The invention provides a preparation method of amino acid loading super-cross-linked alkenyl benzene compound and quaternary ammonium hydroxide copolymerization microspheres. The preparation method comprises: preparing alkenyl benzene compound and quaternary ammonium hydroxide copolymerization microspheres, preparing super-cross-linked alkenyl benzene compound and quaternary ammonium hydroxide copolymerization microspheres, and preparing amino acid loading super-cross-linked alkenyl benzene compound and quaternary ammonium hydroxide copolymerization microspheres. According to the present invention, the prepared surface modified amino acid salt has low volatility (determined by ionic properties) and high surface tension, can maintain high stability in the presence of oxides, and has high chemical reactivity; and with the preparation method, the advantages of high adsorption efficiency, recycling, economy, environmental protection, low energy consumption, simple and easy-operation equipment and commercial application are provided.