In China, safe disposal of hazardous waste is more and more a necessity, urged by rapid economic development. The pyrolysis and combustion characteristics of a residue from producing monopotassium phosphate (monopotassium phosphate residue), considered as a hazardous waste, were studied using a thermogravimetric, coupled with Fourier transform infrared analyzer (TG-FTIR). Both pyrolysis and combustion runs can be subdivided into three stages: drying, thermal decomposition, and final devolatilization. The average weight loss rate during fast thermal decomposition stage in pyrolysis is higher than combustion. Acetic acid, methane, pentane, (acetyl) cyclopropane, 2,4,6-trichlorophenol, CO, and CO 2 were distinguished in the pyrolysis process, while CO 2 was the dominant combustion product.