Synthesis of β‐myrcene/glycidyl methacrylate statistical and amphiphilic diblock copolymers by SG1 nitroxide‐mediated controlled radical polymerization,Journal of Polymer Science Part A: Polymer Chemistry

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Synthesis of β‐myrcene/glycidyl methacrylate statistical and amphiphilic diblock copolymers by SG1 nitroxide‐mediated controlled radical polymerization
Journal of Polymer Science Part A: Polymer Chemistry Pub Date : 2018-02-07 , DOI: 10.1002/pola.28963
Adrien Métafiot _{1,

2,

3} , Jean-François Gérard ₁ , Brigitte Defoort ₂ , Milan Marić ₃

Affiliation

Bulk nitroxide‐mediated polymerization (NMP) of β‐myrcene (My)/glycidyl methacrylate (GMA) mixtures with varying GMA molar feed fraction (f_GMA,0 = 0.10–0.91) was accomplished at 120 °C, initiated by SG1‐based alkoxyamine bearing a N‐succinimidyl ester group (NHS‐BlocBuilder). Low dispersity My/GMA copolymers (Đ < 1.56) with slight number‐average molecular weights (M_ns) deviations from predicted values (M_n,theo with M_n/M_n,theo > 70%) were obtained. The copolymerization was revealed to be statistical, confirmed via Fineman–Ross (r_My = 0.80 ± 0.31 and r_GMA = 0.71 ± 0.15) and Kelen‐Tüdös (r_My = 0.48 ± 0.12 and r_GMA = 0.53 ± 0.18) approaches. Glass transition temperature (T_g) of the statistical P(My‐stat‐GMA)s increased from −77 to +43 °C as the GMA molar fraction incorporated (F_GMA) increased from 0.10 to 0.90. High SG1 chain‐end fidelity for My‐rich and GMA‐rich P(My‐stat‐GMA)s was assessed by phosphorus nuclear magnetic resonance (³¹P NMR, SG1 fraction >69 mol %) and chain‐extensions in toluene with My, GMA and styrene (S) (monomodal shift in M_n). Last, diblock P(My‐b‐GMA) was made and treated with morpholine to produce amphiphilic copolymer able to self‐organize into micelles. © 2018 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2018, 56, 860–878

中文翻译：

SG1硝基氧介导的受控自由基聚合反应合成β-月桂烯/甲基丙烯酸缩水甘油酯统计和两亲性二嵌段共聚物

基于SG1的引发，在120°C下完成了具有不同GMA摩尔进料分数（f _GMA，0 = 0.10–0.91 ）的β-月桂烯（My）/甲基丙烯酸缩水甘油酯（GMA）混合物的本体氮氧化物介导聚合（NMP）。带有N-琥珀酰亚胺基酯基的烷氧基胺（NHS-BlocBuilder）。低分散度我/ GMA共聚物（Đ <1.56）有轻微的数均分子量（中号_Ñ为s）从预测值偏差（中号_N，西奥与中号_ñ /中号_N，西奥 > 70％）获得。通过Fineman-Ross（r _My = 0.80±0.31和r _GMA = 0.71±0.15）和Kelen‐Tüdös（r _My = 0.48±0.12和r _GMA = 0.53±0.18）方法。玻璃化转变温度（Ť_克统计P的）（我的- STAT -GMA）s增加到从-77至+43℃，作为结合（该GMA摩尔分数˚F _GMA）从0.10提高到0.90。高SG1链末端保真度我的富和GMA-P-富含（我的- STAT -GMA）类是由磷核磁共振（评估³¹ P NMR，SG1分数> 69摩尔％）和链扩展的甲苯与我的，GMA和苯乙烯（S）（以单峰移中号_Ñ）。最后，制得二嵌段P（My - b- GMA）并用吗啉处理，以产生能够自组织成胶束的两亲共聚物。©2018 Wiley Periodicals，Inc.J.Polym。科学，A部分：Polym。化学 2018，56，860-878

更新日期：2018-02-07

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