Center for Soft Matter Research, Department of Physics, New York University, 4 Washington Place, New York, New York 10003, United States.
Langmuir. 2010 Dec 7;26(23):17989-96. doi: 10.1021/la1034917. Epub 2010 Nov 8.
Polymeric stabilizers are an essential ingredient for the dispersion polymerization of poly(methyl methacrylate) (PMMA) in nonpolar media. In this contribution, we focus on the synthesis of an amphipathic copolymer consisting of pendant poly(12-hydroxystearic acid) (PHS) chains grafted to an insoluble PMMA backbone. This type of steric stabilizer is well established and capable of producing spherically shaped, monodisperse PMMA colloids. Unfortunately, the comb-graft copolymer is not available commercially; furthermore, the multistep synthesis of the desired stabilizer has proven challenging to reproduce. We discuss the practical matter of preparing PHS-graft-PMMA, and report specific techniques developed over several years in our lab. Gel permeation chromatography, mass spectroscopy, and end group analysis of the stabilizer and the precursor macromonomer reveal important, previously unreported details about the chemical synthesis. Our protocol is reproducible and resulted in the production of low polydispersity PMMA particles.
聚合物稳定剂是分散聚合聚甲基丙烯酸甲酯（PMMA）在非极性介质中的重要组成部分。在本研究中，我们专注于合成一种两亲性嵌段共聚物，该共聚物由接枝在不溶性 PMMA 主链上的支化聚（12-羟基硬脂酸）（PHS）链组成。这种空间位阻稳定剂已经得到了很好的应用，能够制备出球形、单分散的 PMMA 胶体。不幸的是，梳状接枝共聚物目前还没有商业化供应；此外，所需稳定剂的多步合成难以重现。我们讨论了制备 PHS 接枝 PMMA 的实际问题，并报告了我们实验室多年来开发的具体技术。稳定剂和前体大分子单体的凝胶渗透色谱、质谱和端基分析揭示了关于化学合成的重要、以前未报道的细节。我们的方案是可重复的，并产生了低多分散性的 PMMA 颗粒。
