摘要
以N-甲基咪唑为骨架引入1,2-二氯乙烷合成中间体——氯化1-氯乙基-3-甲基咪唑([CeMIM]Cl),再与三乙烯四胺反应合成了氯化1-(三乙基四氨基)乙基-3-甲基咪唑([N_4MIM]Cl)离子液体。通过FTIR、1HNMR对[N_4MIM]Cl进行表征,确证了[N_4MIM]Cl的化学结构。通过循环伏安法测得[N_4MIM]Cl具有较低的氧化还原电势,E1/2为-0.472 V,与有机配体相比,[N_4MIM]Cl具有较好的配位性能。将[N_4MIM]Cl与Cu Br配位用于催化氯化1-烯丙基-3-甲基咪唑离子液体([AMIM]Cl)体系中甲基丙烯酸甲酯(MMA)的原子转移自由基聚合(ATRP)反应,经凝胶渗透色谱法(GPC)测试证明,[N_4MIM]Cl对ATRP反应具有较好的可控性。原子吸收光谱(AAS)测定聚合产物聚甲基丙烯酸甲酯(PMMA)中Cu^(2+)的残留量仅为360 mg/kg。
1-Chloro-ethyl-3-methylimidazolium chloride（[Ce MIM]Cl） was prepared from Nmethylimidazole with 1,2-dichloroethane followed by reacting with triethylenetetramine to afford 1-（triethyl tetramine） ethyl-3-methyl imidazolium chloride（[N_4MIM]Cl） ionic liquid. The chemical structure of [N_4MIM]Cl was confirmed by FTIR and ~1HNMR. [N_4MIM]Cl possessed a lower redox potential by using cyclic voltammetry（CV）,and E1/2was-0. 472 V,which indicated that [N_4MIM]Cl presented a more perfect coordination property than organic ligands. Subsequently,the coordination complex of [N_4MIM]Cl with Cu Br was used as a catalyst for the atom transfer radical polymerization（ATRP） of methyl methacrylate（MMA） in 1-allyl-3-methylimidazolium chloride（[AMIM]Cl）. The result,using gel permeation chromatography（GPC）,revealed that the coordination ionic liquid[N_4MIM]Cl exhibited an excellent control over the ATRP reaction. In addition,the residue of Cu^（2＋）in polymethyl methacrylate（PMMA） was only 360 mg/kg by atomic absorption spectrometry（AAS）determination. As a result,[N_4MIM]Cl was conducive to the separation of catalyst and polymerization product compared with the traditional organic ligands.
作者
薛腾
杜煌
周剑
唐二军
刘少杰
赵地顺
XUE Teng DU Huang ZHOU Jian TANG Er-jun LIU Shao-jie ZHAO Di-shun(College of Chemical and Pharmaceutical Engineering, Hebei University of Science and Technology, Shijiazhuang 050018,Hebei, China Hebei Research Center of Pharmaceutical and Chemical Engineering, Shijiazhuang 050018, Hebei, China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2017年第7期804-809,共6页
Fine Chemicals
基金
国家自然科学基金(21304030)
河北省自然科学基金项目(B2013208183)~~
关键词
配位离子液体
原子转移自由基聚合(ATRP)
配位性能
催化技术
coordination ionic liquids
atom transfer radical polymerization（ATRP）
coordination property
catalysis technology
