The invention provides a hyper-crosslinked resin and its application in adsorption separation of 5-hydroxymethylfurfural. A preparation method for the hyper-cross-linked resin comprises the following steps: S1, mixing an ester monomer, a cross-linking agent, an initiator and a pore forming agent, adding the formed mixture into an aqueous phase containing a dispersing agent, and performing suspension polymerization to obtain precursor resin; and S2, adding a swelling agent and a Lewis acid catalyst into the precursor resin, and performing a post-crosslinking reaction of a suspended double bond to obtain post-crosslinked resin, wherein the ester monomer is one or more selected from the group consisting of ethyl acrylate, butyl acrylate, triethylene glycol dimethacrylate, ethylene glycol dimethacrylate, ethylene glycol diacrylate, methyl methacrylate , glycidyl methacrylate and hydroxyethyl acrylate. The hyper-crosslinked resin provided by the invention has a BET specific surface area of 400 to 1200 m<2>/g, a pore volume of 0.1 to 2.5 cm<3>/g, and an average pore size of 1 to 20 nm.