Miniemulsion SI-ATRP by Interfacial and Ion-Pair Catalysis for the Synthesis of Nanoparticle Brushes
Miniemulsion SI-ATRP by Interfacial and Ion-Pair Catalysis for the Synthesis of Nanoparticle Brushes
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界面和离子对催化细乳液 SI-ATRP 合成纳米颗粒刷
DOI：
10.1021/acs.macromol.2c01114
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发表时间：
2022
期刊：
影响因子：
5.5
通讯作者：
Wu, Hanshu
中科院分区：
文献类型：
--
作者：
Yin, Rongguan;Chmielarz, Paweł;Zaborniak, Izabela;Zhao, Yuqi;Szczepaniak, Grzegorz;Wang, Zongyu;Liu, Tong;Wang, Yi;Sun, Mingkang;Wu, Hanshu
以抗坏血酸（AsAc）为还原剂，丙烯酸正丁酯（BA）为单体，在离子对和界面催化作用下，通过电子转移（SI-ARGET）原子转移自由基聚合（ATRP）再生的表面引发剂，在细乳液（流体力学粒径为105 ~ 128 nm）中合成了致密接枝聚合物/无机纳米粒子杂化材料。在分散介质中使用单一催化剂体系允许使用非常低的催化剂负载（相对于单体低至100 ppm的[Br-CuII（L）]+）制备杂化材料，并获得高单体转化率（高达70%）而没有宏观凝胶化。所得聚合物表现出窄的分子量分布（Mw ≤ 1.31），并且聚合物接枝的纳米颗粒表现出优异的尺寸均匀性。在有机溶剂（例如，四氢呋喃）是稳定的，没有任何颗粒聚集。随后用丙烯酸叔丁酯（tBA）对颗粒刷进行扩链，证明了聚合的活性和链端保真度的高保留。开发的细乳液SI-ARGET ATRP技术与界面和离子对催化提供了许多优势，为传统的疏水ATRP过程中的纳米粒子刷的制备。这些包括高单体转化率、高接枝密度、对聚合速率的更好控制、高链端活性和使用非常少量的铜催化剂。
Densely grafted polymer/inorganic nanoparticle hybrids were synthesizedviaa surface-initiated activator regenerated by electron transfer (SI-ARGET) atom transfer radical polymerization (ATRP) ofn-butyl acrylate (BA) under ion-pair and interfacial catalysis in miniemulsion (hydrodynamic diameters from 105 to 128 nm) with ascorbic acid (AsAc) as the reducing agent. The use of a single-catalyst system in dispersed media allowed the preparation of hybrid materials using a very low catalyst loading (as low as 100 ppm of [Br-CuII(L)]+relative to monomer) and obtaining high monomer conversion (up to 70%) without macroscopic gelation. The resulting polymers exhibited narrow molecular weight distributions (Đ≤ 1.31), and the polymer-grafted nanoparticles showed excellent size uniformity. Dispersions in organic solvents (e.g., tetrahydrofuran) were stable without any particle aggregations. Subsequent chain extension of the particle brushes withtert-butyl acrylate (tBA) proved the livingness of the polymerization and high retention of chain-end fidelity. The developed miniemulsion SI-ARGET ATRP technique with interfacial and ion-pair catalysis offers numerous advantages for the preparation of nanoparticle brushes over the traditional hydrophobic ATRP process. These include a high monomer conversion, high grafting density, better control over polymerization rate, high chain-end livingness, and the use of a very low amount of copper catalyst.
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