A new compound (CHZ)(HTNPG)·0.5H2O was synthesized by mixing carbohydrazide(CHZ) and trinitrophloroglucinol(TNPG) and characterized by elemental analysis and Fourier transform infrared (FTIR) spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system, Pī space group, with a=0.45578(9) nm, b=1.0142(2) nm, c=1.3041(3) nm, α=86.53(3)°, β=99.56(3)°, γ=81.94(3)°, V= 0.5958(2) nm3, Z=2, Dc=2.008 g/cm3, R1=0.0476, and wR2=0.1139. The compound is a di-substituted salt of TNPG, which consists of a cation (CHZ)2+ and an anion (HTNPG)2–. The thermal analysis of the compound was studied by means of differential scanning calorimetry(DSC) and thermogravimetry-derivative thermogravimetry(TG-DTG). Under nitrogen atmosphere at a heating rate of 10 °C/min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature range of 140―232 °C on the DSC trace. The decomposition products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between (CHZ)2+ and (HTNPG)2– enhance the thermal stability of the title compound. A new compound (CHZ) (HTNPG) · 0.5H2O was synthesized by mixing carbohydrazide (CHZ) and trinitrophloroglucinol (TNPG) and characterized by elemental analysis and Fourier transform infrared (FTIR) spectrum. Its crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to triclinic system with a = 0.45578 (9) nm, b = 1.0142 (2) nm, c = 1.3041 (3) °, γ = 81.94 (3) °, V = 0.5958 (2) nm3, Z = 2, Dc = 2.008 g / cm3, R1 = 0.0476, and wR2 = 0.1139. TNPG, which consists of a cation (CHZ) 2+ and an anion (HTNPG) 2-. The thermal analysis of the compound was studied by means of differential scanning calorimetry (DSC) and thermogravimetry-derivative thermogravimetry nitrogen atmosphere at a heating rate of 10 ° C / min, the thermal decomposition of the compound contained one endothermic process of dehydrating stage and two intense exothermic decomposition processes in a temperature r ange of 140-232 ° C on the DSC trace. The existing products of the title compound are nearly gaseous products. The existing complicated hydrogen bond networks and electrostatic attraction between (CHZ) 2+ and (HTNPG) 2- enhance the thermal stability of the title compound.