摘要
采用重结晶法纯化HNS-Ⅱ,用正交试验方法对实验工艺条件进行优化,研究了恒温回流反应温度、反应时间、溶液配比和洗涤溶剂等因素对产物纯度的影响。结果表明:恒温回流反应温度是最主要的影响因素,反应时间对产物纯度有一定影响,溶液配比和所选洗涤溶剂对纯度影响较小,提纯重结晶次数由原料纯度决定。优化提纯的工艺条件为:反应温度(160±2)℃,反应时间1.5h,溶液配比1∶7(g/mL),洗涤溶剂为100%甲醇,优化后产物纯度可达99.7%以上。
The purity of HNS- Ⅱ was increased by recrystallization. Orthogonal design method is used to analyze the optimal conditions of experiment technique. The effects of circumfluence reaction temperature, reaction time, solution scale and washing solvent on purity of production were investigated. The results indicate that the reaction temperature is main influence factor and reaction time has some impacts on HNS purity. However, solution scale and washing solvent have a little influence on it. The times of recrystallizafion was decided by material purity. Finally, the purity of HNS can over 99.7%, while the reaction temperature is （160±2） ℃, reaction fime is 1.5h, solution scale is 1 ： 7 （g/mL） and washing solvent isl00% methanol.
出处
《火工品》
CAS
CSCD
北大核心
2007年第4期13-16,共4页
Initiators & Pyrotechnics
关键词
六硝基
纯化
重结晶
正交设计
HNS
Purification
Recrystallizafion
Orthogonal design
