摘要
为了明确奥克托今(HMX)合成过程中料比的复杂交互作用,并提高HMX含量,采用响应面法考察HMX合成过程中料比的复杂交互作用,建立以原料硝酸(NA)、硝酸铵(AN)、醋酸(AcOH)、醋酐(Ac_(2)O)配比为输入变量,以HMX含量为响应值的多元回归模型,确定了各因素对HMX含量影响的主次,并且基于不同HMX含量对应的原料配比结合加料工艺及反应时间进行工艺优化研究。结果表明,得到的最优工艺为:原料配比(摩尔比)为:HA∶NA∶AN∶Ac_(2)O∶AcOH=1.00∶5.00∶3.50∶8.00∶17.50;底液中添加醋酐Ac_(2)O与AcOH摩尔比1∶54、一段加料中Ac_(2)O与HA摩尔比4∶1、一段反应时间30min、二段反应时间60min、三段反应时间45min、热解时间30min,产品得率为81.82%,HMX质量分数为91.56%。优化后工艺使醋酐用量减少了20%,产物产率提高了6%,HMX质量分数提高了4%左右。
To clarify the complex interactions of the feed ratio in the synthesis process of Octogen(HMX)and increase the content of HMX,the response surface methodology(RSM)was employed to investigate the intricate interactions.A multiple regression model was established using the ratio of raw materials(nitric acid,ammonium nitrate,acetic acid,acetic anhydride)as input variables and the content of HMX as the response variable.The effects of each factor on the content of HMX was determined,and the process optimization was carried out based on the raw material ratios corresponding to different HMX contents,feeding process,and reaction time.The optimal conditions are as following:the raw material ratio(molar ratio)is HA∶NA∶AN∶Ac_(2)O∶AcOH=1.00∶5.00∶3.50∶8.00∶17.50,the acetic anhydride is added to the bottom solution at a ratio of n(Ac_(2)O)∶n(AcOH)=1∶54,and in the first feed at a ratio of n(Ac_(2)O)∶n(HA)=4∶1.Reaction time are set as following:first stage of 30[KG-*9]min,second stage of 60[KG-*9]min,third stage of 45[KG-*9]min,and pyrolysis time of 30[KG-*9]min.Under the optimized conditions,the product yield reaches to 81.82%with the HMX content of 91.56%.Compared with the original process,the amount of acetic anhydride is reduced by 20%,the product yield is increased by 6%,and the content of HMX is improved by approximately 4%.
作者
郜兴宇
朱泰胜
王晓洋
王小军
徐子帅
李子扬
刘永政
赵林秀
李永祥
GAO Xing-yu;ZHU Tai-sheng;WANG Xiao-yang;WANG Xiao-jun;XU Zi-shuai;LI Zi-yang;LIU Yong-zheng;ZHAO Lin-xiu;LI Yong-xiang(School of Chemistry and Chemical Engineering,North University of China,Taiyuan 030051,China;Gansu Yinguang Chemical Industry Group Co.,Ltd.,Baiyin Gansu 730900,China)
出处
《火炸药学报》
北大核心
2025年第7期609-616,I0001,共9页
Chinese Journal of Explosives & Propellants
关键词
有机化学
奥克托今
HMX
醋酐法
工艺优化
响应面法
organic chemistry
Octogen
HMX
acetic anhydride method
process optimization
response surface method