The chloromethylation research of highly crosslinking degree non-polarity macroporous absorption resin D101 was performed by using self-made 1, 4-bis(chloromethoxyl)butane(BCMB), as the chloromethylation reagent and adopting anhydrous zinc chloride (ZnCl2) catalyst. The optimal conditions at 50 ℃ for 14 h in Lewis acid (ZnCl2) catalyst for chloromethylation of resin were found as follows：m(D101) : m(BCMB) : m(CCl4)=1 : 4 : 18.6, swelling time 12 h, the chlorine content of resin was 4％, providing experimental basis for resin modification, functionality and further studying adsorption separation research.