火炸药学报2023，Vol.46Issue(11)：965-970,6.DOI:10.14077/j.issn.1007-7812.202304016
水热法合成3-硝基吡唑的工艺优化
Process Optimization of the Preparation of 3-Nitropyrazole by Hydrothermal Method
仝志珂 1王明亚 1陈军 2侯璐 3丁倩楠 1申帆帆 1潘红霞 2李永祥 1曹端林1
作者信息
- 1. 中北大学化学与化工学院,山西太原 030051
- 2. 湖北东方化工有限公司,湖北襄阳 441400
- 3. 山西江阳化工有限公司,山西太原 030051
- 折叠
摘要
Abstract
In order to solve the problems of long rearrangement time,high toxicity of rearrangement reagents and easy subli-mation of N-nitropyrazole(N-NP)in the synthesis of 3-nitropyrazole(3-NP),N-nitropyrazole was used as raw material to pre-pare 3-NP by the hydrothermal method using xylene as the rearrangement solvent,and the structures were characterized by mi-croscope and IR spectrum.The reaction temperature,reaction time,filling degree and other factors were optimized.The re-sults show that the optimal reaction conditions are as follows:reaction temperature of 180℃,holding time of 3 h,filling de-gree of 15％,and the yield of 3-NP at corresponding theoretical pressure of 6.130 MPa is 100％.The product purity is stabi-lized above 99％,showing that the product obtained by this process can be directly used without post-treatment.The product yield is high when the solid-to-liquid ratio(N-NP∶xylene)is 1∶3 in the hydrothermal method.Due to the low consumption,low cost,and low toxicity of rearrangement solvent,the hydrothermal method is expected to replace the traditional synthetic process of 3-NP.关键词
有机化学/熔铸炸药载体/3-硝基吡唑/3-NP/水热法/热重排/氮杂环化合物Key words
organic chemistry/melt-cast carrier explosive/3-nitropyrazole/hydrothermal method/thermal rearrangement/nitrogen heterocyclic compounds分类
军事科技引用本文复制引用
仝志珂,王明亚,陈军,侯璐,丁倩楠,申帆帆,潘红霞,李永祥,曹端林..水热法合成3-硝基吡唑的工艺优化[J].火炸药学报,2023,46(11):965-970,6.
