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Student Number 87321016
Author Zhe-Ho Geo(高志宏)
Author's Email Address No Public.
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Department Chemical and Materials Engineering
Year 1999
Semester 2
Degree Master
Type of Document Master's Thesis
Language zh-TW.Big5 Chinese
Title 鹵化四丁基銨之合成動力學、溶解、萃取及精製研究
Date of Defense 2000-07-05
Page Count 196
Keyword
  • 季化
  • 萃取
  • 陰離子置換
  • 電解─電透析
  • 飽和溶解度
  • 鹵化四丁基銨
  • Abstract 本研究有鑑於鹵化四丁基銨為一具有高經濟、高附加價值之物質,其應用層面之廣泛,常被使用於均相之相轉移催化反應 (譬如:聚合、酯化、氧化、水解等) 、電化學反應 (譬如:配合鋰鹽來製作電解質液) 、其它應用 (譬如:陽離子界面活性劑等),故本研究旨在研發合成鹵化四丁基銨。
    為了尋求最適合成與精製之條件,本研究進行其合成動力學、飽和溶解度、萃取及精製研究:
    (1) 合成方面
    a. 季化反應 (合成Bu4NI、Bu4NBr與Bu4NCl)
    合成Bu4NI部份,以Bu3N:BuI:chloroform之最適莫耳比 = 1:1:4.34,於50 ℃~90 ℃反應,得Ea = 60.77 kJ╱mole;最適生產條件Bu3N:BuI:chloroform之莫耳比 = 1:1:4.34,於90 ℃下反應3.5 hr,得Bu4NI產率99.8 %。
    合成Bu4NBr部份,以Bu3N:BuBr:N,N-dimethylacetamide之最適莫耳比 = 1:1:3.73,於60 ℃~100 ℃反應,得Ea = 62.75 kJ╱mole;最適生產條件Bu3N:BuBr:N,N-dimethylacetamide之莫耳比 = 1:1.5:3.73,於100 ℃下反應13 hr,得Bu4NBr產率98.5 %。
    合成Bu4NCl部份,以Bu3N 62.5 ml與BuCl 27.6 ml在N,N-dimethylacetamide 90.1 ml中,於80℃下反應8hr,得Bu4NCl 產率 0.075 %。
    b. 陰離子置換方面 (合成Bu4NCl)
    以50 ml BzCl、200 ml H2O、32 g Bu4NI與150 ml chloroform於40℃反應15 hr,得Bu4NCl水溶液之濃度3.1 %。
    c. 電解—電透析反應 (合成Bu4NCl)
    陽極液為初濃度0.592 N碘化四丁基銨之乙醇溶液,陰極液為初濃度0.024 N之HCl水溶液,以定電流3.99A並僅量保持陰、陽極液濃度之操作下;經5 hr,於陰極室中得Bu4NCl水溶液之濃度12.56 %,其電流效率為48.6 %。
    (2) 飽和溶解度方面
    由本研究作Bu4NI與Bu4NBr在水中飽和溶解度( g salt╱g H2O )之測定與文獻值比較,分別為0.018(0.0243)、6.661(6.925),由此知本實驗無論是測定高溶解度或低溶解度之分析方法均可行。
    (3) 萃取方面
    在精製Bu4NBr時,其萃取系統H2O—DMA—CH2Cl2之最佳萃取體積比為11:1:10;在精製Bu4NCl時,該鹽在萃取系統CH2Cl2—H2O之萃取常數KE與在水溶液之濃度M之關係式KE = -0.0083 M2 + 0.0374 M + 0.8798。
    (4) 精製方面
    a. 碘化四丁基銨: 之純度 = 98.135 %, 之純度 = 97.82 %, 結晶產率 = 97.5 %。
    b. 溴化四丁基銨: 之純度 = 97.859 %, 之純度 = 98.11 %, 結晶產率 = 94.3 %。
    c. 氯化四丁基銨: 之純度 = 95.59 %, 之純度 = 95.83 %, 結晶產率 = 93.8%。
    Table of Content 第一章 緒論
    1.1 季銨鹽之合成方法與合成反應動力學...........................1
    1.2 季銨鹽之溶解與萃取平衡之導電度測定........................17
    1.3 季銨鹽之用途..............................................19
    1.4 本研究之動機與主旨........................................31
    第二章 理論
    2.1 季化反應..................................................35
    2.2 陰離子置換反應............................................48
    2.3 電解—電透析反應..........................................49
    第三章 實驗部份
    3.1 實驗與分析之藥品..........................................52
    3.2 實驗裝置及分析儀器........................................54
    3.3 樣品分析..................................................56
    3.4 實驗步驟..................................................59
    第四章 結果與討論
    4.1 季化反應之初步研究可行性實驗..............................74
    4.2 鹵化四丁基銨之飽和溶解度測定..............................80
    4.3 碘化四丁基銨之合成動力學..................................80
    4.4 溴化四丁基銨之合成動力學.................................113
    4.5 氯化四丁基銨之合成動力學.................................144
    4.6 陰離子置換法合成氯化四丁基銨之可行性實驗.................147
    4.7 電解—電透析反應合成氯化四丁基銨.........................152
    4.8 鹵化四丁基銨之精製結果...................................152
    4.9 鹵化四丁基銨之純度鑑定...................................152
    第五章 結論..................................................153
    參考文獻.....................................................156
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