The invention relates to a preparation method of a volatile organic compound adsorbing material, and belongs to the technical field of adsorbents. The preparation method comprises the following steps: taking a fiber-based material as a raw material, carrying out activating treatment through an oxidizing agent, loading an adsorptive active substance on the fiber-based material through a cross-linking reaction, preparing to obtain an adsorbing material crude product, washing the crude product with ethyl alcohol and distilled water repeatedly, removing unreacted substances, and drying to obtain the pure product volatile organic compound adsorbing material. The preparation method is simple, mild in reaction conditions and good in operability, the obtained adsorbing material can adsorb volatile organic compound compositions such as ethyl alcohol, acetone and ethyl acetate in gas can be adsorbed by the obtained adsorbing material, the adsorption capacity is high, the adsorbing material after adsorption can be regenerated through desorption at a high temperature or after saturated steam heating and is repeatedly used more than five times, and the change rate of saturated adsorption capacity is within 10%.