邻氯苯腈的硝化工艺研究  

Study on the Nitration Process of o-Chlorobenzonitrile

作　　者：何江伟 丁兴成 陈琪汉 龚斌彬 王天校 陶彬彬 HE Jiang-wei;DING Xing-cheng;CHEN Qi-han;GONG Bin-bin;WANG Tian-xiao;TAO Bin-bin(Zhejiang Runtu Co.,Ltd.,Shaoxing,Zhejiang 312369,China)

机构地区：[1]浙江闰土股份有限公司,浙江绍兴312369

出　　处：《浙江化工》2022年第10期30-34,共5页Zhejiang Chemical Industry

摘　　要：本文以邻氯苯腈为起始原料,1,2-二氯乙烷为溶剂,硝酸和硫酸的混酸为硝化剂,经硝化反应生成2-氯-5-硝基苯甲腈。考察了溶剂种类、溶剂用量、混酸用量、反应温度、稀释酸度等工艺条件对反应的影响,同时验证了该方法用于连续化硝化的可行性。结果表明,当n(邻氯苯腈):n(硝酸):n(硫酸):n(二氯乙烷)=1:1.15:2.5:2.6,反应体系温度为0℃~15℃,反应时间为3 h,反应效果最佳。在该工艺条件下,产品纯度达98%以上,收率达95%以上。In this paper,o-chlorobenzonitrile was used as the starting material,1,2-dichloroethane was used as the solvent,and the mixed acid of nitric acid and sulfuric acid was used as the nitrating agent,2-chloro-5-nitrobenzonitrile was generated by nitration reaction.The effects of process conditions such as solvent type,solvent dosage,mixed acid dosage,reaction temperature,and dilution acidity on the reaction were investigated,and the feasibility of the method for continuous nitration was verified.The results show that when n(o-chloroben zonitrile):n(nitric acid):n(sulfuric acid):n(dichloroethane)=1:1.15:2.5:2.6,the temperature of the reaction system is 0℃~15℃,and the reaction time is 3 h,the reaction effect is the best.Under this process condition,the product purity reaches more than 98%,and the yield reaches more than 95%.

关 键 词：邻氯苯腈 硝酸 硫酸 1 2-二氯乙烷 微通道反应器 

分 类 号：TQ246.7[化学工程—有机化工]