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Systematic study of the synthesis and characterization of 3,3'-sulfonylbis(6-chloro benzenesulfonic acid) disodium salt monomer for proton conducting polymeric membranes in fuel cell applications

机译:用于燃料电池中质子传导聚合物膜的3,3'-磺酰基双(6-氯苯磺酸)二钠盐单体的合成和表征的系统研究

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摘要

The copolymers based on the monomer 3,3'-sulfonylbis(6-chlorobenzenesulfonic acid) di-sodium salt, abbreviated as SDCDPS in this paper, are found to have very promising properties for developing cost effective alternate proton exchange membranes. The synthesis and characterization of this monomer by sulfonation of dichloro diphenyl sulfone (DCDPS) was briefly discussed by Ueda et al. During the extensive studies conducted in our laboratory on the various copolymer of this monomer, we have found that purity of SDCDPS, as expected, plays a very important role in obtaining copolymers of high molecular weight and hence possessing better film properties. As a part of continuation of this project, it was required to scale up the monomer and polymer synthesis. This prompted us to conduct a systematic investigation of the synthesis and characterization of SDCDPS. The issues we focused on include: 1) time and temperature required for the reaction in order to obtain good yields, 2) identifying the impurities formed in the di-sulfonation reaction, and 3) choosing the best solvent combination for the recrystallization in order to get high purity monomer with constant water content. The optimization of these various process control parameters is expected to define quality control criteria for scale up production of the monomer in high yield and purity with good consistency.
机译:在本文中缩写为SDCDPS的基于单体3,3'-磺酰基双(6-氯苯磺酸)二钠盐的共聚物被发现具有开发具有成本效益的替代质子交换膜的非常有前途的性能。 Ueda等人简要讨论了通过磺化二氯二苯砜(DCDPS)来合成和表征该单体的方法。在我们实验室中对该单体的各种共聚物进行的广泛研究中,我们发现,SDCDPS的纯度如预期的那样,在获得高分子量的共聚物中具有非常重要的作用,因此具有更好的薄膜性能。作为该项目继续的一部分,需要扩大单体和聚合物的合成规模。这促使我们对SDCDPS的合成和表征进行了系统的研究。我们关注的问题包括:1)为了获得良好的收率,反应所需的时间和温度,2)识别在二磺化反应中形成的杂质,以及3)为重结晶选择最佳的溶剂组合以便获得恒定水含量的高纯度单体。这些各种过程控制参数的优化有望定义质量控制标准,以便以高收率和高纯度以良好的一致性扩大规模生产单体。

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