A Novel Method for 13C-NMR Spectroscopy of Polymer in Emulsion: Quantitative Analysis of Microstructure of Crosslinked Polybutadiene in Latex
A Novel Method for 13C-NMR Spectroscopy of Polymer in Emulsion: Quantitative Analysis of Microstructure of Crosslinked Polybutadiene in Latex
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乳液中聚合物的 13C-NMR 光谱新方法：胶乳中交联聚丁二烯微观结构的定量分析
DOI：
10.5254/1.3538836
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发表时间：
1999
影响因子：
1.5
通讯作者：
Yasuyuki Tanaka
中科院分区：
文献类型：
--
作者：
S. Kawahara;Saori Bushimata;T. Sugiyama;C. Hashimoto;Yasuyuki Tanaka
介绍了一种利用高分辨~(13)C-核磁共振谱研究聚合物乳液的新方法。聚合物乳液是由聚合物分散体和水组成的非均相体系。获得最佳光谱的聚丁二烯胶乳的适宜表面活性剂浓度为1w/v%，干胶含量为10%。胶乳样品的共振峰的半宽几乎与在溶液中获得的半宽相同，后者大约是使用交联或可溶聚丁二烯固体样品获得的半宽的三分之一。然而，乳胶样品的信噪比略低于溶液样品。胶乳样品的自旋-晶格弛豫时间T1与固体样品相似。这些结果表明，乳胶态13C-核磁共振波谱将是表征分散体交联凝胶结构的一种强有力的技术，因为它提供了可与溶液态谱相媲美的高分辨率谱，显示出与固体13C-核磁共振谱相对应的较短的T1。用高分辨乳胶态13C-核磁共振谱测定了聚丁二烯的各种异构体在分散体中的浓度。
A novel analytical method using high resolution 13 C-NMR spectroscopy to study polymer latex, which is a heterogeneous system comprising polymer dispersoid and water, is described. The appropriate concentrations of surfactant and dried rubber content of a polybutadiene latex, which give the best spectrum, were found to be 1 w/v % and 10%, respectively. The half-widths of resonance peaks for the latex sample were almost identical to the half-widths obtained in solution, which were about one-third the width of those obtained using a solid sample of either a crosslinked or soluble polybutadiene. Nevertheless, the signal to noise ratio for the latex sample was slightly smaller than that for the solution sample. The values of spin-lattice relaxation time, T 1 , for the latex sample were similar to those for the solid sample. These demonstrate that the latex state 13 C-NMR spectroscopy will be a powerful technique for structural characterization of crosslinked gels in the dispersoid because it gives a high resolution spectrum comparable to solution state spectroscopy, showing short T 1 values corresponding to those for solid state 13 C-NMR spectroscopy. High resolution latex state 13 C-NMR spectroscopy was used to determine the concentrations of the various isomers of the polybutadiene in the dispersoid.