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

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

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

更新时间：2025-12-10

- Synthesis and characterization of 3,3′-disulfonated-4,4′-difuorodiphenyl sulfone disodium salt
- CIESC Journal Issue 11, Pages: 2937-2942(2009)
- 作者机构：
  
  南京理工大学化工学院
- 作者简介：
- 基金信息：
- DOI：
  CLC：
- Online First：05 November 2009，
  
  Published：05 November 2009
- 稿件说明：
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BI Huiping, CHEN Shouwen, GAO Zhilin, et al. Synthesis and characterization of 3,3′-disulfonated-4,4′-difuorodiphenyl sulfone disodium salt[J]. CIESC Journal, 2009, (11): 2937-2942.
DOI：

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

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。

Abstract

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

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.

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