The Synthesis Research Of Hexachlorocyclotriphosphazene And Its Energetic Derivatives

Cyclophosphazene is a kind of inorganic compound which nitrogen andphosphorus alternatively array in single and multiple bonds as the backbond. It is animportant chemical intermediate that rolled stability and reactivity into one. Thesynthesis research of cyclophosphazene energetic derivatives is a new researchdirection in the field of energetic materials research.This thesis takes PCl5 and NH4Cl as the raw materials, establishes on traditionalsynthesis method and synthesizes the most representative hexa-chlorocyclotriphosphazenein cyclophosphazenes by improving synthesis technology andadopting the new synthesis system of using mixed catalyst and acid binding agent.Hexachlorocyclotriphosphazene's ethylenediamine substitution reaction gains1,1-ethylenediamine-3,3,5,5-tetrachloro-cyclotrip-hosphazene, which lay thefoundation for amido nitration and realizing cyclophosphazene's side chain havingN-NO2. The product of ethylenediamine substitution and sodium azide undergo azidereaction in acetone solvent,obtained 1,1-(N,N-ethylenedinitramino)-3,3,5,5-tetraazidocyclotriphosphazen with the performance of explosion.Through experimental research,educes the main conclusions as follows:1.The synthesis system of using mixed catalyst and acid binding agent using forsynthesizing hexachlorocyclotriphosphazene has simple operation, short reaction timeand so on. Through experimental study, the optimal experimental conditions are:utilization of monochlorobenzene as the reaction solvent, anhydrous magnesiumchloride, anhydrous zinc chloride and pyridine as mixed catalyst,pyridine as the acidbinding agent, pyridine:phosphorus pentachloride(mass ratio):1.15:1, PCl5: NH4Cl( molar ratio): 1: 1.1, 2 hours of reaction time. Yield is 83.6%.2.the optimum conditions for ethylenediamino experiment are: Using ether as a reaction solvent, The reaction temperature is 8-9℃, the reaction time is 7 hours afterfeeding, ethylenediamine dropping to 3ml/min, and the molar ratio ofhexachlorocyclo-triphosphazene and ethylenediamine is 1:2.1.3.The optimum experimental conditions of azido reaction are: the reactiontemperature is 23-24℃, the reaction time is 22 hours, sodium azide refined bygrinding and ultrasonic treatment, and the molar ratio of 1,1-ethylenediamine-3,3,5,5-tetrachloro-cyclotriphosphazene and sodium azide is 1:5.4.Discusses the experimental reaction mechanism, uses the means of infraredspectrum,and melting point determination to characterize the experimental products.This dissertation does the pilot work for the synthesis of cyclophosphazeneenergetic materials, and lay the foundation for synthesis of green primary explosive1,1-(N,N-ethylenedinitramino)-3,3,5,5-tetraazidocyclotriphosphazene,which issignificant.