The metal–organic framework UiO-66 with metal zirconium as the node has been synthesized using zirconium chloride and terephthalic acid. Anticancer drugs (CPT and DOX) and a photosensitizer (RB) were encapsulated via a post-loading method, and then the surface was modified with NH₂-PEG-FA to form RB-Drug@UiO-66-FA. The introduction of folic acid (FA) increased the stability and biocompatibility of the nanomaterials. Through X-ray diffraction and zeta potential analysis, we confirm that the modified material maintains its original structure and can effectively encapsulate the drug. By testing its performance, we showed that the drugs were released at high levels in the acidic environment where cancer cells survive. After 552 nm laser irradiation, a large amount of ¹O₂ was produced, promoting apoptosis. These results indicated that the materials demonstrate a good, combined effect of chemotherapy and photodynamic therapy.