Trichlorotrinitrobenzene(TCTNB) with purity of 89% was dissolved in 1，2-dichloroethane at 45 ℃. The obtained solution was quenched to precipitate the solid. Filtrating and drying at 80 ℃ for 16 h gave TCTNB with purity of 99.2%. The crystal structure of TCTNB was determined with X-ray diffraction.