The famous heat-resistant explosive-2,2',2'',4,4',4'',6,6',6''-nonanitro-1,1':3',1''-terphenyl (NONA) was synthesized by the Ullmann reaction, and its separation and purification was achieved by the solvent-antisolvent method and the anisole reflux method, which are more simple and easy to operate than conventional methods. The molecular structure of NONA was characterized by X-ray single crystal diffraction, FT-IR, H-1 NMR, mass spectrometry and elemental analysis. The thermal behavior of NONA was studied by thermogravimetric-differential scanning calorimetry (TG-DSC), Moreover, the heats of formation, detonation properties, and bond dissociation of NONA were calculated. The results show that the NONA crystals belong to the orthorhombic system and the Pbca (61) space group where a=16.8223 (11) angstrom, b=11.9573 angstrom, c=23.0972 (14) angstrom, a/b=1.4069, b/c=0.5177, c/a=1.3730, V=4645.99(50) angstrom(3), =1.81644g/cm(3), Z=8, and F(000)=2560. The decomposition temperature is 364.8 degrees C, the calculated heats of formation is -148.2kJ/mol, the detonation velocity and detonation pressure are 7720.66m/s and 26.58GPa, respectively, and the initiation bond is C(3)-NO2 with a dissociation energy of 249.3kJ/mol.