|本期目录/Table of Contents|

[1]汪营磊,刘卫孝,汪伟,等.微反应技术合成不敏感硝酸酯增塑剂TMETN和PGDN[J].火炸药学报,2018,41(4):359-362,368.[doi:10.14077/j.issn.1007-7812.2018.04.007]
 WANG Ying-lei,LIU Wei-xiao,WANG Wei,et al.Synthesis of Insensitive Nitrate Plasticizers TMETN and PGDN by Micro Reaction Technology[J].,2018,41(4):359-362,368.[doi:10.14077/j.issn.1007-7812.2018.04.007]
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微反应技术合成不敏感硝酸酯增塑剂TMETN和PGDN()
     
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《火炸药学报》[ISSN:1007-7812/CN:61-1310/TJ]

卷:
41卷
期数:
2018年第4期
页码:
359-362,368
栏目:
出版日期:
2018-08-23

文章信息/Info

Title:
Synthesis of Insensitive Nitrate Plasticizers TMETN and PGDN by Micro Reaction Technology
作者:
汪营磊 刘卫孝 汪伟 朱勇 李斌栋 陈斌 丁峰 姬月萍
1. 西安近代化学研究所, 陕西 西安 710065;
2. 南京理工大学, 江苏 南京 210094
Author(s):
WANG Ying-lei LIU Wei-xiao WANG Wei ZHU Yong LI Bin-dong CHEN Bin DING Feng JI Yue-ping
1. Xi’an Modern Chemistry Research Institute, Xi’an 710065, China;
2. Nanjing University of Science and Technology, Nanjing 210094, China
关键词:
微反应器硝化12-丙二醇二硝酸酯(PGDN)三羟甲基乙烷三硝酸酯(TMETN)增塑剂
Keywords:
micro reactornitration12-propylene glycol dinitrate(PGDN)trimethylolethane trinitrate(TMETN)plasticizer
分类号:
TJ55;TQ22
DOI:
10.14077/j.issn.1007-7812.2018.04.007
文献标志码:
-
摘要:
利用微反应技术,分别以1,2-丙二醇、三羟甲基乙烷为原料,硝硫混酸为硝化剂,合成了1,2-丙二醇二硝酸酯(PGDN)和三羟甲基乙烷三硝酸酯(TMETN);采用红外光谱、核磁共振等对其结构进行了表征,同时优化了微反应器硝化反应条件。结果表明,TMETN和PGDN结构与间歇式合成产物一致,合成TMETN的较佳硝化温度为17~20℃,硝酸与三羟甲基乙烷的最佳摩尔比为5.6∶1.0,收率达90.0%以上,纯度达98.5%;合成PGDN的较佳反应温度为20~22℃,硝酸与1,2-丙二醇的摩尔比为2.7∶1.0。该工艺具有反应温度范围宽、硝酸用量少和收率高等优点。
Abstract:
Trimethylethane trinitrate (TMETN) and 1, 2-propylene glycol dinitrate (PGDN) were synthesized by micro reaction technology, using 1, 2-propylene glycol and trimethylethane as raw materials and nitric acid/sulphuric acid as nitrating agent respectively. Their structures were characterized by FTIR and NMR etc. and nitration reaction conditions of micro reactor were optimized through the micro reactor method developed in this study. The results show that their structures were consistent with those from intermittent synthesis product. The better nitration temperature of TMETN is 17-20℃, and the optimum molar ratio of HNO3 and trimethylethane is 5.6:1.0. The yield is over 90.0%. The purity is 98.5%. The better reaction temperature of synthesizing PGDN is 20-22℃, and the molar ratio of HNO3 to 1, 2-propylene glycol is 2.7:1.0. The process has the advantages of wide reaction temperature range, low nitric acid dosage and high yield,etc.

参考文献/References:

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备注/Memo

备注/Memo:
收稿日期:2018-04-09;改回日期:2018-06-24。
基金项目:国家自然科学基金(No.21173163)
作者简介:汪营磊(1983-),男,博士,副研究员,从事含能材料合成及性能研究。E-mail:wangyl204@163.com
通讯作者:汪伟(1978-),男,研究员,从事含能材料合成及性能研究。E-mail:jdhxww@163.com
更新日期/Last Update: 1900-01-01