BACKGROUNDLevulinic acid (LA) is an important biomass‐platform compound. The preparation of LA from biomass will inevitably produce many by‐products. However, there are few investigations focused on the separation and purification of LA from biomass hydrolysate. This study designed a series of hyper‐cross‐linked resins to adsorb LA from sugarcane bagasse hydrolysate, investigated the adsorption behavior of LA onto resin in a fixed‐bed system and established a relevant model to depict the adsorption process, which can provide reference for LA separation.RESULTSThe hyper‐cross‐linked resin G10PTEPA synthesized by poly(styrene‐divinylbenzene‐glycidyl methacrylate) resin G10 with the Friedel–Crafts reaction and amination reaction using tetraethylenepentamine (TEPA) had the best adsorption performance. The adsorption capacity of LA onto G10PTEPA in the sugarcane bagasse hydrolysate was 95.02 mg g−1, which was improved by 37% compared with G10. The maximum efficiency of the fixed‐bed onto G10PTEPA was 86.01% at flow rate of 0.6 mL min−1, with bed volume of 14 mL, fixed‐bed diameter of 2 cm, and feed LA concentration of 19.0 g · L−1. After elution by ethanol, a five‐fold increase in the concentration of LA with a purity of 80% was achieved. The Thomas model and the Yoon–Nelson model fitted well (R2 > 0.99) to the fixed‐bed adsorption behavior of LA onto G10PTEPA and can give accurate predictions.CONCLUSIONThe resin G10PTEPA was the best‐performing adsorbent for LA adsorption. Larger fixed‐bed diameter, higher flow rate and higher inflow concentration were beneficial to increase the mass transfer driving force. This study provides a potential adsorbent and theoretical guidance for LA separation. © 2023 Society of Chemical Industry.