4-N,N-二甲氨基硫代苯甲酸合成工艺的研究  

Study on the Synthetic Process of 4-N,N-dimethylaminothiobenzoic Acid

作　　者：汪锐 赵晓敏 解凯钧 李政浩 樊飞龙 王振宣 付强 潘高峰 刘恒驿 WANG Rui;ZHAO Xiaomin;XIE Kaijun;LI Zhenghao;FAN Feilong;WANG Zhenxuan;FU Qiang;PAN Gaofeng;LIU Hengyi(School of Petrochemical Technology,Jilin Institute of Chemical Technology,Jilin 132022,China;Jilin Second Geological Survey Institute,Jilin 132000,China;Jilin Chemical Fiber Group Co.Ltd.,Jilin 132115,China)

机构地区：[1]吉林化工学院石油化工学院,吉林吉林132022 [2]吉林省第二地质调查所,吉林吉林132000 [3]吉林化纤集团有限公司,吉林吉林132115

出　　处：《吉林化工学院学报》2022年第7期1-5,共5页Journal of Jilin Institute of Chemical Technology

基　　金：吉林化工学院科学技术研究项目(2020021);吉林化工学院重大科技项目(2020010);吉林化工学院博士启动项目(2021016).

摘　　要：对以4-N,N-二甲氨基苯甲酰氯和NaHS为原料合成4-N,N-二甲氨基硫代苯甲酸(DMATBA)的工艺进行了研究,重点考察了反应溶剂种类、反应浓度、n(NaHS)n(4-N,N-二甲氨基苯甲酰氯)投料比、反应时间、反应温度、n(NaHS)n(HCl)用量比对产物收率的影响.实验结果表明,最佳的合成工艺为:反应溶剂DMF,反应浓度1.0 mol·L^(-1),n(NaHS)n(4-N,N-二甲氨基苯甲酰氯)=21,反应时间2.5 h,反应温度25℃,n(NaHS)n(HCl)=11(pH=3);经由酸化、萃取、减压蒸馏处理后,DMATBA总收率可达到82.1%,纯度为93.6%.The process of synthesizing 4-N,N-dimethylaminothiobenzoic acid(DMATBA)with 4-N,N-dimethylaminobenzoyl chloride and NaHS as raw materials was studied,involving the influence of the type of reaction solvent,reaction concentration,n(NaHS)n(4-N,N-dimethylaminobenzoyl chloride)feed ratio,reaction time,reaction temperature and n(NaHS)n(HCl)dosage ratio on the yields of the product.The effects of solvent type,reaction concentration,n(NaHS)n(4-N,N-Dimethylaminobenzyl Chloride)feeding ratio,reaction time,reaction temperature,n(NaHS)n(HCl)dosage ratio of on product yield were investigated.Experimental results show that the best synthesis process in this screen involved reaction solvent DMF,reaction concentration 1.0 mol/L,n(NaHS)n(4-N,N-dimethylaminobenzoyl chloride)=21,reaction time 2.5 h,reaction temperature 25℃,n(NaHS)n(HCl)=11(pH=3);after acidification,extraction,and vacuum distillation,the total yield of DMATBA can reach 82.1%,and the purity is 93.6%.

关 键 词：4-N N-二甲氨基硫代苯甲酸 合成工艺 收率 

分 类 号：TH3[机械工程—机械制造及自动化]