博碩士論文 93324050 詳細資訊




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姓名 廖振凱(Chen-Kai Liao)  查詢紙本館藏   畢業系所 化學工程與材料工程學系
論文名稱 溴化四丁基銨鹽之製備與其電解─電透析方法以合成氯化四丁基銨鹽之研究
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★ 四丁基銨鹽之溶解度、締合常數、活性係數及分佈係數★ 溶劑與陰離子(Y)之結構對一典型相轉移催化親核取代反應BzCl + Bu4NY→BzY + Bu4NCl之反應性之效應
★ 溶劑、親核劑(QBr)陽離子之結構及溫度對相轉移催化反應BzCl + QBr<--> BzBr + QCl 之反應 性之效應★ 溶劑、基質結構及溫度對相轉移催化親核取代反應ROH + Bu4NCl<-->RCl +Bu4NOH 之反應 性之效應
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摘要(中) 摘要
  氯化四丁基銨鹽 Bu4NCl 是一常用的相轉移催化劑,在某些酯化反應特具功效。但由於氯化四丁基銨鹽難以季化合成,故利用電解﹣電透析溴化四丁基銨鹽 Bu4NBr 以合成之。
  本研究首先對於三丁胺 Bu3N 與碘丁烷 BuBr 之季化反應合成溴化四丁基銨鹽 Bu4Br。選擇一既容易進行反應且容易結晶之溶劑,本實驗選擇 DMA 當溶劑,其反應莫耳比為 Bu3N : BuBr : DMA = 1 : 1 : 3.73,溫度控制在 100℃,反應 16 小時候,冷卻析出結晶鹽,過濾後取出。其濾液再加入適當溶劑,利用溶解度與介電常數之不同,可再次析出結晶鹽。如此循環可將產率提高,亦可得到高純度之溴化四丁基銨鹽 Bu4NBr。
  本實驗裝置為四隔室型,陽極採用鉑鈦合金電極板,陰極採用不鏽鋼電極板。陽極室通入 NaCl 水溶液,濃縮室通入 NaBr 水溶液,淡化室通入 Bu4NBr 水溶液,陰極室通入 HCl 水溶液,配合陽離子交換膜 Nafion NX982TX 及陰離子交換膜 Asahi AMV。在陽極室與濃縮室溶液濃度固定不變情況下,則由實驗所得數據可知,電流效率、電壓效率與淡化室液、陰極室液濃度、電流密度、流速及各隔室間寬度之關係。以及電能消耗與淡化室液、陰極室液濃度、電流密度、流速及各隔室間寬度之關係。
  同時由無因次的分析,可得電流效率和電壓效率與系統操作變因有著無因次之關係。
摘要(英) Abstract
Tetrabutylammonium chloride is a phase transfer catalyst which is especially useful in some solid-liquid phase transfer catalyzed esterifications. It is not feasible to synthesize this compound by quaternization or by nucleophilic double displacement because that both the quaternization rate constant and the displacement equilibrium constant are very small. The tetrabutylammonium chloride can be prepared by the electrodialysis of tetrabutylammonium iodide. The advantages of the process are that the iodide can be easily obtained by quaternization and that only a cation exchange membrane is need. But, the disadvantages are that it is slightly soluble in water and the produced iodine would be absorbed on the anode. This project proposes a new electrodialysis process for synthesizing the tetrabutylammonium chloride.
From the derived current density equation and the applied voltage equation in this project, it is inspected that the factors affecting both the current efficiency and the voltage efficiency are: current density, concentration, flow velocities of electro-lytes and width of compartments.
From the two equations, the dimensionless correlations of two efficiencies with the operating variables are also proposed. The parameters in the equations will be ob-tained in this project so as to get the basic information for synthesizing tetrabu-tylammonium chloride.
