微反应器合成1,2,4-丁三醇三硝酸酯的工艺研究  

Synthesis processes of 1,2,4-butanetriol trinitrate in microreactor

作　　者：毛明珍[1] 王伦[1] 张晓光[1] 张媛媛[1] 卫天琪 张建功[1] 王月梅[1] 张选利 郭旺军[1] MAO Ming-zhen;WANG Lun;ZHANG Xiao-guang;ZHANG Yuan-yuan;WEI Tian-qi;ZHANG Jian-gong;WANG Yue-mei;ZHANG Xuan-li;GUO Wang-jun(Xi’an Modern Chemistry Research Institute,State Key Laboratory of Fluorine&Nitrogen Chemicals,Xi’an 710065,China)

机构地区：[1]西安近代化学研究所氟氮化工资源高效开发与利用国家重点实验室,陕西西安710065

出　　处：《应用化工》2022年第1期73-75,共3页Applied Chemical Industry

基　　金：国家自然科学青年基金(21702159)。

摘　　要：以1,2,4-丁三醇(BT)水溶液为起始原料,发烟硝酸/浓硫酸为硝化剂,采用微反应器连续合成1,2,4-丁三醇三硝酸酯,考察反应温度、物料及混酸比例、停留时间对反应影响。结果表明,优化工艺参数为:1,2,4-丁三醇∶发烟硝酸∶浓硫酸的摩尔比为1∶5∶4,反应温度15℃,停留时间48 s,工艺收率90.5%,产品含量98.8%。与传统间歇釜式合成工艺相比,该工艺实现了1,2,4-丁三醇三硝酸酯合成反应的稳定进行,反应温度接近室温,消除了过程反应热的积累和温度波动,缩短反应时间。1,2,4-Butanetriol(BT) as raw materials and nitric acid(HNO;)/sulphuric acid(H;SO;) as a nitrating agent.The influences of the ratio of two materials, reaction temperature and residence time on the yield of BTTN were investigated.The result showed that the optimized process conditions are as follows: molar ratio of BT∶HNO;∶H;SO;is 1∶5∶4,the reaction temperature of 15 ℃,the residence time of 48 s, the yield of process is 90.5% and the purity of BTTN is 98.8%.The new process could make the BTTN synthesis reaction stable and eliminate the accumulation of reaction heat and temperature fluctuations.Furthermore, shorten the reaction time.

关 键 词：1 2 4-丁三醇三硝酸酯 微反应器 连续流 合成 

分 类 号：TQ56[化学工程—炸药化工] O69[理学—化学]