This study investigates the ab initio atom transfer radical polymerization of butyl methacrylate using activator generated by electron transfer in a well-mixed 2 L emulsion reactor. A first time reported polymerization system initiates by a catalyst complex with hexamethylenetetramine as a ligand and in presence of sodium dodecyl sulfate as an anionic surfactant. The system shows a relatively low monomer conversion rate of 14% and a controlled number average molecular weight (M_n) of 8 kg mol⁻¹ with a polydispersity index (Ð) of 1.24 for 2 h reaction time. A statistical design of experiments is followed to study the effects of reaction temperature, surfactant amount, stirring speed, and ligand amount to assess their impact on the monomer conversion, M_n, and Ð. A fractional factorial with a resolution IV design is adopted and an empirical regression model is developed from eight experimental trials. The results tell that the reaction temperature has the greatest influential on the process outputs. Also, the surfactant amount and stirring speed strongly affect the conversion rate, while the ligand amount strongly affects the M_n and Ð. The results also show that the temperature–surfactant interaction is the most significant on the conversion rate and M_n.

中文翻译：

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甲基丙烯酸丁酯AGET ATRP在搅拌乳液反应器中的实验筛选设计

本研究在充分混合的 2 L 乳液反应器中使用由电子转移产生的活化剂研究甲基丙烯酸丁酯的从头原子转移自由基聚合。首次报道的聚合体系是通过以六亚甲基四胺作为配体并在十二烷基硫酸钠作为阴离子表面活性剂存在下的催化剂络合物引发的。该系统显示出 14% 的相对较低的单体转化率和8 kg mol ^-1的受控数均分子量 ( Mn )，具有多分散性指数 ( _D) 为 1.24，反应时间为 2 小时。遵循实验的统计设计来研究反应温度、表面活性剂用量、搅拌速度和配体量的影响，以评估它们对单体转化率、Mn和_D的影响。采用具有分辨率 IV 设计的部分因子，并从 8 个实验试验中开发了一个经验回归模型。结果表明，反应温度对工艺产出的影响最大。此外，表面活性剂用量和搅拌速度对转化率有很大影响，而配体量对M _n和D 有很大影响. 结果还表明，温度-表面活性剂的相互作用对转化率和M _n最显着。