硝酸异丙酯的连续流微通道合成及动力学  

Continuous Flow Microchannel Synthesis and Kinetics of Isopropyl Nitrate

作　　者：吴越江 詹乐武 侯静 李斌栋[1] WU Yue-jiang;ZHAN Le-wu;HOU Jing;LI Bin-dong(School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China)

机构地区：[1]南京理工大学化学与化工学院,江苏南京210094

出　　处：《火炸药学报》2025年第3期265-270,I0005,共7页Chinese Journal of Explosives & Propellants

基　　金：国家自然科学基金面上项目(No.21875109)。

摘　　要：为了解决传统工艺制备硝酸异丙酯(IPN)存在的反应过程不易控制、反应温度过高及收率低等问题,采用心型微通道反应器,以异丙醇为原料、二氯甲烷为溶剂,经发烟硝酸和乙酸酐的作用合成了硝酸异丙酯(IPN);考察了异丙醇、发烟硝酸和乙酸酐摩尔比、发烟硝酸质量分数、总流速、反应温度等因素对硝化反应的影响。结果表明,在温度10℃,总流速60mL/min,发烟硝酸质量分数98%,异丙醇、发烟硝酸和乙酸酐的摩尔比1∶1.2∶0.9,异丙醇和二氯甲烷质量比1∶1的条件下,转化率可达99.83%。建立了均相IPN硝化反应动力学模型,拟合得到活化能为37.05kJ/mol,指前因子为4.93×10^(4)L/(mol·s)。To solve the problems associated with difficulty in reaction controlling,high reaction temperature,and low yield in the synthesis of isopropyl nitrate(IPN)by conventional process,a heart-shaped microchannel reactor was used to synthesize IPN by using isopropanol as raw material and dichloromethane as solvent,through the reaction of fuming nitric acid and acetic anhydride.The effects of factors such as the molar ratio of isopropanol,fuming nitric acid and acetic anhydride,the mass fraction of fuming nitric acid,total flow rate,and reaction temperature on the nitrification reaction were investigated.Results show that at the temperature of 10℃,total flow rate of 60mL/min,mass fraction of fuming nitric acid of 98%,molar ratio of isopropanol,fuming nitric acid and acetic anhydride of 1∶1.2∶0.9,and mass ratio of isopropanol and dichloro-methane of 1∶1,the conversion rate can reach to 99.83%.A homogeneous kinetic model for the nitration reaction of IPN was established.The activation energy is 37.05kJ/mol by fitting,and the pre-exponential factor is 4.93×10^(4) L/(mol·s).

关 键 词：有机化学 微通道反应器 硝酸异丙酯 IPN 硝化反应 异丙醇 二氯甲烷 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O62[理学—有机化学]