离子液体中电化学介导的ATRP：[BMIm] [OTf]中丙烯酸甲酯的受控聚合<a href="#fn1" title="现有电子补充信息（ESI）：实验细节，ILs和乙腈中eATRP的比较，恒电流eATRP以及纯化和回收的ILs的表征。参见DOI：10.1039 / c7py02134h">†</a>,Polymer Chemistry

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离子液体中电化学介导的ATRP：[BMIm] [OTf]中丙烯酸甲酯的受控聚合 †
Polymer Chemistry ( IF 4.1 ) Pub Date : 2018-01-09 00:00:00 , DOI: 10.1039/c7py02134h
Francesco De Bon _{1,

2,

3,

4} , Marco Fantin _{5,

6,

7,

8} , Abdirisak A. Isse _{1,

2,

3,

4} , Armando Gennaro _{1,

2,

3,

4}

Affiliation

丙烯酸甲酯（MA）的电化学介导的原子转移自由基聚合（e ATRP）首次在离子液体1-丁基-3-甲基咪唑鎓三氟甲磺酸盐（[BMIm] [OTf]）中进行。离子液体是特别适合用作溶剂ëATRP是因为（i）不需要支持电解质，（ii）聚合物的纯化很简单，并且（iii）催化剂可以循环使用，并保持其大部分原始活性。聚合反应相对较快且控制得当，可在2小时内以> 90％的转化率提供约1.1分散度的聚合物。探索了不同的条件，包括施加的电势，施加的电流，温度，单体/溶剂比，目标聚合度（从276到828）和催化剂负载（低至45 ppm）。通过实现电化学开关（开/关切换）以及通过聚（丙烯酸甲酯）-Br与丙烯腈的扩链来确认MA聚合的活性。首次通过“催化卤素交换”进行扩链，即使用180 ppm的铜络合物将链端从C–Br转化为C–Cl。这提供了良好控制的聚（丙烯酸甲酯）-b-聚（丙烯腈）-Cl共聚物。

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Electrochemically mediated ATRP in ionic liquids: controlled polymerization of methyl acrylate in [BMIm][OTf]†

Electrochemically mediated atom transfer radical polymerization (eATRP) of methyl acrylate (MA) was carried out for the first time in an ionic liquid, 1-butyl-3-methylimidazolium trifluoromethanesulfonate ([BMIm][OTf]). Ionic liquids are particularly suitable as solvents for eATRP because (i) a supporting electrolyte is not required, (ii) purification of the polymer is simple, and (iii) the catalyst can be recycled maintaining most of its original activity. Polymerization was relatively fast and well-controlled, affording polymers with a dispersity of ∼1.1 at >90% conversion in 2 h. Different conditions were explored, including applied potential, applied current, temperature, the monomer/solvent ratio, targeted degree of polymerization (from 276 to 828), and catalyst loading (down to 45 ppm). The livingness of MA polymerization was confirmed by realizing an electrochemical switch (ON/OFF toggling) and by the chain extension of poly(methyl acrylate)-Br with acrylonitrile. Chain extension was carried out for the first time by a “catalytic halogen exchange”, i.e. 180 ppm of a Cu complex was used to convert the chain end from C–Br to C–Cl. This afforded a well-controlled poly(methyl acrylate)-b-poly(acrylonitrile)-Cl copolymer.

更新日期：2018-01-09

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