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The trans-resveratrol (RSV)-loaded silica aerogel (RLSA) was prepared by the sol-gel method, adding the drug during the aging process, solvent replacement and freeze drying. A series of characterizations showed that RSV stays in the silica aerogel in two ways. First, RSV precipitates due to minimal solubility in water during the solvent replacement process. After freeze drying, the solvent evaporates and the RSV recrystallizes. It can be seen from scanning electron microscope (SEM) and transmission electron microscope (TEM) images that the recrystallized RSV with micron-sized long rod-shaped is integrated with the dense silica network skeleton. Second, from small-angle X-ray scattering (SAXS) results, a portion of the RSV molecules is not crystallized and the size is extremely small. This can be attached to the primary and secondary particles of silica to enhance its network structure and inhibit shrinkage, which is why the volume and pore size of RLSA is larger. In addition, the diffusion of RSV in silica alcogel was studied by a one-dimensional model. The apparent diffusion coefficients of inward diffusion, outward diffusion and internal diffusion were calculated by fitting the time- and position-dependent concentration data. It was found that the outward diffusion coefficient (5.25 × 10−10 m2/s) is larger than the inward (2.93 × 10−10 m2/s), which is probably due to the interface effect. The diffusion coefficients obtained for different concentrations in the same process (inward diffusion) are found to be different. This suggests that the apparent diffusion coefficient obtained is affected by molecular adsorption.