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Precision AABB-type cyclocopolymers via alternating cyclocopolymerization of disiloxane-tethered divinyl monomers
Polymer Chemistry ( IF 4.1 ) Pub Date : 2019/12/20 , DOI: 10.1039/c9py01748h Jun Lu 1, 2, 3, 4, 5 , Junjiang Li 1, 2, 3, 4, 5 , Jinghang Wang 1, 2, 3, 4, 5 , Min Du 1, 2, 3, 4, 5 , Hewen Liu 1, 2, 3, 4, 5
Polymer Chemistry ( IF 4.1 ) Pub Date : 2019/12/20 , DOI: 10.1039/c9py01748h Jun Lu 1, 2, 3, 4, 5 , Junjiang Li 1, 2, 3, 4, 5 , Jinghang Wang 1, 2, 3, 4, 5 , Min Du 1, 2, 3, 4, 5 , Hewen Liu 1, 2, 3, 4, 5
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Attempts to synthesize copolymers with structural sophistication and precision still remain elusive. Here, we report a facile synthesis of a new type of precision cyclocopolymer containing an AABB-type repeating chain sequence via the free radical cyclopolymerization of divinyl monomers bMA and bSt in the presence of ZnCl2. RAFT polymerization conditions can afford the AABB-type alternating cyclocopolymers with controlled molecular weight and narrow polydispersity. Kinetic research on the cyclocopolymerization shows that bMA and bSt polymerize in an equimolar ratio during the ZnCl2-modulated RAFT copolymerization process. The AABB-type alternating structures are verified by 2D 1H–13C COSY techniques and MALDI-TOF MS. The main-chain CH or CH2 NMR signals (both 1H and 13C NMR) in the cyclocopolymers suggest a chain sequence of a high order, and prove the absence of either the homopolymer structures or the intersecting ABAB-type structure. MALDI-TOF MS shows that the cyclocopolymer has a regularly repeating structure and a uniform repeating unit. In the absence of ZnCl2, bMA prefers to homopolymerize. Our work shows that the alternating cyclocopolymerization is a facile route to afford cyclocopolymers with a precision chain sequence and group spacing.
中文翻译：
通过二硅氧烷系链的二乙烯基单体的交替环共聚反应来制备精密AABB型环共聚物
合成具有结构复杂性和精确度的共聚物的尝试仍然难以实现。在这里，我们报告了通过在ZnCl 2存在下通过二乙烯基单体bMA和bSt的自由基环聚合反应，轻松合成一种新型AABB型精密环共聚物的过程。RAFT聚合条件可以提供具有可控的分子量和窄的多分散性的AABB型交替环共聚物。对环共聚的动力学研究表明，在ZnCl 2调节的RAFT共聚过程中，bMA和bSt以等摩尔比聚合。AABB型交替结构已通过2D 1 H– 13验证C舒适技术和MALDI-TOF MS。环状共聚物中的主链CH或CH 2 NMR信号（1 H和13 C NMR）均显示出高阶的链序列，并证明既没有均聚物结构也没有相交的ABAB型结构。MALDI-TOF MS表明该环共聚物具有规则的重复结构和均匀的重复单元。在没有ZnCl 2的情况下，bMA倾向于均聚。我们的工作表明，交替进行的环状共聚是提供具有精确链序列和基团间距的环状共聚物的便捷途径。
更新日期：2020-02-13
中文翻译：
通过二硅氧烷系链的二乙烯基单体的交替环共聚反应来制备精密AABB型环共聚物
合成具有结构复杂性和精确度的共聚物的尝试仍然难以实现。在这里，我们报告了通过在ZnCl 2存在下通过二乙烯基单体bMA和bSt的自由基环聚合反应，轻松合成一种新型AABB型精密环共聚物的过程。RAFT聚合条件可以提供具有可控的分子量和窄的多分散性的AABB型交替环共聚物。对环共聚的动力学研究表明，在ZnCl 2调节的RAFT共聚过程中，bMA和bSt以等摩尔比聚合。AABB型交替结构已通过2D 1 H– 13验证C舒适技术和MALDI-TOF MS。环状共聚物中的主链CH或CH 2 NMR信号（1 H和13 C NMR）均显示出高阶的链序列，并证明既没有均聚物结构也没有相交的ABAB型结构。MALDI-TOF MS表明该环共聚物具有规则的重复结构和均匀的重复单元。在没有ZnCl 2的情况下，bMA倾向于均聚。我们的工作表明，交替进行的环状共聚是提供具有精确链序列和基团间距的环状共聚物的便捷途径。
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