3,4-二氯苯甲醛肟化反应热危险性研究  

Thermal hazard study of oximation reaction of 3,4-dichlorobenzaldehyde

作　　者：阳亦 苏学 钱华[1,3] 李芳 YANG Yi;SU Xue;QIAN Hua;LI Fang(School of Chemistry and Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,Jiangsu Province,China;Suzhou New Century Testing Technology Service Limited Company,Suzhou 215000,Jiangsu Province,China;China National Quality Supervision Testing Center for Industrial Explosive Materials,Nanjing 210094,Jiangsu Province,China)

机构地区：[1]南京理工大学化学与化工学院,江苏南京210094 [2]苏州新世纪检测技术服务有限公司,江苏苏州215000 [3]国家民用爆破器材质量检验检测中心,江苏南京210094

出　　处：《化学工程》2023年第4期84-88,共5页Chemical Engineering(China)

摘　　要：为研究3,4-二氯苯甲醛肟化反应过程热危险性,分别采用差示扫描量热仪(DSC)、绝热加速量热仪(ARC)、Gaussian 09软件和反应量热仪(RC1e),对原料、产物的热分解情况以及肟化反应过程的热效应进行研究。结果表明:原料3,4-二氯苯甲醛吸热量为157.08 kJ/kg,盐酸羟胺放热量为2561.63 kJ/kg,反应后混合物料放热量为462.52 kJ/kg;反应失控情况下,最大反应速率到达时间为24 h时所对应的温度T D24为501.78 K;反应过程体系理论计算所得反应热为153.36 kJ/kg,实验测得放热量为139.47 kJ/kg。综合考虑以实测数据对工艺危险度等级进行评估,可知工艺存在冲料及分解风险,并给出了相应的建议措施。In order to investigate the thermal hazard of oximation reaction of 3,4-dichlorobenzaldehyde,differential scanning calorimeter(DSC),acceleration rate calorimeter(ARC),Gaussian 09 software and reaction calorimeter(RC1e)were used to study the thermal decomposition of raw materials and products as well as the thermal effect of reaction.The absorbed heat of 3,4-dichlorobenzenaldehyde is 157.08 kJ/kg,heat of decomposition of hydroxylamine hydrochloride and reacted mixture is 2561.63 kJ/kg and 462.52 kJ/kg,respectively.The initial temperature T D24 corresponding to the maximum reaction rate at arriving time 24 h is 501.78 K under the uncontrolled reaction.The calculated heat of reaction is 153.36 kJ/kg,which is comparable to the measured result 139.47 kJ/kg.Based on the conducted measured data,it is known that the oximation process have the risk of flushing and decomposition,and the corresponding recommendations are given.

关 键 词：3 4-二氯苯甲醛 肟化反应 热危险性 绝热加速量热仪 反应量热仪 

分 类 号：X937[环境科学与工程—安全科学]