摘要
以3-氨基-4-氯苯甲酸和正十六醇为原料,二甲苯为溶剂,对甲苯磺酸为催化剂,通过酯化合成了3-氨基-4-氯苯甲酸十六酯。采用FTIR、~1HNMR对产品的结构进行表征。考察了醇酸物质的量比、催化剂加量、反应物质量分数对酯化率的影响。结果表明∶n(醇)∶n(酸)=1.2∶1,催化剂用量为体系总质量的5%,反应物为体系总质量的65%,反应时间7 h,酯化率达96.20%,单程收率为73.91%。另外,确立了产物提纯、提高单程收率和滤液去除催化剂后回收、重复使用的最佳系统工艺路线,单程收率提至78.90%,总收率为82.62%,产品的纯度高于98.00%。
Hexadecyl 3-amino-4-chlorobenzoate was synthesized by esterification of 3-amino-4-chlorobenzoic and n-hexadecanol using xylene as solvent in the presence of catalyst of p-toluenesulfonic acid.The product was characterized by FTIR and^1HNMR.The effects of molar ratio of 3-amino-4-chlorobenzoic to n-hexadecanol,amount of catalyst,reactants’mass fraction on the esterification rate were investigated.The optimal conditions were obtained as follows∶n(n-hexadecanol)∶(3-amino-4-chlorobenzoic)=1.2∶1,amount of catalyst being 5%of the total mass of the system,reacants’mass fraction 65%and reaction time7 h.Under the above-mentioned conditions,the esterification rate was 96.20%,and the once-through yield was 73.91%.In addition,the best system route for product purification was established to improve once-through yield and the filtrate recovery and reuse after removal of catalyst.The once-through yield increased to 78.90%,the total yield was 82.62%,and the purity of the product was higher than 98.00%.
作者
周丹
苏韵
许巍巍
解一军
ZHOU Dan;SU Yun;XU Wei-wei;XIE Yi-jun(Institute of Polymer Materials,School of Chemical Engineering,Hebei University of Technology,Tianjin 300130,China;Shenyang Photosensitive Chemcial Research Institute Co.Ltd,Shenyang 110141,Liaoning,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2019年第8期1722-1726,共5页
Fine Chemicals
