2,2′-二硫代水杨酸的合成工艺研究  

Process for Preparation of 2, 2'-Dithiodibenzoic Acid

作　　者：倪越彪 贾建洪[2] 徐俊平 高建荣[2] 孙炬晖 

机构地区：[1]上虞市洁源环保科技有限公司,浙江上虞312369 [2]浙江工业大学,绿色化学合成技术国家重点实验室培育基地,杭州310032

出　　处：《化工生产与技术》2010年第3期8-10,共3页Chemical Production and Technology

基　　金：浙江省重大科技专项(2008C11052)

摘　　要：以邻氨基苯甲酸为原料,经亚硝酸钠和盐酸重氮化后,在低温下与液体二氧化硫进行硫化反应得到2,2'-二硫代水杨酸。考察并优化了合成工艺参数,重氮化温度为0～5℃,催化剂为硫酸铜,助催化剂为碘化钾,硫化温度为5℃,液体二氧化硫的用量按n(邻氨基苯甲酸):n(SO2)=1:4选择。在此条件下收率为95.8%,高效液相色谱仪测定质量分数为98.1%。目标产物经红外、元素分析、质谱结构确认。该路线具有收率高、操作简单、产品纯度高等优点。2,2′-dithiodibenzoic acid was prepared from anthranilic acid,sodium nitrite,hydrochloric acid and liquid sulfur dioxide via diazotization reaction and sulfidation reaction.The process parameters were investigated in details and the optimum reaction conditions were as follows: the temperature of diazotization 0~5 ℃,CuSO4 as catalyst,KI as cocatalyst,temperature of sulfidation 5 ℃,dosage of liquid sulfur dioxide n(anthranilic acid)∶n(SO2)=1∶4,the yield was 95.8% by anthranilic acid and the purity (HPLC) was 98.1%.The chemical structures of the product was identified and confirmed by IR,MS and elemental analysis.The process has the advantages such as high yield,simple operation and high purity.

关 键 词：2 2’二硫代水杨酸 邻氨基苯甲酸 液体二氧化硫 重氮化 硫化 

分 类 号：TQ245.4[化学工程—有机化工]