【正文】
1丁基 3甲基咪唑六氟 磷酸鹽離子液體合成研究摘 要離 子 液 體 是 指 完 全 由 正 負 離 子 所 組 成 , 并 且 在 室 溫 或 接 近 室 溫 下 呈 現(xiàn) 液態(tài) 的 鹽 , 也 稱 為 低 溫 熔 融 鹽 。 與傳統(tǒng)的有機溶劑相比,它具有很多優(yōu)點:(1) 幾乎沒有蒸汽壓、不揮發(fā)、無臭;(2) 有較大的穩(wěn)定溫度范圍,較好的化學(xué)穩(wěn)定性及較寬的電化學(xué)窗口;(3) 通過陰陽離子的設(shè)計可調(diào)節(jié)其對水、有機物及聚合物的溶解性。本實驗通過微波輔助加熱法制備 1丁基3甲基咪唑六氟磷酸鹽離子液體。制備的基本過程:將藥品 l甲基咪唑、溴代正丁烷、六氟磷酸鉀按一定比例混合于反應(yīng)容器內(nèi),然后置于微波爐中加熱。將制得的產(chǎn)物進行提純,并進行紅外分析,確定其是否為目標(biāo)產(chǎn)品。本實驗通過對加熱方法、加熱時間及藥品的配比等方面的改變,最終確定一個產(chǎn)率較高的實驗方案:將混合好的藥品(l甲基咪唑、溴代正丁烷、六氟磷酸鉀摩爾比為:1::)放入微波爐,功率調(diào)至最低,采用加熱 3 s,暫停 30 s 的間歇加熱方法,反應(yīng)時間 100 min,再用去離子水和乙醚分別對其洗滌數(shù)次,最后對產(chǎn)物進行減壓蒸餾,最終產(chǎn)物產(chǎn)率在 60%左右。關(guān)鍵詞:微波,提純,離子液體,紅外光譜,1丁基3甲基咪唑六氟磷酸鹽STUDY ON SYNTHESIS OF1BUTYL3METHYLIMIDAZOLIUM HEXAFLUOROPHOSPHATE IONIC LIQUID ABSTRACT Ionic liquids are posed entirely of positive and negative ions, and present at or near room temperature liquid salt, also known as lowtemperature molten salt. Compared with traditional anic solvents, it has many advantages: 1. almost no vapor pressure, nonvolatile, colorless, odorless。 2. with a greater range of stable temperature, good chemical stability and wide electrochemical interface。 3. it can be adjusted the solubility for water, anic pounds and polymers through the design of ions. In this study, 1butyl3methylimidazolium hexafluorophosphate ionic liquid was prepared using microwave. The basic process of preparation: lmethylimidazole, nbutane bromide and potassium hexafluorophosphate were mixed in the container at a certain propotion, and then heated with the microwave. Purify the product, and take the infrared analysis to determine whether the target product. The experimental program with a higher yield was ultimately established by changing heating method, heating time and the ratio of drugs and so on. Firstly, mixture of drugs were putted in the microwave ovens, most lowend gear prepared by heating 3 s, suspended 30 s intermittent heating method, reaction time was 100 min. Secondly, deionized water and ether were used to wash them several times, respectively. Finally, the products were carried on the reduced pressure distillation, and the final product yield was around 60%.KEY WORDS: Microwave, purification, infrared spectroscopy, ionic liquid hexafluorophosphate, 1butyl3methylimidazolium 目 錄第 1 章 緒 論 ...............................................................................................1167。 離子液體的定義 ..........................................................................1167。 離子液體的發(fā)展史 ......................................................................1167。 離子液體的分類 ..........................................................................2167。 離子液體的性質(zhì)及應(yīng)用 ..............................................................3167。 離子液體的性質(zhì) ................................................................3167。 離子液體的應(yīng)用 ................................................................3167。 離子液體的合成 ..........................................................................4167。 離子液體的合成 ................................................................5167。 微波加熱的原理 ................................................................5第 2 章 試驗材料與原理 .............................................................................9167。 試劑與儀器 ..................................................................................9167。 主要儀器 ............................................................................9167。 主要試劑 ............................................................................9167。 實驗原理 ....................................................................................10第 3 章 1丁基3甲基咪唑六氟磷酸鹽離子液體的合成 .......................11167。 [Bmim]PF6 合成的工藝流程 ......................................................11167。 微波爐加熱方案的確定 ............................................................12167。 微波爐檔位的確定 ..........................................................12167。 加熱方法及時間的確定 ...................