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Synthesis of Poly(trimethylene carbonate) Oligomers by Ring‐Opening Polymerization in Bulk
Macromolecular Chemistry and Physics ( IF 2.5 ) Pub Date : 2020-01-29 , DOI: 10.1002/macp.201900367 Xiang Li 1, 2, 3 , Nathalie Mignard 1, 2, 3 , Mohamed Taha 1, 2, 3 , Carlos Fernández‐de‐Alba 1, 2, 4 , Jianding Chen 5 , Shengmiao Zhang 5 , Laure Fort 6 , Frédéric Becquart 1, 2, 3
Macromolecular Chemistry and Physics ( IF 2.5 ) Pub Date : 2020-01-29 , DOI: 10.1002/macp.201900367 Xiang Li 1, 2, 3 , Nathalie Mignard 1, 2, 3 , Mohamed Taha 1, 2, 3 , Carlos Fernández‐de‐Alba 1, 2, 4 , Jianding Chen 5 , Shengmiao Zhang 5 , Laure Fort 6 , Frédéric Becquart 1, 2, 3
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Telechelic poly(trimethylene carbonate) (PTMC) oligomers are synthesized and carefully characterized with molar masses between 300 and 5000 g mol−1 in bulk by ring‐opening polymerization (ROP) with 1,3‐dioxan‐2‐one (trimethylene carbonate or TMC) as monomer and 1,4‐butanediol (BDO) as co‐initiator. 1,5,7‐Triazabicyclo[4.4.0]dec‐5‐ene (TBD) organic catalyst and tin(II) bis(2‐ethylhexanoate) (Sn(Oct)2) organometallic initiator are chosen comparatively. Due to the bi‐functionality of BDO and relatively low TMC/BDO feed ratios, it is proved that PTMC chains are elaborated from one or both the BDO alcohol functions, producing two coexisting kinds of PTMC chains with BDO unit at the chain end or in the backbone. Additionally, PTMC chains bear permanent and fast exchange reactions at 100 °C, leading to both a dynamic redistribution of chains and their extension with BDO unit numbers mainly from 0‐4 but up to 6. Longer reaction times and lower TMC/BDO molar ratios bring about more predominant exchange reactions and MALDI‐TOF allows to detail the structures evolutions deeply. Better average molar masses control and narrower distributions are obtained with TBD as compared to Sn(Oct)2. PTMC molar masses can be predicted simply by the TMC/BDO feed ratio with TBD. Kinetically, TBD is the most efficient. The glass transition temperature Tg is found to respect Flory–Fox model.
中文翻译：
开环聚合本体合成聚碳酸三亚甲基酯低聚物
通过与1,3-二恶烷-2-酮（碳酸三亚甲基酯或碳酸三亚甲基酯）的开环聚合（ROP），合成并仔细表征了远螯聚碳酸三亚甲基酯（PTMC）低聚物，其摩尔质量在300至5000 g mol -1之间。TMC）作为单体，1,4-丁二醇（BDO）作为共引发剂。1,5,7-三氮杂双环[4.4.0] dec-5-烯（TBD）有机催化剂和双（2-乙基己酸）锡（II）（Sn（Oct）2）比较选择有机金属引发剂。由于BDO的双重功能和相对较低的TMC / BDO进料比，已证明PTMC链是由一种或两种BDO醇官能团精制而成的，产生了两种共存的PTMC链，在链端或链端带有BDO单元。骨干。此外，PTMC链在100°C时会发生永久和快速的交换反应，从而导致链的动态重新分布以及其BDO单元数的扩展（主要是0-4至最多6）。更长的反应时间和更低的TMC / BDO摩尔比带来更重要的交换反应，而MALDI-TOF允许深入详细地描述结构演变。与Sn（Oct）2相比，TBD具有更好的平均摩尔质量控制和更窄的分布。可以通过与TBD的TMC / BDO进料比简单地预测PTMC摩尔质量。从动力学上说，TBD是最有效的。发现玻璃化转变温度T g符合Flory-Fox模型。
更新日期：2020-01-29
中文翻译：
开环聚合本体合成聚碳酸三亚甲基酯低聚物
通过与1,3-二恶烷-2-酮（碳酸三亚甲基酯或碳酸三亚甲基酯）的开环聚合（ROP），合成并仔细表征了远螯聚碳酸三亚甲基酯（PTMC）低聚物，其摩尔质量在300至5000 g mol -1之间。TMC）作为单体，1,4-丁二醇（BDO）作为共引发剂。1,5,7-三氮杂双环[4.4.0] dec-5-烯（TBD）有机催化剂和双（2-乙基己酸）锡（II）（Sn（Oct）2）比较选择有机金属引发剂。由于BDO的双重功能和相对较低的TMC / BDO进料比，已证明PTMC链是由一种或两种BDO醇官能团精制而成的，产生了两种共存的PTMC链，在链端或链端带有BDO单元。骨干。此外，PTMC链在100°C时会发生永久和快速的交换反应，从而导致链的动态重新分布以及其BDO单元数的扩展（主要是0-4至最多6）。更长的反应时间和更低的TMC / BDO摩尔比带来更重要的交换反应，而MALDI-TOF允许深入详细地描述结构演变。与Sn（Oct）2相比，TBD具有更好的平均摩尔质量控制和更窄的分布。可以通过与TBD的TMC / BDO进料比简单地预测PTMC摩尔质量。从动力学上说，TBD是最有效的。发现玻璃化转变温度T g符合Flory-Fox模型。
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