3,3′-二磺化-4,4′-二氟二苯砜二钠盐的合成与表征

化工学报 ›› 2009, Vol. 60 ›› Issue (11): 2937-2942.

• 材料化学工程与纳米技术 • 上一篇

3,3′-二磺化-4,4′-二氟二苯砜二钠盐的合成与表征

毕慧平;陈守文;高智琳;张莎;王连军

南京理工大学化工学院

出版日期:2009-11-05 发布日期:2009-11-05

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

BI Huiping;CHEN Shouwen;GAO Zhilin;ZHANG Sha;WANG Lianjun

Online:2009-11-05 Published:2009-11-05

摘要/Abstract

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、¹H NMR 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20 h。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。

关键词:

磺化反应, 二氟二苯砜, 磺化聚芳醚砜, 质子交换膜

Abstract:

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 SO₃ 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.

Key words:

磺化反应, 二氟二苯砜, 磺化聚芳醚砜, 质子交换膜

毕慧平, 陈守文, 高智琳, 张莎, 王连军. 3,3′-二磺化-4,4′-二氟二苯砜二钠盐的合成与表征 [J]. 化工学报, 2009, 60(11): 2937-2942.

BI Huiping, CHEN Shouwen, GAO Zhilin, ZHANG Sha, WANG Lianjun. Synthesis and characterization of 3,3′-disulfonated-4,4′-difuorodiphenyl sulfone disodium salt[J]. CIESC Journal, 2009, 60(11): 2937-2942.

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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

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