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• TiO 2 /diatomite calcined at 550 °C exhibited enhanced VOC degradation efficiency. • Optimal degradation conditions are RH = 0%, flow rate = 1 L/min, and VOC = 10 ppm. • VOC has a high value degradation rate when the composite dosage was 3.76 mg/cm2. • Key parameters had obvious impact on the VOC adsorption and degradation. The TiO 2 /diatomite composites with excellent adsorption and photo-degradation performances were leveraged to investigate the influences of calcination temperature and operating factors on their properties. The results showed that the calcination temperature was closely bound up with the crystallization of TiO 2 and the specific surface area of composite. The composite with calcination temperature of 550 °C exhibited enhanced photocatalytic owing to the high surface area and small TiO 2 crystallite size. A series of dynamic degradation experiments were conducted to investigate the effect of various operating parameters on acetone and p -xylene adsorption/degradation performances of the composite. The results illustrated that when the relative humidity (0–70%), gas flow rate (1–4 L/min), and VOC concentration (10–40 ppm) were set as the low values, the high total organic carbon degradation rate could be acquired. The total organic carbon degradation rate reached to a high value when the composite dosage was 3.76 mg/cm2. With the increase of light intensity (0.48–1.33 mW/cm2), the total organic carbon degradation rate presented an upward trend and then kept stable. The absorbent-photocatalyst hybrid TiO 2 /diatomite composite could be the promising VOC purification materials. [ABSTRACT FROM AUTHOR]