3,3′-二磺化-4,4′-二氟二苯砜二钠盐的合成与表征  

Synthesis and characterization of 3,3'-disulfonated-4,4'-difuorodiphenyl sulfone disodium salt

作　　者：毕慧平[1] 陈守文[1] 高智琳[1] 张莎[1] 王连军[1] 

机构地区：[1]南京理工大学化工学院,江苏南京210094

出　　处：《化工学报》2009年第11期2937-2942,共6页CIESC Journal

基　　金：江苏省自然科学基金项目(BK2007211);教育部留学回国人员科研启动基金项目;南京理工大学留学回国人员科研启动基金项目~~

摘　　要：以工业级4,4′-二氟二苯砜(DFDPS)为原料,利用升华方法进行纯化处理后,采用发烟硫酸直接磺化,通过改变反应物计量比、反应温度、反应时间等参数,系统研究了3,3′-二磺化-4,4′-二氟二苯砜二钠盐(SDFDPS)的制备方法。采用HPLC、UV、1HNMR及FTIR对磺化产物结构及纯度进行了表征,由此得到最佳的磺化条件为:反应物摩尔比(SO3:DFDPS)为3.0:1,在110℃下反应20h。在此反应条件下的磺化产物中未发现单磺化产物以及未磺化的原料DFDPS。经过乙醇/水两次重结晶后,总收率达到75%。以合成的SDFDPS为原料合成了磺化度60%的磺化聚芳醚砜聚合物,该聚合物具有较高的相对黏度,同样也表明了SDFDPS的高纯度。3,3＇-Disulfonated-4,4＇-difluorophenyl sulfone （ SDFDPS ） was synthesized from 4,4＇- difluorophenyl sulfone （DFDPS） with industrial grade. The starting material DFDPS was purified by sublimation before use. The reaction condition was optimized by varying the molar ratio of SOa to DFDPS, reaction temperature and reaction time. The purity and yield of the product was determined by using HPLC, UV, ^1H NMR and FTIR. The optimized reaction condition was found as that the molar ratio of SO3 to DFDPS is 3.0 ： 1 with a reaction temperature of 110℃ for 20 h, under which neither monosulfonated product nor DFDPS residue was detected. The product SDFDPS was obtained with a total yield of 75% upon recrystallization twice from ethanol/water. Poly（arylene ether sulfone） copolymer with 60% sulfonation degree prepared from the synthesized SDFDPS shows a high relative viscosity, which also indicates the high purity of the synthesized SDFDPS.

关 键 词：磺化反应 二氟二苯砜 磺化聚芳醚砜 质子交换膜 

分 类 号：O625.752[理学—有机化学] O631[理学—化学]