Herberg Artjom, Yu Xiaoqian, Kuckling Dirk
Department Chemie, Universität Paderborn, Warburger Str. 100, D-33098 Paderborn, Germany.
Polymers (Basel). 2019 Apr 13;11(4):678. doi: 10.3390/polym11040678.
Studies on the end group stability of poly(-isopropylacrylamide) during the atom transfer radical polymerization (ATRP) process are presented. Polymerization of -isopropylacrylamide was conducted in different solvents using a copper(I) chloride/MeTren catalyst complex. The influence of the ATRP solvent as well as the polymer purification process on the end group stability was investigated. For the first time, mass spectrometry results clearly underline the loss of ω end groups via an intramolecular cyclization reaction. Furthermore, an ATRP system based on a copper(I) bromide/MeTren catalyst complex was introduced, that showed not only good control over the polymerization process, but also provided the opportunity of block copolymerization of -isopropylacrylamide with acrylates and other -substituted acrylamides. The polymers were characterized using H-NMR spectroscopy and size exclusion chromatography. Polymer end groups were determined via ESI-TOF mass spectrometry enhanced by ion mobility separation (IMS).
本文介绍了聚（N-异丙基丙烯酰胺）在原子转移自由基聚合（ATRP）过程中端基稳定性的研究。使用氯化亚铜/甲基三乙烯四胺催化剂络合物在不同溶剂中进行N-异丙基丙烯酰胺的聚合反应。研究了ATRP溶剂以及聚合物纯化过程对端基稳定性的影响。质谱结果首次明确证实了通过分子内环化反应导致ω端基的损失。此外，还引入了一种基于溴化亚铜/甲基三乙烯四胺催化剂络合物的ATRP体系，该体系不仅对聚合过程具有良好的控制能力，还为N-异丙基丙烯酰胺与丙烯酸酯及其他N-取代丙烯酰胺的嵌段共聚提供了机会。通过核磁共振氢谱（H-NMR）和尺寸排阻色谱对聚合物进行了表征。通过离子淌度分离（IMS）增强的电喷雾电离飞行时间质谱（ESI-TOF）测定聚合物端基。
