Synthesis, Characterization And Performance Of 2,6-Bis(Picrylamino)-3,5-Dinitropyridine

In this thesis,2,6-bis(picrylamino)-3,5-dinitropyridine(PYX) was synthesised and refined product was prepared by recrystallization.The effects of solvents on particle size was investigated,The single crystal of PYX was analysized.An improvement synthetic route for the total synthesis of PYX was introduced from 4-nitrochlorobenzene and 2,6-diaminopyridine.It mainly discussed the influence of each reaction step of the main factors combining with the reaction mechanism,Optimizing each factor of unit reactions, reaction condition was obtained and the total yield reached 52.59%.The experimental results show that the PYX sample prepared by recrystallization from NMP is perfect.At the same time,the thermal analysis and thermal decomposition kinetics calculation indicated that the temperature of the exothermic peaks of PYX(NMP) is 368.33℃at 10℃·min-1 heating rate, and its activation energy is 169.88kJ·mol-1.SEM results show that those particles which were cuboid structures were all uniform distribution,bright and clean.Refined products of PYX which are diminished respectively with DMSO, DMF, NMP are obtained from crude PYX.The results shows that PYX has the smallest average size 5.206μm at the condition of using NMP as solvent and water as nonsolvent, SEM results show that those particles which are cuboid structures are smooth,spotless and light.Single crystal of PYX was characterized by X-ray diffraction analysis.The single crystal of PYX belongs to monoclinic,space group P21/c with cell parameter a=1.3796(3)n-m,b=1.7130(3)nm,c=1.5313(3)nm,α=90.00°,β=98.73(3)°,γ=90.00°,Mr=819.60,V=3.5769(1)n m3,Z=4,Dc=1.522mg/m3,F(000)=1688,μ=0.130mm-1,R=0.1421.wR=0.1968.The planes of two benzene rings were parallel to each other which confirmed by the mathematical calculation and were both formed 64.33°with the plane of pyridine ring.