FOX-7在DMSO-H_2O二元混合体系中的结晶研究  

Crystallization of FOX-7 in DMSO-H_2O Binary Mixed System

作　　者：刘璐 刘才林[1] 杨海君[1] 郝世龙[2] 周小清[2] 李洪珍[2] LIU Lu;LIU Cai-lin;YANG Hai-jun;HAO Shi-long;ZHOU Xiao-qing;LI Hong-zhen(School of Material Science and Engineering,Southwest University of Science and Technology,Mianyang 621010,China;Institute of Chernical Materials,CAEP,Mianyang 621999,China)

机构地区：[1]西南科技大学材料科学与工程学院,四川绵阳621010 [2]中国工程物理研究院化工材料研究所,四川绵阳621999

出　　处：《含能材料》2018年第8期638-644,共7页Chinese Journal of Energetic Materials

基　　金：国家自然科学基金资助(11302199)

摘　　要：为获得不同结晶条件对1,1‐二氨基‐2,2‐二硝基乙烯(FOX‐7)晶体质量和形貌的影响规律,实现对其晶体形态的控制,使用Crystal SCAN多通道结晶仪,采用浊度法测定了20~95℃,FOX‐7在二甲基亚砜(DMSO)、水(H_2O)及其二元混合溶剂中的溶解度以及在DMSO/H_2O=2∶1(体积比)混合溶剂中的介稳区宽度。采用降温法研究了FOX‐7在多种结晶条件下的晶体形态,并测试了晶体的机械感度和热性能。结果表明,FOX‐7的溶解度随着温度的升高和二元混合溶剂中DMSO含量的增加而增加;介稳区宽度随着温度的升高、降温速率的减小和搅拌速率的增大而变窄。降温结晶过程中,FOX‐7的晶体形态显著受溶剂比例、结晶起始温度和降温速率的影响,在50~80℃,降温速率不低于2℃·min^(-1)的条件下,可得到长径比几乎相同、形貌规则的立方块状高品质FOX‐7晶体,并且粒径在20~150μm内可控。同时,FOX‐7的晶体质量越好,晶体颗粒密度越大,热分解温度越高;FOX‐7的撞击感度都较低,且受颗粒形貌影响小,但摩擦感度受颗粒形貌影响较大,其中长柱状晶体的摩擦感度最小,片状晶体的最大。To obtain the influence rule of different crystallization conditions on the quality and morphology of 1,1‐diamino‐2,2‐dinitroethylene（FOX‐7）crystals and realize the control of its crystal morphology,the solubility of FOX‐7 in dimethyl sulfox‐ide（DMSO）,water（H2O）and its binary mixed solvent in the range of 20-95 ℃ and the metastable zone width of binary sol‐vent mixtures DMSO/H2O=2∶1（in volume ratio）were measured by turbidimetric method using a Crystal SCAN multi‐channel crystallizer. The crystal morphology of FOX‐7 under various crystallization conditions was investigated by cooling method,and the mechanical sensitivity and thermal performance of FOX‐7 were tested. Results show that the solubility of FOX‐7 increases with the increase of temperature and DMSO content in binary mixed solvent. The width of metastable zone becomes narrower with the increase of temperature,decrease of cooling rate and increase of stirring rate. In the process of cooling crystallization,the crystal morphology of FOX‐7 is significantly affected by solvent ratio,starting temperature and cooling rate of crystallization. In the range of 50-80 ℃,at the cooling rate of higher than 2 ℃·min^-1,the cube‐like high‐quality FOX‐7 crystal with almost the same aspect ratio and regular morphology can be obtained,and particle size is controllable in the range of 20-150 μm. At the same time,the better crystal quality of FOX‐7,the higher crystal density and the higher thermal decomposition temperature. The impact sensitivity of FOX‐7 is lower and small affected by the crystal morphology,but the friction sensitivity is greatly affected by parti‐cle morphology,the frictional sensitivity value of columnar‐like crystals is the smallest and that of plate‐like crystals is the largest.

关 键 词：炸药 1 1‐二氨基‐2 2‐二硝基乙烯(FOX‐7) 结晶 二甲基亚砜(DMSO) 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O64[理学—物理化学]