硅胶固定化季铵SO_3H型离子液体的合成与性能  

Synthesis and Properties of Silica-immobilized Quaternary Ammonium SO_3H Acidic Ionic Liquids

作　　者：刘春萍[1] 刘刚[1] 孙琳[1] 温全武[1] 刘军深[1] 胡玉才[1] 

机构地区：[1]鲁东大学化学与材料科学学院,山东烟台264025

出　　处：《鲁东大学学报（自然科学版）》2009年第4期356-360,365,共6页Journal of Ludong University:Natural Science Edition

基　　金：山东省优秀中青年科学家奖励基金(2004BS08001);鲁东大学自然科学基金(20052902)

摘　　要：以硅胶为载体,γ-氯丙基三乙氧基硅烷(NQ-53)为偶联剂,哌啶和1,4-丁烷磺内酯为反应性功能基,p-CH3PhSO3H,CF3COOH,H2SO4和HBF4为质子酸,设计合成了4种新型硅胶固定化季铵SO3H型酸性离子液体.分别经红外光谱、元素分析和TG分析测定了离子液体的功能基结构和稳定性,并用紫外光谱法测定了其Hamm ett酸度.初步探讨了H+促进下4种离子液体对合成乙酸异戊酯的催化性能.结果表明,酸性离子液体的Hamm ett酸度函数H0在0.67—0.82,酯化反应体系中若有少量无机酸的参与,可有效地提高乙酸异戊酯的收率,反应体系中加入1.0 g离子液体和1.0 mL浓盐酸,乙酸异戊酯的收率为67.7%,比采用盐酸或离子液体单组分催化时酯的产率提高了20%—40%.该合成方法操作简单,产物与离子液体容易分离,离子液体可重复利用.Four novel silica-immobilized quaternary ammonium acidic ionic liquids were synthesized using silica gel as a vector,γ-chloropropyltriethoxysilane（NQ-53） as a coupler,piperidine and 1,4-butanesultone as functional substrates and p-CH3PhSO3H,CF3COOH,H2SO4,HBF4 as proton donor.Their structure,thermal stability and Hammett acidity were determined by FTIR,element analysis,TG analysis and UV spectrum,respectively.The catalytic esterification efficiency of the ionic liquids promoted by H＋ was preliminarily studied under different conditions.The results showed that Hammett acidity function H0 of the four acidic ionic liquids were between 0.67—0.82;the yield of isoamyl acetate increased efficiently when the ionic liquid was added along with a small quantity of inorganic acid.The yield of isoamyl acetate was 67.7% when 1.0 g the ionic liquid and 1.0 mL 37%HCl were applied.Compared with catalysis efficiency by using ionic liquids or inorganic acid alone,the yield of isomyl acetate increased by 20%—40%.The esterification product could be easily separated by simple phase separation.In addition,the ionic liquids can be reused.

关 键 词：酸性离子液体 硅胶固定化 Hammett酸度 酯化反应 

分 类 号：TQ426.6[化学工程]