用于ATRP反应体系的配位离子液体的合成

Synthesis of coordinated ionic liquids for ATRP reaction system

在微波反应器中通过有机多胺与氯化1-氯乙基-3-甲基咪唑离子液体[Ce MIM]Cl的烷基化反应,合成了具有配位功能离子液体[N3MIM]Cl,以替换传统的有机配体,与催化剂Cu Br配位形成催化体系,催化离子液体中的原子转移自由基聚合(ATRP)。研究了反应工艺对离子液体合成的影响,结果发现采用微波反应器加热,反应时间短,产物收率高。当反应物配比1.5:1、反应温度为75℃、微波反应3 h时,产物[N3MIM]Cl的收率达98.6%。采用电喷雾质谱和红外光谱测定离子液体结构,证明该离子液体为[N3MIM]Cl。将所合成配位离子液体替代有机配体,用于离子液体中MMA的ATRP反应,结果表明:配位离子液体可提高催化剂在离子液体中的溶解性,使过渡金属催化剂容易与聚合产物分离。

The coordination function of ionic liquids [N3MIM]Cl was prepared by the alkylation reaction of organic polyamines and 1-chloro-ethyl-3-methyl chloride ionic liquid [CeMIM]Cl using a microwave reactor. The functionalized ionic liquids can form catalytic system with CuBr, replacing traditional organic ligands, in atom transfer radical polymerization (ATRP) reaction where ionic liquids was used as reaction medium. The effects of reaction conditions on the yield of ionic liquids have been studied. The results showed that the reaction time was short with higher yield using the microwave reactor. The yield of product [N3MIM]Cl was 98.6% when the reactant ratio was 1.5:1, the reaction temperature was 75℃ and microwave reaction time was 3 h. Electrospray ionization mass spectrometry and IR were used to determine the structures of ionic liquids [N3MIM]Cl. The coordinated ionic liquid that would replace of organic ligand was used in the ATRP of MMA in ionic liquids. The results showed that: the coordination function of ionic liquid can increase the solubility of the catalyst in the ionic liquids, so that the transition metal catalyst is easily separated from the polymer product.