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(1) Background: Iron tetrasulfophthalocyanine with a large nonlinear optical coefficient, good stability, and high catalytic activity has aroused the attention of researchers in the field of photo-Fenton reaction. Further improvement of the visible light photo-Fenton catalytic activity under circumneutral pH conditions for their practical application is still of great importance. (2) Methods: In this paper, iron tetrasulfophthalocyanine (FePcS) and phosphomolybdic acid (PMA) cointercalated layered double hydroxides (LDH) were synthesized by the ion-exchange method. All samples were fully characterized by various techniques and the results showed that FePcS and PMA were successfully intercalated in layered double hydroxides and the resulted compound exhibited strong absorption in the visible light region. The cointercalation compound was tested as a heterogeneous catalyst for the visible light photo-Fenton degradation of bisphenol A (BPA) at circumneutral pH. (3) Results: The results showed that the degradation and total organic carbon removal efficiencies of bisphenol A were 100% and 69.2%, respectively. (4) Conclusions: The cyclic voltammetry and electrochemical impedance spectroscopy measurements demonstrated that the main contribution of PMA to the enhanced photo-Fenton activity of FePcS-PMA-LDH comes from the acceleration of electron transfer in the reaction system. Additionally, the possible reaction mechanism in the photo-Fenton system catalyzed by FePcS-PMA-LDH was also proposed.

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Synthesis of FePcS–PMA–LDH Cointercalation Composite with Enhanced Visible Light Photo-Fenton Catalytic Activity for BPA Degradation at Circumneutral pH