In-situ IR Monitoring the Synthesis of Amphiphilic Copolymery P(HEMA-co-tBMA) via ARGET ATRP  

原位红外跟踪ARGETATRP合成两亲共聚物P(HEMA-co-tBMA)(英文)

作　　者：林文静 杨友强 陈锐毫 文秀芳 钱宇 蔡成志 章莉娟 

机构地区：[1]School of Chemistry and Chemical Engineering,South China University of Technology [2]Department of Chemistry & Center for Materials Chemistry,University of Houston

出　　处：《Chinese Journal of Chemical Engineering》2014年第9期1046-1054,共9页中国化学工程学报（英文版）

基　　金：Supported by the National Natural Science Foundation of China(21176090,21136003);Team Project of Natural Science Foundation of Guangdong Province(S2011030001366);Science and Technology Foundation of Guangdong Province(2012B050600010);Fundamental Research Funds for the Central Universities(2013ZP0010)

摘　　要：The amphiphilic copolymer poly（hydroxyethyl methacrylate-co-tert-butyl methacrylate） [P（HEMA-co-tBMA）] was synthesized by activators regenerated by electron transfer atom transfer radical polymerization （ARGET ATRP）, with the synthesis process monitored by in-situ infrared spectroscopy （IR）. The molecular weight, chem- ical structure and characteristics of the copolymer were determined by 1H NMR, gas chromatography and gel permeation chromatography. The influences of various parameters on the living polymerization were explored. The molecular weight of the copolymer with narrow molecular weight distribution （Mw/Mn 〈 1.50） increases ap- proximately linearly with the monomer conversion, indicating a good control of polymerization. In the reaction temperature range from 50 ℃ to 90 ℃, the monomer conversion is higher at 60 ℃. The tBMA conversion rate decreases gradually with the increase of tBMA content, while the HEMA conversion is hardly affected by HEMA content. Weak polar solvent is more favorable to the polymerization compared to polar solvent. The molar ratio of reducing agent to catalyst has significant effect on the polymerization and increasing the amount of reducing agent will accelerate the reaction rate but causes wider molecular weight distribution. It is indicated that in-situ IR monitoring contributes to a more in-depth understanding of the mechanism of methacrylate monomer copolymerization.The amphiphilic copolymer poly(hydroxyethyl methacrylate-co-tert-butyl methacrylate) [P(HEMA-co-tBMA)]was synthesized by activators regenerated by electron transfer atom transfer radical polymerization(ARGET ATRP), with the synthesis process monitored by in-situ infrared spectroscopy(IR). The molecular weight, chemical structure and characteristics of the copolymer were determined by1 H NMR, gas chromatography and gel permeation chromatography. The influences of various parameters on the living polymerization were explored.The molecular weight of the copolymer with narrow molecular weight distribution(Mw/Mnb 1.50) increases approximately linearly with the monomer conversion, indicating a good control of polymerization. In the reaction temperature range from 50 °C to 90 °C, the monomer conversion is higher at 60 °C. The tBMA conversion rate decreases gradually with the increase of tBMA content, while the HEMA conversion is hardly affected by HEMA content. Weak polar solvent is more favorable to the polymerization compared to polar solvent. The molar ratio of reducing agent to catalyst has significant effect on the polymerization and increasing the amount of reducing agent will accelerate the reaction rate but causes wider molecular weight distribution. It is indicated that in-situ IR monitoring contributes to a more in-depth understanding of the mechanism of methacrylate monomer copolymerization.

关 键 词：ln-sltu IR monitoringAmphiphilic copolymerARGET ATRPConversion rate 

分 类 号：O631.5[理学—高分子化学] O657.33[理学—化学]