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通过反碘转移聚合制备的聚苯乙烯-b-聚(正丁基丙烯酸酯)嵌段共聚物的结构解析的高级分析方法。

Advanced analytical methods for the structure elucidation of polystyrene-b-poly(n-butyl acrylate) block copolymers prepared by reverse iodine transfer polymerisation.

机构信息

Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, 7602 Matieland, South Africa.

Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, 7602 Matieland, South Africa.

出版信息

Anal Chim Acta. 2015 Sep 10;892:183-94. doi: 10.1016/j.aca.2015.08.005. Epub 2015 Aug 22.

DOI:10.1016/j.aca.2015.08.005
PMID:26388490
Abstract

Reverse iodine transfer polymerisation (RITP) is a living radical polymerisation technique that has shown to be feasible in synthesising segmented styrene-acrylate copolymers. Polymers synthesised via RITP are typically only described regarding their bulk properties using nuclear magnetic resonance spectroscopy and size exclusion chromatography. To fully understand the complex composition of the polymerisation products and the RITP reaction mechanism, however, it is necessary to use a combination of advanced analytical methods. In the present RITP procedure, polystyrene was synthesised first and then used as a macroinitiator to synthesise polystyrene-block-poly(n-butyl acrylate) (PS-b-PBA) block copolymers. For the first time, these PS-b-PBA block copolymers were analysed by a combination of SEC, in situ(1)H NMR and HPLC. (1)H NMR was used to determine the copolymer composition and the end group functionality of the samples, while SEC and HPLC were used to confirm the formation of block copolymers. Detailed information on the living character of the RITP process was obtained.

摘要

反向碘转移聚合(RITP)是一种活自由基聚合技术,已被证明在合成分段苯乙烯-丙烯酸酯共聚物方面是可行的。通过 RITP 合成的聚合物通常仅使用核磁共振波谱和尺寸排阻色谱法来描述其本体性质。然而,为了充分了解聚合产物的复杂组成和 RITP 反应机理,有必要使用多种先进的分析方法。在本 RITP 程序中,首先合成聚苯乙烯,然后将其用作大分子引发剂来合成聚苯乙烯-嵌段-聚(n-丁基丙烯酸酯)(PS-b-PBA)嵌段共聚物。首次使用 SEC、原位(1)H NMR 和 HPLC 组合分析这些 PS-b-PBA 嵌段共聚物。(1)H NMR 用于确定样品的共聚物组成和端基官能团,而 SEC 和 HPLC 用于确认嵌段共聚物的形成。获得了关于 RITP 过程的活性质的详细信息。

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