Abstract: Crown ether dibenzo-18-crown-6 (DBC) was chloromethylated using 1,4-bis(chloromethoxy)butane (BCMB) as chloromethylation reagent. DBC was transferred into chloromethylated crown ether CMDBC. The nucleophilic substitution between chloromethyl groups of CMDBC and the hydroxyl groups of crosslinked polyvinyl alcohol (CPVA) microspheres was carried out, and immobilization of DBC on CPVA microspheres was realized, resulting in functional microspheres DBC-CPVA. Based on seting up the method to determine the immobilization amount of DBC, bromothymol blue-solid extraction method, effects of main factors on the immobilization reaction were mainly investigated. Results show that the reaction temperature and solvent polarity affect the immobilization reaction greatly, and the microspheres DBC-CPVA with a DBC immobilization amount of 1.72 mmol/g can be obtained at 70 ℃ and in DFM solvent with stronger polarity.