Synthesis and characterization of dumbbell-shaped polystyrene

Synthesis and characterization of dumbbell-shaped polystyrene
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哑铃型聚苯乙烯的合成与表征

DOI:
10.1016/j.polymer.2016.10.037
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发表时间:
2016
期刊:
影响因子:
4.6
通讯作者:
Y. Matsushita
Y. Matsushita
中科院分区:
化学2区
文献类型:
--
作者:
Y. Doi;A. Takano;Y. Matsushita

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通过在具有两个二苯基乙烯(DPE)型乙烯基的高度纯化的环状PS(R-30;Mw= 33.7kg/mol)和双官能活性线性PS(L-80;Mw= 84.0kg/mol)之间的偶联反应,阴离子合成哑铃形聚苯乙烯(PS)样品,其中环连接在线性链的两端。确认所获得的粗偶联产物除了作为副产物的未反应的L-80和R-30以及单尾蝌蚪聚合物之外还包括目标哑铃聚合物。为了分离哑铃聚合物,进行了连续的尺寸排阻色谱(SEC)和相互作用色谱(IC)分级。发现具有足够高纯度(99.9%)的哑铃链(D-30/80/30;Mw= 147 kg/mol)与具有IC模式中的单尾的蝌蚪聚合物分离,这仅仅是由于它们的链结构的小差异,即,在线性链的一个或两个链端上存在小环。这是首次成功制备高分子量、高纯度哑铃形聚合物的报道,该产品必须适合于精确物理性质的研究。
A dumbbell-shaped polystyrene (PS) sample, where rings are attached on both ends of a linear chain, was anionically synthesized by a coupling reaction between highly-purified ring PS (R-30;Mw= 33.7 kg/mol) with two diphenylethylene (DPE) type vinyl groups and bifunctional living linear PS (L-80;Mw= 84.0 kg/mol). The crude coupling product obtained was confirmed to include a targeted dumbbell polymer in addition to unreacted L-80 and R-30, and a single-tail tadpole polymer as byproducts. To isolate the dumbbell polymer, successive size-exclusion chromatography (SEC) and interaction chromatography (IC) fractionations were performed. It was found out that the dumbbell chain (D-30/80/30;Mw= 147 kg/mol) with sufficiently high purity (99.9%) was separated from the tadpole polymer with a single-tail in IC mode just due to a small difference in their chain architectures, i.e., the presence of the small rings on either one or both chain ends of a linear chain. This is the first report on successful preparation of a dumbbell-shaped polymer with high molecular weight and high purity, and the present product must be suitable for investigation of accurate physical properties.
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影响因子: 41.2
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