乙烯基磺酸酯的RAFT聚合可控制合成聚乙烯基磺酸锂和磺化嵌段共聚物,Macromolecules

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乙烯基磺酸酯的RAFT聚合可控制合成聚乙烯基磺酸锂和磺化嵌段共聚物
Macromolecules ( IF 5.1 ) Pub Date : 2010-08-06 00:00:00 , DOI: 10.1021/ma100905w
Hideharu Mori ₁ , Eisuke Kudo ₁ , Yousuke Saito ₁ , Atsuhiko Onuma ₂ , Makoto Morishima ₂

Affiliation

通过常规的自由基聚合和可逆的加成-断裂链转移（RAFT）聚合反应，聚合了四种乙烯基磺酸酯衍生物，新戊基乙磺酸酯（NES），乙丁基乙磺酸酯（BES），异丙基乙磺酸酯（IPES）和苯基乙磺酸酯（PES）。。对于这些RAFT聚合，比较了三种黄药型链转移剂（CTA），二硫代氨基甲酸酯型CTA和二硫酯型CTA。在各种CTAs中，O-乙基-S-（1-甲氧基羰基）乙基二硫代碳酸酯最有效地获得具有低多分散性的聚（NES）和聚（BES）。为了确定条件，检查了温度，CTA与引发剂摩尔比等几个参数的影响，从而确定了对聚合反应的最佳控制。在合适的条件下使用黄原酸酯型CTA，通过形成相对较低的多分散性产物，分子量随转化率线性增加以及控制分子量的可行性，证实了NES聚合的合理控制。消耗的单体与所用CTA量的比率。BES的聚合行为与NES相当。聚（NES）的新戊基的脱保护顺利进行，得到水溶性聚（乙烯基磺酸锂）。NES的RAFT聚合反应通过使用聚（N-乙烯基咔唑）-大号CTA，然后脱保护。

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RAFT Polymerization of Vinyl Sulfonate Esters for the Controlled Synthesis of Poly(lithium vinyl sulfonate) and Sulfonated Block Copolymers

Four vinyl sulfonate ester derivatives, neopentyl ethenesulfonate (NES), 1-butyl ethenesulfonate (BES), isopropyl ethenesulfonate (IPES), and phenyl ethenesulfonate (PES), were polymerized by conventional radical polymerization and reversible addition−fragmentation chain transfer (RAFT) polymerization. Three xanthate-type chain transfer agents (CTAs), a dithiocarbamate-type CTA, and a dithioester-type CTA were compared for these RAFT polymerizations. Among various CTAs, O-ethyl-S-(1-methoxycarbonyl) ethyldithiocarbonate was the most efficient to obtain poly(NES) and poly(BES) having low polydispersities. The effects of several parameters, such as temperature and CTA to initiator molar ratio, were examined in order to determine the conditions, leading to optimal control of the polymerization. With the xanthate-type CTA under suitable conditions, reasonable control of the polymerization of NES was confirmed by the formation of the relatively low polydispersity products, linear increase in the molecular weight with the conversion, and feasibility in the control of the molecular weight based on the ratio of monomer consumed to the amount of CTA used. The polymerization behavior of BES was comparable to that of NES. Deprotection of the neopentyl group of the poly(NES) proceeded smoothly to give water-soluble poly(lithium vinyl sulfonate). Synthesis of the well-defined block copolymer involving the poly(lithium vinyl sulfonate) segment was conducted by RAFT polymerization of NES using poly(N-vinylcarbazole) macro-CTA, followed by deprotection.

更新日期：2010-08-06

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