The invention relates to a new carbon-based adsorption material and a preparation method thereof, mainly solving the problem that an adsorption recovery material is poor in hydrophobicity, low in capacity of adsorbing target organic matter molecules, severe in difficulty of vacuum desorption, and low in adsorption/desorption rate in a high-humidity environment. According to the preparation method, resorcinol or m-trihydroxybenzene and gracial acetate acid are taken as reaction raw materials, a formaldehyde aqueous solution is taken as a reaction solvent, and the high-specific-surface-area carbon-based adsorption material is prepared through a process of sol gel freeze drying and carbonization activation, so that the problem is well solved. The new carbon-based adsorption material can be used in engineering material technology.