrothermal method, respectively. On this basis, by regulating the Fe³⁺ quantity during the hydrothermal reaction, F/Ag/Fe₃O₄@MIL-100(Fe) and hollow Fe₃O₄@MIL-100(Fe) (F/AFM and HFM) with higher MIL-100(Fe) ratios and better photo-Fenton activities were obtained. The main research contents and results are as follows:

(1) Magnetically separable ACFM heterojunction was constructed by one-step synthesis of AgCl and MIL-100(Fe) via SILAR. The synthetic method is a simple process with controllable content of MIL-100(Fe) in ACFM. Due to the high charge separation efficiency at the interface between AgCl and MIL-100(Fe) heterojunction, the prepared ACFM-15 has excellent photo-Fenton activity, degrading 92.9% of RhB after 30 min photo-Fenton reaction, which is higher than that of sFM-15.

(2) Magnetically separable monodispersed AFM core-shell structures were prepared by direct hydrothermal reaction between AF and H₃btc. This method can effectively avoid the aggregation of Ag nanoparticles, and the loading of MIL-100(Fe) can be regulated by the amount of H₃btc. Thanks to the enhanced light absorption and charge separation by Ag nanoparticles, the prepared AFM-2 has excellent photo-Fenton activity, degrading 88.5% of RhB after 30 min photo-Fenton reaction, which is much higher than that of hFM.

(3) F/AFM and HFM were synthesized by introducing Fe³⁺ into the hydrothermal reaction between AF and H₃btc and modulating the amount of Fe³⁺. The introduction of Fe³⁺ increased the MIL-100(Fe) deposition and specific surface area of catalysts, and the degradation efficiencies of RhB by F/AFM-1 and F/AFM-2 after 30 min photo-Fenton reaction are 97.1% and 95.9%, respectively, both better than that of AFM-2.