苯二甲酸的连续硝化反应研究  

Study on Continuous Flow Nitration of Phthalic Acid

作　　者：肖燕[1] 王源 王俊峰 周英雷 夏春年[1] XIAO Yan;WANG Yuan;WANG Jun-feng;ZHOU Ying-lei;XIA Chun-nian*(College of Pharmacy,Zhejiang University of Technology,Hangzhou,Zhejiang 310014,China;Juxian Pharmaceutical Technology Co.,Ltd.,Taizhou,Zhejiang 317016,China)

机构地区：[1]浙江工业大学药学院,浙江杭州310014 [2]浙江聚贤医药科技有限公司,浙江台州317016

出　　处：《浙江化工》2020年第4期19-24,共6页Zhejiang Chemical Industry

基　　金：浙江工业大学横向(H1160190007)。

摘　　要：以邻苯二甲酸酐、间苯二甲酸和对苯二甲酸为原料,在连续流反应器中采用硝酸/硫酸混酸工艺合成了苯二甲酸硝基衍生物,研究了反应温度、硝酸/硫酸配比及用量、停留时间等对反应的影响。结果表明:对苯二甲酸硝化不适用于在连续化反应器中进行;间苯二甲酸在微通道反应器中硝化的最优条件为:n(间苯二甲酸):n(发烟硝酸):n(浓硫酸)=1:1.7:7,反应温度为75℃,保留时间为40.9 s,转化率为99.8%,5-硝基间苯二甲酸产率为95%,选择性为100%;邻苯二甲酸酐在微通道反应器中硝化的最优条件为:n(邻苯二甲酸酐):n(发烟硝酸):n(浓硫酸)=1:1.5:3,反应温度为90℃,保留时间为60.6 s,转化率为100%,3-硝基邻苯二甲酸收率为37%,选择性为41.3%。Using phthalic anhydride,isophthalic acid and terephthalic acid as raw materials,a nitro derivative of phthalic acid was synthesized by a nitric acid/sulfuric acid mixed acid process in a continuous flow reactor.The effects of reaction temperature,nitric acid/sulfuric acid ratio and dosage,and residence time on the reaction were studied.The results show that the nitration of terephthalic acid is not suitable for continuous reactors;the optimal conditions for the nitration of isophthalic acid in a microchannel reactor are:n(isophthalic acid):n(fuming nitric acid):n(concentrated sulfuric acid)=1:1.7:7,reaction temperature is 75℃,retention time is 40.9 s,conversion rate is 99.8%,yield of 5-nitroisophthalic acid is 95%,and selectivity is 100%;The optimal conditions for nitration of phthalic anhydride in the microchannel reactor are:n(phthalic anhydride):n(fuming nitric acid):n(concentrated sulfuric acid)=1:1.5:3,the reaction temperature is 90℃,retention time is 60.6 s,conversion rate is 100%,yield of 3-nitrophthalic acid is 37%,selectivity is 41.3%.

关 键 词：间苯二甲酸 邻苯二甲酸酐 对苯二甲酸 硝化 微通道 连续流 

分 类 号：TQ245.12[化学工程—有机化工]