硝硫磷混酸对甲苯一硝化选择性的影响及工艺过程研究  

EFFECT OF NITRATE SULFUR PHOSPHORUS MIXED ACID ON SELECTIVITY of TOLUENE NITRATION AND PROCESS RESEARCH

作　　者：韩俊涛[1] 郭瓦力[1] 符丽[1] 桑国龙 

机构地区：[1]沈阳化工大学,辽宁沈阳110142

出　　处：《精细石油化工》2014年第6期51-56,共6页Speciality Petrochemicals

基　　金：沈阳市科技计划项目(1091036-4-00);沈阳市科技计划项目(F12-188-9-00)

摘　　要：以甲苯为原料,考察了硝硫磷混酸对甲苯一硝化选择性的影响,结果表明:在保证硝化能力的前提下,水的质量分数以20%为宜,磷酸的引入明显降低了邻对比,提高了对硝基甲苯的选择性。利用响应面软件对间歇工艺条件进行了优化,适宜的工艺条件为硝酸/硫酸/磷酸/水(质量比)=0.1∶0.29∶0.41∶0.2,加料温度40℃,加料时间30min,反应温度60℃,反应时间180min,硝化比1.19,搅拌速率330r/min,在此条件下甲苯转化率为99.28%,邻对比1.31,对硝基甲苯收率41.55%。同时对静态混合管式连续选择性硝化工艺进行初步探索,进行了相同反应时间条件下的间歇对照试验,结果表明,采用静态混合反应技术后的硝硫磷混酸硝化过程,可以提高甲苯转化率,强化传质传热效果。Effects of sulfur phosphorus nitrate mixed acid on toluene nitration selectivity were investigated with toluene as raw material.Suitable mass fraction of water was 20% at normal nitrification ability.Introduction of phosphate significantly reduces O/P to improve selectivity of p-nitrotoluene.Design-Expert 7.0 software was used to optimize process conditions.Suitable process conditions were that nitric acid∶sulphuric acid∶phosphate acid∶water=0.1∶0.29∶0.41∶0.2,feed temperature was 40 ℃,charge period was 30 min,reaction temperature was 60 ℃,reaction time was 180 min,nitrification ratio was 1.19 and stirring speed was 330 r/min.Toluene conversion rate could be 99.28%,o-/p-=1.31,yield of p-nitrotoluene was 41.55% under these conditions.At the same time,static mixing tube continuous nitrification process was studied.Intermittent comparison results under the same reaction time show that static mixing tube reaction technology can improve toluene conversion rate and strengthen effects of mass and heat transfer.

关 键 词：硝化能力 邻对比 静态混合器 对硝基甲苯 

分 类 号：TQ246.1[化学工程—有机化工]