论文总字数：19099字

摘 要

离子液体是由有机阳离子与有机或者无机阴离子组成的,在室温或接近室温下呈现液态的盐,具有不易挥发、导电性强、黏度大、可设计性、良好的溶解性等优点。此外，离子液体在分离和纯化、废旧化合物的回收、废气中二氧化碳的提取等方面也显示出了应用前景。

本课题主要通过加热回流法两步合成目标离子液体，第一步通过季铵化反应制备出含目标阳离子的卤盐；第二步再用目标阴离子置换出卤素阴离子从而反应得到目标离子液体。通过对合成产物进行核磁、紫外的检测，对其结构进行表征和分析。实验结果表明：在80℃、1-甲基咪唑：氯（溴）代正丁烷为1:1.1时、乙腈为溶剂加热回流48h，产率分别为72.90%和89.96%；在65℃、[bmim]Cl: NaBF₄和[bmim]Br:KPF₆为1:1.1时，分别以丙酮和蒸馏水为溶剂加热回流12小时，产率各为91.67%、83.62%。课题的目的在于通过改变反应条件寻找到合成离子液体的最佳组合条件，并为开发新型的离子液体提供宝贵的经验，具有重要的研究意义和应用价值。

关键词：咪唑类离子液体；合成；表征

Abstract

Ionic liquids are composed of organic cation and inorganic or organic anion. It’s kinds of liquid salt at room temperature or approximately. Ionic liquids have many advantages, such as less volatile, strong electrical conductivity and large viscosity, designed and good solubility. Meanwhile, Ionic liquids have prospect of potential application, separation and purification of substance, reclycling of waste compounds, extraction of carbon dioxide in industrial waste gases.

The main product was mainly made by the two -step reaction and heating reflux. The first step is to get halide salt including target cation by quaternary ammoniation reaction. And the second step is that halogen ions is substituted by target anion to get target ionic liquids. In order to characterize and analyze its structure, product was the first characterize by ultraviolet and NMR. This is the result. 1 molar equivalent of 1-methyl imidazole was dissolved in acetonitrile, charged with 1.1 molar equivalent of halogenated n-butane, and heated to reflux for 48 hours at 80℃. The yield of 1-butyl-3-methylimidazolium chloride ([bmim]Cl) is 72.9% and 1-butyl-3-methylimidazolium bromide ([bmim]Br) is 89.96%.1 molar equivalent of [bmim] Br was dissolved in distilled water, charged with 1.1 molar equivalent of potassium hexafluorophosphat, and heated to reflux for 12 hours at room temperature.1 molar equivalent of [bmim]Cl was dissolved in acetone, charged with 1.1 molar equivalent of sodium tetrafluorobrate, and heated to reflux for 12 hours at room temperature. The yield of 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim][PF6]) is 83.62% and 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF4]) is 91.67%. The purpose of our project is to find the best combination condition of synthetized ionic liquid by controlling reaction factors and provides precious practical experience for exploiting new ionic liquids, which has important significance of theoretical research and application value.

Key word: Ionic liquids of imidazoles; Synthetize; Characterization

目 录

摘要 I

Abstract II

第一章 文献综述 1

1.1 离子液体研究的背景和意义 1

1.2 离子液体的性质 1

1.3. 离子液体的合成方法 2

1.3.1 传统加热法 2

1.3.2.微波法 3

1.3.3超声波法 3

1.4 咪唑类离子液体的应用 3

1.4.1 离子液体在分离与萃取中的应用 4

1.4.2离子液体在合成中的应用 4

1.4.3离子液体在催化中的应用 4

1.5 咪唑类离子液体的展望 4

第二章 实验部分 6

2.1 实验仪器及药品 6

2.1.1实验仪器 6

2.1.2 实验药品 7

2.2 实验原理 8

2.2.1 季铵化反应 8

2.2.2 复分解反应 8

2.3 实验过程 9

2.3.1 卤化1-丁基-3-甲基咪唑的制备 9

2.3.2 1-丁基-3-甲基咪唑四氟硼酸盐的制备 11

2.3.3 1-丁基-3-甲基咪唑六氟磷酸盐的制备 12

第三章 结果与讨论 13

3.1 结果 13

3.1.1离子液体中间体的结果与讨论 13

3.1.2 目标离子液体的结果与讨论 16

3.2 讨论 18

3.2.1 实验过程优化的讨论 18

3.2.2 反应条件优化的讨论 20

第四章 总结与展望 22

4.1 总结 22

4.2 展望 22

参考文献 24

致 谢 26

第一章 文献综述

1.1 离子液体研究的背景和意义

离子液体是由有机阳离子与有机或无机阴离子组成的,在室温下或接近室温下呈液态的盐,具有良好的导电性、较大的粘度、可设计性、不容易挥发、以及对许多有机物和无机盐有良好的溶解性等特点。它能够通过聚合反应、选择性烷基化、酰基化反应、胺化反应、电化学合成、室温和常压下的催化加氢反应、支链脂肪酸的制备等方面得到应用，并逐渐显示出催化体系可循环、反应速率快、转化率高、重复使用等优点^[1]。

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