In a 500 mL four-necked flask equipped with an electric stirrer and a condenser tube, the solvent chlorobenzene, 174 g (2 mol) morpholine and 0.348 g 5% aqueous dodecyldimethylbenzylammonium hydroxide were added sequentially, and 81.08 g (1 mol) of 37% formaldehyde solution was slowly put into the four-necked flask under an ice-water bath, and the temperature was not exceeded at 70 during the feeding process, and the temperature was kept at 70 for 3 hrs after finishing feeding. It was held for 3 hours, then cooled to room temperature and distilled under reduced pressure to remove the solvent chlorobenzene and water to obtain the target product N,N'-methylenebismorpholine 189.23 g in 98.01% yield.