Synthesis Of Hexabenzylhexaazaisowurtzitane And Fundamental Research For Its Process Design

The development and research of energetic compounds is a hot topic in the field of energetic materials.Hexanitrohexaazaisowurtzitane has received wide attention as a high energy density compound with high energy content.The polyaza-isoindazide derivatives are intermediates for the preparation of hexanitrohexaazaisowurtzitane and play important role in various fields.Hexabenzylhexaazaisowurtzitane is the main synthetic precursor of the cage structure.The reaction condition,kinetic and system properties of the synthesis are important for the development of the reactor and the overall industrialization of the energetic materials.Synthesis of Hexabenzylhexaazaisowurtzitane and fundamental research for its process design were investigated in this paper.The main contents are as follows:(1)The main raw materials of the synthesis of hexabenzylhexaazaisowurtzitane are benzylamine and glyoxal.The hexabenzylhexaazaisowurtzitane is prepared by addition reaction,dehydration and condensation under the catalysis of acid.The effects of feed ratio,catalyst,reaction time and temperature,solvent type on the yield were investigated and the suitable reaction conditions were determined.The scaled-up experiments were carried out within a certain range,the product yield was stable at 81%.The purity of the crude product is 92%and the purity after purification is 98%,which satisfies the requirements of subsequent reaction.(2)The kinetic experiment was carried out with the reaction temperature of 15?35? in suitable reaction conditions.An apparent reaction kinetic model was established with the combination of reaction mechanism and actual reaction conditions,and the synthetic experimental data were fitted to obtain reaction kinetic parameters.Statistical test of the dynamic model was carried out.(3)The thermal conductivities and densities of benzylamine-acetonitrile-water system,being basic physical properties of fluids,are of great significance for the industrial development of its related reactions.The thermal conductivities and densities of benzylamine-water system,benzylamine-acetonitrile system,acetonitrile-water system,and benzylamine-acetonitrile-water system were measured in the range of 288.15?313.15K at atmospheric pressure,respectively,covering the hole concentration range.The experimental thermal conductivities and densities were correlated.(4)The stirred tank reactor of hexabenzylhexaazaisowurtzitane,for the pilot scale synthesis of the 1kg energetic compound,was designed,and the relevant assembly diagram of the reactor was given.