Kaiser Andreas, Brandau Sven, Klimpel Michael, Barner-Kowollik Christopher
Preparative Macromolecular Chemistry, Institut für Technische Chemie und Polymerchemie, Karlsruhe Institute of Technology (KIT), Engesserstr. 18, 76128 Karlsruhe, Germany.
Macromol Rapid Commun. 2010 Sep 15;31(18):1616-21. doi: 10.1002/marc.201000162. Epub 2010 Sep 6.
In the current work we present results on the controlled/living radical copolymerization of acrylonitrile (AN) and 1,3-butadiene (BD) via reversible addition fragmentation chain transfer (RAFT) polymerization techniques. For the first time, a solution polymerization process for the synthesis of nitrile butadiene rubber (NBR) via the use of dithioacetate and trithiocarbonate RAFT agents is described. It is demonstrated that the number average molar mass, $\overline M _{\rm n} $, of the NBR can be varied between a few thousand and 60 000 g · mol(-1) with polydispersities between 1.2 and 2.0 (depending on the monomer to polymer conversion). Excellent agreement between the experimentally observed and the theoretically expected molar masses is found. Detailed information on the structure of the synthesized polymers is obtained by variable analytical techniques such as infrared spectroscopy (IR), nuclear magnetic resonance (NMR) spectroscopy, differential scanning calorimetry, and electrospray ionization-mass spectrometry (ESI-MS).
在当前工作中，我们展示了通过可逆加成-断裂链转移（RAFT）聚合技术对丙烯腈（AN）和1,3-丁二烯（BD）进行可控/活性自由基共聚的结果。首次描述了一种通过使用二硫代乙酸酯和三硫代碳酸酯RAFT试剂合成丁腈橡胶（NBR）的溶液聚合工艺。结果表明，NBR的数均摩尔质量$\overline M _{\rm n} $可以在几千到60000 g·mol⁻¹之间变化，多分散指数在1.2到2.0之间（取决于单体到聚合物的转化率）。实验观察到的摩尔质量与理论预期的摩尔质量之间具有良好的一致性。通过可变分析技术，如红外光谱（IR）、核磁共振（NMR）光谱、差示扫描量热法和电喷雾电离质谱（ESI-MS），获得了关于合成聚合物结构的详细信息。
