Shell powder loaded with nano-zero valent iron (MS-NZVI/SP) was prepared by mangosteen shell extract and shell powder and was used to investigate the Fenton-like degradation effect of eriochrome black T. The prepared samples were characterized by SEM, XRD and FTIR. The results showed that MS-NZVI/SP was successfully prepared and displayed uniform spherical particles. The surface of MS-NZVI/SP was covered with organic polyphenols. Furthermore, it had good stability and reusability. The degradation performance of eriochrome black T on MS-NZVI/SP was optimized by single factor experiments. The optimized conditions were as follows: loading mass ratio of shell powder to nano zero-valent iron of 1∶1, temperature of 35 ℃, pH of solution of 3, hydrogen peroxide dosage of 4 mL, synthetic material of 100 mg. Under these conditions, the degradation efficiency of eriochrome black T could reach 93.01%. The degradation process of eriochrome black T conformed to the quasi-secondary kinetic model.