The change in current in the solution was detected with high sensitivity by applying an electrochemical methodology that showed the hydrolysis of PBSs.

Hydrogen peroxide (H2O2) is considered one of the most important chemical products and has a promising future in photocatalytic preparation, which is green, pollution‐free, and hardly consumes any non‐renewable energy. This study involves the preparation of benzoxazine with Si─O bonds via the Mannich reaction, followed by co‐hydrolysis to produce photocatalysts containing benzoxazine with Si─O─Ti bonds. In this study, a benzoxazine photocatalyst with Si─O─Ti bonds is synthesized and characterized using fourier transform infrared spectroscopy, nuclear magnetic resonance, and X‐ray photoelectron spectroscopy. The size and elemental distribution of the nanoparticles are confirmed by transmission electron microscopy and scanning electron microscopy. The photocatalytic synthesis of H2O2 is tested using the titanium salt detection method, and the rate is found to be 7.28 µmol h−1. Additionally, the catalyst exhibits good hydrolysis resistance and could be reused multiple times. The use of benzoxazine with Si─O─Ti bonds presents a promising experimental and theoretical foundation for the industrial production of H2O2 through photocatalytic synthesis.