臺灣博碩士論文加值系統

本研究首先以相平衡計算軟體 PE 2000分別以 Peng-Robinson 狀態方程式與 Petel-Teja 狀態方程式搭配傳統雙參數混合律，進行二氧化碳-異丙醇、二氧化碳-水及異丙醇-水等三組雙成分系統之理論迴歸計算，求得最佳之交互作用參數。結果發現，Peng-Robinson 與 Petel-Teja 兩種狀態方程式，皆適用於上述三組雙成分系統之理論迴歸計算。
其次，利用求出之雙成分最佳交互作用參數，以 Peng-Robinson狀態方程式配合雙參數混合律，計算出二氧化碳-異丙醇-水三成分系統在溫度 338.15 K，壓力137.9及172.3 bar下的相平衡數據，結果與文獻的實驗數據吻合。然在 338.15 K /137.9 bar 條件下之相圖其樑線由二氧化碳豐富的氣相為端點輻射向外，與文獻所載由水豐富的液相為端點輻射向外之樑線不同，有可能是其溫度 338.15 K 略高於文獻之 333.15 K 造成。另外由 338.15 K 之相圖亦觀察到，其兩相區樑線形狀的改變壓力為 172.3 bar。
隨著環保意識的抬頭及溶劑價格高漲，廢溶劑的回收與再精製漸受重視。異丙醇廣泛應用平於面顯示器及半導體產業中，作為製程清洗用之溶劑，故本文另一研究主題為異丙醇水溶液的分離。傳統的異丙醇水溶液分離技術有共沸蒸餾、薄膜蒸發、反應萃取蒸餾以及鹽析萃取。本研究利用商業模擬軟體Aspen Plus，於溫度 333.15 K，壓力 100 bar下，進行實驗室規模超臨界二氧化碳萃取異丙醇水溶液製程之穩態模擬，並找出此製程之最適操作條件。結果發現，將 85 wt.% 異丙醇水溶液純化至99 wt.% 所需之理論板數，與文獻計算結果相近。
最後，將實驗室規模模擬所得之製程最適操作條件，進行超臨界二氧化碳萃取製程之放大模擬，估算其能源耗用約為傳統共沸蒸餾製程之 62.4%。值此能源價格高漲之際，超臨界二氧化碳萃取製程應為異丙醇水溶液分離值得推廣之另一選擇。

In this study, the Peng-Robinson equation of state and Petel-Teja equation of state with two-parameters mixing rule were used to fit the experimental data of the binary systems CO2-isopropanol, CO2-water, and isopropanol-water to find the binary interaction parameters by software PE 2000. The results showed that both equations of state are equally suitable for these three binary-systems.
With these interaction parameters from the three binary systems, the phase equilibrium of CO2-isopropanol-water at 338.15 K, 137.9 bar and 172.3 bar were found. The calculated results showed the two phase region were in good agreement with literatures, yet tie lines at 338.15 K and 137.9 bar were different from literature at 333.15 K and 132 bar. It was noted that a critical change of tie lines occurs at 172.3 bar along the increase of pressure at 338.15 K.
In addition, separation of aqueous isopropanol with supercritical carbon dioxide at 333.15 K and 100 bar was studied in this work. Aspen Plus was used to compute the theoretical number of plate with 85 wt.% aqueous isopropanol feed. The results were consistent with results from lab scale experiments. The optimum operation conditions were also determined. With the optimized conditions, a full scale unit for the azeotropic separation was simulated, and the estimated energy consumption was about 62.4% compared to traditional heterogeneous azeotropic distillation. This study shows that CO2 is an energy-saving alternative to azeotropic separation of isopropanol and water.

