六硝基六氮杂异伍兹烷在硝酸中的转晶

采用硝酸含水体系将α、γ-HNIW晶体转晶成-εHNIW晶体;用在线粒度仪实时监测HNIW晶体成核、生长的动力学过程;研究了降温、不溶溶剂水的加入、晶种的加入对ε-HNIW晶体析出的影响;用FTIR、SEM、激光粒度仪对转晶得到的样品进行了晶型、形貌及粒度分布的表征。结果表明:在温度低于64℃、有ε-HNIW晶种存在的条件下,通过降温和加入不溶溶剂水,可以转晶得到ε-HNIW晶体,得率98%。

Re-crystallization of Hexanitrohexaazaisowurtzitane in Nitric Acid with FBRM

High energy density compound hexanitrohexaazaisowurtzitane(HNIW) has several polymorphs,among which ε-HNIW with highest density is practically applied.Usually,α-HNIW and γ-HNIW crystals are obtained after the intermediate is nitrified in the synthesis of HNIW.The α-HNIW and γ-HNIW crystals were re-crystallized by lowering the temperature of the solution and adding anti-solvent water to the solution after they had been dissolved completely.FBRM(focused beam reflectance measurement) was used to monitor the process of re-crystallization,that could present the time of adding crystal seeds and record the kinetics process of nucleation and growth of crystals.The samples were characterized by FTIR,SEM and laser diffraction particle size measurement.The result shows that in the presence of crystal seeds,by lowering the temperature below 64 ℃ and adding anti-solvent water,ε-HNIW crystals are formed with recovery of 98% by weight,and the recovery by adding water is better than that by lowering the temperature.