搅拌间歇式乳液反应器中甲基丙烯酸甲酯的实验研究：ARGET ATRP法

Experimental Investigation of Methyl Methacrylate in Stirred Batch Emulsion Reactor: AGET ATRP Approach.

作者信息

Awad Mohammed, Duever Thomas, Dhib Ramdhane

机构信息

Department of Chemical Engineering, Ryerson University, 350 Victoria Street, Toronto, ON M5B 2K3, Canada.

出版信息

Materials (Basel). 2020 Dec 18;13(24):5793. doi: 10.3390/ma13245793.

DOI:10.3390/ma13245793

PMID:33353143

原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC7766881/

Abstract

This study examines the ab initio emulsion atom transfer radical polymerization (ATRP) initiated by an eco-friendly reducing agent to produce poly(methyl methacrylate) (PMMA) polymer with controlled characteristics in a 2 L stirred batch reactor. The effect of the reaction temperature, surfactant concentration, monomer to water ratio, and stirring speed was thoroughly investigated. The results showed that PMMA coagulation becomes quite severe at a certain temperature threshold. However, the coagulation could be avoided at mild reaction temperature, since the outcomes showed that loading more surfactant to the system under high mixing speed has balanced the polymer mixture and yielded high monomer conversion. The PMMA product was analyzed by gravimetry and GPC measurements and after 5 h of polymerization at a reaction temperature of 50 °C, monomer conversion of 64.1% was obtained, and PMMA polymer samples produced had an average molar mass of 4.5 kg/mol and a polydispersity index of 1.17. The structure of the PMMA polymer was successfully proved by FTIR and nuclear magnetic resonance (NMR) spectroscopy. The results confirm the living feature of MMA AGET ATRP in emulsion medium and recommend further investigation for other types of surfactant.

摘要

本研究考察了由一种环保型还原剂引发的从头算乳液原子转移自由基聚合（ATRP），以在2 L搅拌间歇式反应器中制备具有可控特性的聚甲基丙烯酸甲酯（PMMA）聚合物。深入研究了反应温度、表面活性剂浓度、单体与水的比例以及搅拌速度的影响。结果表明，在一定温度阈值下，PMMA的凝聚变得相当严重。然而，在温和的反应温度下可以避免凝聚，因为结果表明，在高混合速度下向体系中加入更多表面活性剂可使聚合物混合物达到平衡，并获得较高的单体转化率。通过重量法和凝胶渗透色谱（GPC）测量对PMMA产物进行了分析，在50℃的反应温度下聚合5 h后，单体转化率达到64.1%，所制备的PMMA聚合物样品的平均摩尔质量为4.5 kg/mol，多分散指数为1.17。通过傅里叶变换红外光谱（FTIR）和核磁共振（NMR）光谱成功证实了PMMA聚合物的结构。结果证实了甲基丙烯酸甲酯（MMA）活化剂引发的电子转移再生催化剂原子转移自由基聚合（AGET ATRP）在乳液介质中的活性特征，并建议对其他类型的表面活性剂进行进一步研究。