摘要I
Abstract III
誌謝IV
目錄V
圖目錄VIII
表目錄X
第一章 緒論1
1.1 前言1
1.2 超臨界流體2
1.2.1 超臨界流體之簡介2
1.2.2 超臨界流體之優缺點及其存在之問題7
1.2.3 超臨界流體之應用9
1.3 研究動機11
1.4 文獻回顧11
1.5 論文章節安排13
第二章 相平衡原理與計算14
2.1 前言14
2.2 相平衡理論14
2.3 狀態方程式與混合律17
2.4 相平衡計算21
2.5 結果與討論22
2.5.1 雙成分系統相平衡理論計算22
2.5.1.1 二氧化碳-異丙醇系統22
2.5.1.2 二氧化碳-水系統23
2.5.1.3 異丙醇-水系統23
2.5.2 三成分系統相平衡理論計算30
第三章 分離單元36
3.1 前言36
3.2 超臨界流體萃取流程36
3.3 相平衡39
3.3.1 相平衡關係表示方法39
3.3.2 二氧化碳-異丙醇-水三成分系統相平衡資料40
3.4 熱力學模式與參數49
3.5 製程模擬55
3.5.1 製程設計概念55
3.5.2 模擬結果分析55
3.5.2.1 分離壓力對異丙醇收率之影響56
3.5.2.2 S/F Ratio對萃取相中異丙醇濃度之影響56
3.5.2.3 萃取壓力對萃取相中異丙醇濃度之影響56
3.5.2.4 萃取溫度之影響57
3.5.2.5 回流比之影響57
3.5.3 模擬結果討論57
第四章 製程比較67
4.1 前言67
4.2 傳統共沸蒸餾製程67
4.3 超臨界二氧化碳萃取製程68
4.4 結果討論68
第五章 結論與未來展望72
5.1 結論72
5.2 未來展望73
參考文獻 74
附錄 85
圖目錄
圖1.1 超臨界流體在相圖上的位置3
圖1.2 純物質於臨界點附近之相圖5
圖2.1 泡點壓力計算法計算流程25
圖2.2 CO2-IPA雙成分系統汽液相平衡數據以Peng-Robinson及Petel-Teja狀態方程式關聯結果與實驗值之比較27
圖2.3 CO2-H2O雙成分系統汽液相平衡數據以Peng-Robinson及Petel-Teja狀態方程式關聯結果與實驗值之比較28
圖2.4 IPA-H2O雙成分系統汽液相平衡數據以Peng-Robinson及Petel-Teja狀態方程式關聯結果與實驗值之比較29
圖2.5 33315K下隨壓力變化之CO2-IPA-H2O三成分系統相圖32
圖2.6 以Peng-Robinson狀態方程式計算之CO2-IPA-H2O相平衡數據與實驗值之比較(338.15K，137.9 bar)33
圖2.7 以Peng-Robinson狀態方程式計算之CO2-IPA-H2O相平衡數據與實驗值之比較(338.15K，172.3 bar)34
圖3.1 超臨界二氧化碳分餾流程圖38
圖3.2 相對揮發度42
圖3.3 CO2-IPA-H2O系統於313.15K，103.4 bar 下之麥克-希爾圖44
圖3.4 CO2-IPA-H2O系統於318.15K，124.1 bar 下之麥克-希爾圖45
圖3.5 CO2-IPA-H2O系統於338.15K，137.9 bar 下之麥克-希爾圖46
圖3.6 CO2-IPA-H2O系統於338.15K，172.3 bar 下之麥克-希爾圖47
圖3.7 不同條件下之IPA/H2O分離因子及迴歸曲線48
圖3.8 Aspen Plus建立之超臨界二氧化碳萃取製程模擬流程圖52
圖3.9 實驗室規模之超臨界二氧化碳萃取製程模擬流程圖及結果60
圖3.10 分離壓力對IPA收率之影響61
圖3.11 S/F ratio 對萃取相中 IPA濃度之影響62
圖3.12 萃取壓力與塔頂IPA濃度之關係63
圖3.13 萃取溫度與塔頂/塔底濃度之關係64
圖3.14 回流比與塔頂IPA 濃度之關係65
圖4.1 異丙醇共沸蒸餾模擬流程圖及結果69
圖4.2 超臨界二氧化碳萃取模擬流程圖及結果70
表目錄
表1.1 氣體、超臨界流體及液體的特性4
表1.2 一些常用作超臨界萃取溶劑的流體之臨界性質6
表2.1 常用的立方型狀態方程式20
表2.2 以Peng-Robinson及Petel-Teja狀態方程式搭配傳統雙參數混合律所迴歸之雙成分交互作用參數26
表2.3 以Peng-Robinson狀態方程式搭配傳統雙參數混合律所迴歸之CO2-IPA-H2O系統最佳交互作用參數及計算之相平衡數據偏差值比較(338.15K)35
表3.1 二氧化碳-異丙醇-水三成分系統相平衡資料43
表3.2 高壓下常用的熱力學模式53
表3.3 Aspen Plus 迴歸之雙成分交互作用參數53
表3.4 不同熱力學模式之Aspen Plus模擬結果54
表3.5 Aspen Plus 模擬超臨界二氧化碳萃取之基本組織架構58
表3.6 Aspen Plus 模擬之設定操作條件59
表3.7 Aspen Plus 模擬超臨界二氧化碳萃取製程最適操作條件66
表4.1 異丙醇水溶液純化製程之能源耗用比較71

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