Abstract: This is an article in the field of ceramics and composites. Methylene blue is a typical pollutant industrial wastewater.It will bring great harm to the water body if it is discharged arbitrarily without treatment. We prepared a kind of attapulgite/nano iron composite (DDBAC/ATP/nZVI), that the attapulgite was roasted, organic modified and then loaded with nano iron (nZVI) by liquid-phase reduction. The optimum preparation process is obtained: attapulgite raw soil is calcined at 300 ℃ for 1.5 h, 20 mmol/100 g benzalkonium chloride(DDBAC)is added, then ultrasonic is used for 20 min, and then nano iron is loaded by liquid-phase reduction method. The ratio of iron to soil is 1:3, KBH₄ concentration is 0.25 mol/L and reaction time is 3 h. The XRD, FTRI, SEM, XPS, BET confirm that DDBAC and nano iron are successfully loaded on the surface of attapulgite. The maximum removal of methylene blue by DDBAC/ATP/nZVI is 114.94 mg/g, and the application performance of the DDBAC/ATP/nZVI remains stable within 60 days.