摘要
以w(SO3) =3 0 %的发烟硫酸为磺化剂 ,间苯二甲酸 (IPA)为反应原料制备间苯二甲酸二甲酯 5 磺酸钠(SIPM)。运用正交实验设计 ,确定了最佳磺化反应条件为 :反应温度 185℃ ,反应时间 4 5h ,反应原料配比n(IPA)∶n(SO3) =1 0 0∶1 15。通过高效液色谱 (HPLC)法确定中和深度控制在pH =5 0。SIPM制备收率达到85 2 % ,w(SIPM ) =99 5 % ,各项指标符合美国杜邦公司 2 0 0
The title compound(SIPM) was prepared from isophthalic acid(IPA),using w(SO_3)=30% oleum as sulfonating agent.By orthogonal experimental design method,the optimum sulfonation reaction conditions were determined:n(IPA)∶n(SO_3)=1.00∶1.15 at 185 ℃ for 4.5 h.By HPLC method,the neutralization process was controlled at pH value of 5.0.Yield of SIPM was 85.2% and the purity was w(SIPM)=99.5%.Specifications of the product comformed with the standard of Du Pont Co..
出处
《精细化工》
EI
CAS
CSCD
北大核心
2003年第1期50-52,共3页
Fine Chemicals