非水体系合成水杨酰胺的工艺研究  

Synthesis of Salicylamide in Non-aqueous System

作　　者：王喆 唐浩洋 杨振浩 刘卫东 罗和安[2] 刘国文 周锦萍 WANG Zhe;TANG Hao-yang;YANG Zhen-hao;LIU Wei-dong;LUO He-an;LIU Guo-wen;ZHOU Jin-ping(Hunan Haili Chemical Industry Co.,Ltd.,Changsha 410007,China;School of Chemical Engineering,Xiangtan University,Xiangtan 411105,China;National Engineering Research Center of Agrochemicals,Hunan Research Institute of Chemical Industry Co.,Ltd.,Changsha 410014,China;Agrochemical Key Laboratry of Hunan Province,Changsha 410014,China)

机构地区：[1]湖南海利化工股份有限公司,湖南长沙410007 [2]湘潭大学化工学院,湖南湘潭411105 [3]湖南化工研究院有限公司国家农药创制工程技术研究中心,湖南长沙410014 [4]农用化学品重点实验室,湖南长沙410014

出　　处：《精细化工中间体》2024年第3期10-14,47,共6页Fine Chemical Intermediates

基　　金：芙蓉计划省企业科技创新创业团队(湖南海利化工新材料科技创新创业团队)。

摘　　要：以水杨酸为原料,在固体酸强酸树脂催化下与甲醇酯化反应合成水杨酸甲酯,再和氨气在甲醇中氨化反应合成水杨酰胺。优化反应条件为:酯化反应,m(强酸树脂)∶m(水杨酸)=0.35∶1.00,n(甲醇)∶n(水杨酸)=10∶1,反应温度135℃,固体酸循环催化10次后,水杨酸甲酯平均收率81.1%,纯度99.2%;氨化反应,n(氨气)∶n(水杨酸甲酯)=4.0∶1.0,m(甲醇)∶m(水杨酸甲酯)=1.0∶1.0,m(亚硫酸钠)∶m(水杨酸甲酯)=0.002∶1.000,反应温度60℃,水杨酰胺收率99.3%,纯度99.1%。该法具有产品纯度高、收率高、废水少、绿色环保等优势。As raw material,cyclical acid was esterified with methanol under the catalysis of solid acid to get methyl salicylate,and then the methyl salicylate was ammoniated with ammonia in methanol to synthesize salicylamide.The optimized reaction conditions were as following:in esterfication reaction,the mass ratio of strong acid resins to salicylic acid was 0.35:1.00,the molar ratio of methanol to salicylic acid was 10:1,and the reaction temperature was 135 C.After catalysis for 10 cycles of solid acid,the average yield of methyl salicylate was 81.1%and the content was 99.2%.In ammonification reaction,the molar ratio of ammonia to methyl salicylate was 4.0:1.0,the mass ratio of methanol to methyl salicylate was 1.0:1.0,the mass ratio of sodium sulfite to methyl salicylate was 0.002:1.000,and the reaction temperature was 60℃,with the yield and the content of salicylamide as 99.3%and 99.1%,respectively.This method has the advantages of high purity,high yield,less wastewater and is environmentally friendly.

关 键 词：水杨酰胺 水杨酸甲酯 水杨酸 固体酸 合成 

分 类 号：TQ450.4[化学工程—农药化工]