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首页> 外文期刊>Journal of Macromolecular Science. Pure and Applied Chemistry >Synthesis and Characterization of Four-Arm Star Poly(epsilon-caprolactone)-Block-Poly(cyclic-carbonate methacrylate) Copolymers by Combining Ring-Opening Polymerization With Atom Transfer Radical Polymerization
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Synthesis and Characterization of Four-Arm Star Poly(epsilon-caprolactone)-Block-Poly(cyclic-carbonate methacrylate) Copolymers by Combining Ring-Opening Polymerization With Atom Transfer Radical Polymerization

机译：开环聚合与原子转移自由基聚合相结合的四臂星形聚（ε-己内酯）-嵌段-聚（甲基丙烯酸环碳酸酯）共聚物的合成与表征

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摘要

Well-defined four-arm star poly(epsilon-caprolactone)-block-poly(cyclic carbonate methacrylate) (PCL-b-PCCMA) copolymers were synthesized by combining ring-opening polymerization (ROP) with atom transfer radical polymerization (ATRP). First, a four-arm poly(epsilon-caprolactone) (PCL) macroinitiator [(PCL-Br)(4)] was prepared by the ROP of epsilon-CL catalyzed by stannous octoate at 110 degrees C in the presence of pentaerythritol as the tetrafunctional initiator followed by esterification with 2-bromoisobutyryl bromide. The sequential ATRP of CCMA monomer was carried out by using the (PCL-Br)(4) tetrafunctional macroinitiator (MI) and in the presence of CuBr/2, 2 '-bipyridyl system in DMF at 80 degrees C with [(MI)]:[CuBr]:[bipyridyl] = 1:1:3 to yield block polymers with controlled molecular weights (M-n (NMR) = 10700 to 27300g/mol) by varying block lengths and with moderately narrow polydispersities (M-w/M-n = 1.2-1.4). Block copolymers with different PCL: PCCMA copolymer composition such as 50:50, 70:30 and 74:26 were prepared with good yields (48-74%). All these block copolymers were well characterized by NMR, FTIR and GPC and tested their thermal properties by DSC and TGA.
机译：通过将开环聚合（ROP）与原子转移自由基聚合（ATRP）结合，合成了定义明确的四臂星形聚（ε-己内酯）-嵌段-聚（甲基丙烯酸环状碳酸酯）（PCL-b-PCCMA）共聚物。首先，在季戊四醇的存在下，辛酸亚锡在110℃下由RO催化的epsilon-CL的ROP制备了四臂聚ε-己内酯（PCL）大分子引发剂[（PCL-Br）（4）]。四官能引发剂，然后用2-溴异丁酰溴进行酯化。 CCMA单体的顺序ATRP是通过使用（PCL-Br）（4）四官能大分子引发剂（MI）并在CuBr / 2，2'-联吡啶系统存在下于80°C在DMF中与[（MI） ]：[CuBr]：[联吡啶基] = 1：1：3，通过改变嵌段长度和适度窄的多分散性（Mw / Mn = 1.2），可制得分子量可控制的嵌段聚合物（Mn（NMR）= 10700至27300g / mol） -1.4）。以良好的产率（48-74％）制备具有不同的PCL：PCCMA共聚物组成例如50∶50、70∶30和74∶26的嵌段共聚物。所有这些嵌段共聚物均已通过NMR，FTIR和GPC很好地表征，并通过DSC和TGA测试了它们的热性能。

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