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This invention discloses a method for preparing an amphiphilic photocatalyst using carbon nitride-supported metal oxides and its application in the aqueous-phase benzene hydroxylation reaction. This catalyst not only retains the unique amphiphilicity of carbon nitride, improving the interfacial contact and mass transfer process between the water / benzene phases and promoting the rapid and efficient transfer of •OH generated in the aqueous phase to benzene to participate in the reaction, but also forms a good interfacial contact between the metal oxide and carbon nitride phases during molten salt heat treatment. Under illumination, photogenerated electrons can efficiently migrate from carbon nitride to the surface of the metal oxide, driving the rapid photo-Fenton reaction. Therefore, this catalyst exhibits excellent catalytic performance in the photocatalytic aqueous-phase benzene hydroxylation reaction to prepare phenol. This invention does not require the addition of additional organic solvents and can achieve a highly efficient benzene hydroxylation reaction in a pure aqueous phase, conforming to the concept of green chemistry and showing good prospects for industrial application.