關鍵字(中) ★ 氯化四丁基銨鹽
★ 電解─電透析
關鍵字(英) ★ tetrabutylammonium chloride
★ electrodialysis-electrolysis
論文目次 目錄
摘要.................................................................I
目錄.................................................................IV
圖目錄.................................................................IX
表目錄.................................................................XI
符號說明.................................................................XII
第一章 前言............................................................1
1-1 鹵化四級銨鹽之性質.............................................1
1-2 鹵化四級銨鹽之合成方法.........................................2
1-2-1 碘化四級銨鹽之合成方法..................................2
1-2-2 氯化四級銨鹽之合成方法..................................3
1-2-3 其它鹵化四級銨鹽之合成方法..............................4
1-3 鹵化四丁基銨鹽之應用...........................................5
1-3-1 當相轉移催化劑..........................................5
1-3-2 其他重要的用途..........................................7
1-4 電解﹣電透析之簡介.............................................7
1-4-1 電透析之濃縮﹣淡化過程..................................8
1-4-2 電透析之應用............................................8
1-4-3 對於電解﹣電透析之合成.................................10
1-4-4 季銨氫氧化物非電解﹣電透析之合成.......................12
1-5 本文的動機與主旨..............................................13
第二章 理論部份.......................................................14
2-1 二分子親核取代反應之速率方程式................................14
2-2 溶劑對季化反應之效應..........................................16
2-3 由阿瑞尼亞定律解釋溫度對反應速率常數之影響....................16
2-4 電解﹣電透析之流程............................................17
2-5 離子通量方程式與電極間之電位梯度..............................18
2-6 通電初態系統之濃度分佈........................................21
2-7 平衡極電位與電荷轉移過電程....................................21
2-7-1 平衡極電位.............................................21
2-7-2 電荷轉移過電壓.........................................24
2-8 擴散電位......................................................25
2-9 歐姆電位降....................................................25
2-10 Donnan potential.............................................26
2-11 濃度偏極化...................................................27
2-12 系統外加電壓方程式...........................................28
2-13 電流效率、電壓效率及電能消耗與無因次操作變數群之關係式.......30
第三章 實驗部份.......................................................37
3-1 實驗及分析用藥品..............................................37
3-2 實驗裝置及分析儀器............................................38
3-2-1 實驗裝置...............................................38
3-2-2 電導度計...............................................39
3-2-3 離子層析儀.............................................39
3-3 樣品分析......................................................39
3-3-1 電導度分析.............................................39
3-3-1.1 淡化室 Q+ 分析.......................................40
3-3-1.2 陰極室 Q+ 分析.......................................40
3-3-2 離子層析儀(IC)之校正曲線極樣品分析.....................40
3-4 實驗步驟......................................................42
3-4-0 溴化四丁基銨鹽的製備...................................42
3-4-1 極限電流密度之測定.....................................42
3-4-2 HCl(aq) 濃度對電流效率、電壓效率及電能消耗之影響.......43
3-4-3 QBr(aq) 濃度對電流效率、電壓效率及電能消耗之影響.......43
3-4-4 電流密度對電流效率、電壓效率及電能消耗之影響...........44
3-4-5 HCl(aq) 流速對電流效率、電壓效率及電能消耗之影響.......44
3-4-6 QBr(aq) 流速對電流效率、電壓效率及電能消耗之影響.......45
3-4-7 隔室寬度對電流效率、電壓效率及電能消耗之影響...........45
第四章 結果與討論.....................................................46
4-1 極限電流密度之測定............................................46
4-2 HCl(aq) 濃度對電流效率、電壓效率及電能消耗之影響..............46
4-3 QBr(aq) 濃度對電流效率、電壓效率及電能消耗之影響..............47
4-4 HCl(aq), QBr(aq) 濃度對電流效率、電壓效率及電能消耗影響之比較.48
4-5 電流密度對電流效率、電壓效率及電能消耗之影響..................49
4-6 HCl(aq) 流速對電流效率、電壓效率及電能消耗之影響..............50
4-7 QBr(aq) 流速對電流效率、電壓效率及電能消耗之影響..............51
4-8 HCl(aq), QBr(aq) 流速對電流效率、電壓效率及電能消耗影響之比較.51
4-9 隔室寬度對電流效率、電壓效率及電能消耗之影響..................52
4-10 電流效率及電壓效率與無因次操作變數群之關係式.................53
4-11 電解﹣電透析之最適條件.......................................55
第五章 結論..........................................................80
參考文獻..............................................................83
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指導教授 王天財(Ten-Tsai Wang) 審核日期 2006-7-22
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