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The invention discloses a preparation process of a Ti-MOF / BiOF composite material, and relates to the field of photocatalysis of nano materials. The preparation method comprises the following steps: putting N, N-dimethylformamide (DMF), methanol, terephthalic acid and tetrabutyl titanate (TBOT) into a reactor lined with polytetrafluoroethylene, keeping the temperature of 150 DEG C for 24 hours, collecting, washing, drying and activating to obtain Ti-MOF. The preparation method comprises the following steps: respectively dissolving bismuth nitrate and NaF in ethylene glycol and water, carrying out ultrasonic dissolution, and then adding a proper amount of Ti-MOF into the bismuth nitrate solution; under stirring, dropwise adding the NaF solution into the bismuth nitrate solution, transferring the mixed solution into a reaction kettle for reaction, cooling, cleaning and drying to obtain the Ti-MOF / BiOF composite material. The material has good adsorption performance and photocatalytic performance, and can efficiently degrade novel perfluorinated / polyfluorinated compounds in water under simulated sunlight.