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研究生:許世杰
研究生(外文):Shih-Chieh Hsu
論文名稱:間氯酚與對氯酚之固液相平衡研究
論文名稱(外文):Research of Solid-Liquid Equilibrium of 3-chlorophenol and 4-chlorophenol
指導教授:李亮三
指導教授(外文):Liang-Sun Lee
學位類別:碩士
校院名稱:國立中央大學
系所名稱:化學工程與材料工程研究所
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:112
中文關鍵詞:固液平衡結晶締合結晶法分離流程
外文關鍵詞:adductive agentseparation processSLEcrystallizationadductive crystallization
相關次數:
  • 被引用被引用:5
  • 點閱點閱:134
  • 評分評分:
  • 下載下載:0
  • 收藏至我的研究室書目清單書目收藏:2

摘要
工業上常需分離混合物以得到更高純度的產物,可行的方法有很多,本論文乃是研究以締合結晶法來分離沸點相近的間氯酚及對氯酚混合物。在此分別嘗試以苯胺及特丁醇為中和劑,探討中和劑之合適性。經雙成份之固液相圖研究發現,苯胺與對氯酚及間氯酚生成1:1之複合物;特丁醇則與對氯酚及間氯酚生成2:1之複合物,故兩者均為頗合適的中和劑。我們進一步探討對氯酚、間氯酚與苯胺以及對氯酚、間氯酚與特丁醇兩組三成份之固液相行為,並繪製出三成份固液相圖,利用相圖所提供之資料,我們嘗試找出可行的分離流程,並依不同入料成份加以探討。
本研究中相圖之建立乃是利用固體消失法,經由在□溫槽中,觀察各不同成份組成之樣品的最後固體消失溫度而來。而數據關聯部份,採用了物理化學模式,以計算活性係數;於無合熔點之系統,以共熔點為分界點,以Wilson模式及NRTL模式計算活性係數;對於有合熔點之系統,則以共熔點及合熔點為分界點,採ICM模式以及依槓桿原理修正後的xi、γi來關聯其結果。


Abstract
It is very common to have to separate mixtures for getting high purity products. An adductive crystallization method was employed in this study to separate closing-boiling point m-chlorophenol + p-chlorophenol mixtures in this study. Neutralizing agents including tert-butanol and aniline have been tested for separating the mixtures and their applicability were discussed. We found that aniline could be a potential neutralizing agent by the fact that it forms complexes with both m-chlorophenol and p-chlorophenol. Consequently, we further investigated the solid-liquid phase behavior for the ternary system of aniline + m-chlorophenol +p-chlorophenol . This ternary phase diagram provided us useful information for finding a feasible separation procedure and favorable operation conditions. The separating process was discussed by different initial composition of m-chlolrpheno+p-chlorophenol mixture.
This diagram is built by observing the final disappearance temperature of the solid phase under accurately controlled bed temperature. For the curve fitting, the Ott & Goates fitting is chosen. As for the correlation, Wilson , NRTL and ICM models have been used to calculate the activity coefficients of the systems with or without congruent points. And the calculating shows the NRTL model gives better results .


目錄
中文摘要I
目錄III
表目錄V
圖目錄VIII
符號說明XI
第一章緒論
前言1
1-1 結晶簡介1
1-2 基本固液平衡相圖及分析3
1-3 締合結晶法之理論基礎6
1-4 實驗系統7
1-5 文獻回顧9
1-6 本文各章重點13
第二章固液相平衡數據量測
前言17
2-1 藥品17
2-2 實驗設備17
2-3 固液平衡量測步驟18
2-3-1 配置樣品18
2-3-2 熔點之量測19
2-4 實驗設備配置說明及注意事項20
2-5 雙成份系統之量測結果21
2-6 三成份系統之量測結果24
2-6-1 中和劑為苯胺24
2-6-2 中和劑為特丁醇26
2-6-3 三成份相圖之分析27
2-7 分離程序28
2-7-1 中和劑為苯胺28
2-7-2 中和劑為特丁純30
2-8 熔化熱之量測32
第三章理論計算90
3-1 固液相平衡法則91
3-2 含共熔點之固液相平衡理論95
3-3 含合熔點之固液相平衡理論95
3-4 活性係數之計算98
3-5 三成份系統之固液相平衡計算99
第四章結果與討論101
第五章結論與建議103
參考文獻105


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