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Synthesis and characterization of poly(n-butyl methacrylate)-b-polystyrene diblock copolymers by atom transfer radical emulsion polymerization

机译:原子转移自由基乳液聚合聚聚(甲基丙烯酸正丁酯)-b-聚苯乙烯二嵌段共聚物的合成与表征

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摘要

Poly(n-butyl methacrylate) (PBMA)-b-polystyrene (PSt) diblock copolymers were synthesized by emulsion atom transfer radical polymerization (ATRP). PBMA macroinitiators that contained alkyl bromide end groups were obtained by the emulsion ATRP of n-butyl methacrylate with BrCH3CHCOOC2H5 as the initiator; these were used to initiate the ATRP of styrene (St). The latter procedure was carried out at 85 degreesC with CuCl/4,4'-di(5-nonyl)2,2'-bipyridine as the catalyst and polyoxyethylene(23) lauryl ether as the surfactant. With this technique, PBMA-b-PSt diblock copolymers were synthesized. The polymerization was nearly controlled; the ATRP of St from the macroinitiators showed linear increases in number-average molecular weight with conversion. The block copolymers were characterized with IR spectroscopy, H-1-NMR, and differential scanning calorimetry. The effects of the molecular weight of the macroinitiators, macroinitiator concentration, catalyst concentration, surfactant concentration, and temperature on the polymerization were also investigated. Thermodynamic data and activation parameters for the ATRP are also reported. (c) 2005 Wiley Periodicals, Inc.
机译:采用乳液原子转移自由基聚合(ATRP)合成了聚甲基丙烯酸正丁酯(PBMA)-b-聚苯乙烯(PSt)二嵌段共聚物。以BrCH3CHCOOC2H5为引发剂,采用甲基丙烯酸正丁酯乳液ATRP制得含有烷基溴末端基团的PBMA宏引发剂;这些用于启动苯乙烯(St)的ATRP。后一过程在85°C下进行,以CuCl/4,4'-二(5-壬基)2,2'-联吡啶为催化剂,聚氧乙烯(23)十二烷基醚为表面活性剂。利用该技术合成了PBMA-b-PSt二嵌段共聚物。聚合几乎得到控制;来自宏引发剂的St的ATRP显示,数均分子量随转化呈线性增加。采用红外光谱、H-1-NMR和差示扫描量热法对嵌段共聚物进行了表征。还研究了大引发剂分子量、大引发剂浓度、催化剂浓度、表面活性剂浓度和温度对聚合反应的影响。还报告了ATRP的热力学数据和活化参数。(c) 2005 Wiley Periodicals, Inc.

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