含能材料2024，Vol.32Issue(3)：235-241,7.DOI:10.11943/CJEM2023256
微反应器内FOX-7的连续合成工艺
Continuous Synthesis of FOX-7 in Microreactor System
摘要
Abstract
The study investigated the nitration of 2-methyl-4,6-pyrimidinone(MPO)with nitrate sulfur mixed acid in a micro-channel reactor,and further prepared 1,1-diamino-2,2-dinitroethylene(FOX-7)through hydrolysis reaction.N-octane was in-troduced as an inert solvent to generate slug flow for the reaction system.The reaction occurred inside disperse droplets,thus solving the problem of clogging of nitration intermediates in the microchannel reactor and achieving process intensification and continuous operation.The effects of reaction temperature,residence time,material ratio,and hydrolysis conditions on the prod-uct yield were investigated.The combination of microreactor and stirred reactor was proposed.At the molar ratio of nitric acid to MPO of 4.4,reaction temperature of 30℃,and residence time of 3 min in the microreactor followed by a 30 min insulation re-action in a stirred kettle,and the ring-opening realized by the hydrolysis with ice water for 2 h,the yield of FOX-7 could reach 90.1％,with a purity of over 99％.关键词
微反应器/过程强化/过程安全/1,1-二氨基-2,2-二硝基乙烯(FOX-7)/硝化反应Key words
microreactor/process intensification/process safety/1,1-diamino-2,2-dinitroethylene(FOX-7)/nitration分类
军事科技引用本文复制引用
刘璇,尧超群,廉应江,韩梅,陈光文..微反应器内FOX-7的连续合成工艺[J].含能材料,2024,32(3):235-241,7.基金项目
国家自然科学基金项目(21991103) （21991103）
