臺灣博碩士論文加值系統

異丙醇水溶液共沸物的分離是在生化或電子工業用上一項重要的操作。然而這類共沸物通常是需要特殊技術來分離的複雜性非理想混合物。對於上述混合物之所有分離技術中，萃取蒸餾是一種最有效的方法。但是對可以用來增加混合物相對揮發度的質傳分離劑的選擇仍然是更進一步應用萃取蒸餾的一種障礙。丙二醇為廣泛使用於開發可注射用配方給水難溶性藥物的賦形劑，它們的低毒性、低蒸氣壓、與高的水中溶解度能夠避免對環境的污染，使得它們可能成為萃取分離水溶液共沸物的有效綠色溶劑。
本研究包含三組雙成分系統：異丙醇 + 水、異丙醇 + 1,3-丙二醇、水 + 1,3-丙二醇，以及一組三成分系統：異丙醇 + 水 + 1,3-丙二醇於101.3 kPa 下之汽液相平衡系統；物理性質方面，溫度於 298.15 K、308.15 K、318.15 K 和 328.15 K 下，進行三組雙成份系統：異丙醇 + 1,3-丙二醇、異丙醇 + 水、1,3-丙二醇 + 水，而三成分系統：異丙醇 +水 + 1,3-丙二醇，則是在溫度298.15 K下進行。密度是以震盪管式密度計測量，黏度是以Ubbelohde毛細管黏度計測量，表面張力是以白金片法表面張力計測量，折射率是以阿貝折射率計測量。
汽液相平衡實驗系統中液相活性係數計算方式分為含逸壓係數及修正Raoult’s law兩種。氣相逸壓係數是利用SRK的狀態方程式來計算。在雙成分系統中，只在異丙醇 + 水系統中有最小共沸點的產生。在熱力學一致性測試部分，異丙醇 + 水之雙成分系統是使用Kojima測試法及Van Ness直接測試法來進行測試，異丙醇 + 1,3-丙二醇與 1,3-丙二醇 + 水系統是使用Van Ness直接測試法來進行測試。實驗數據是以二參數Margules、Wilson、NRTL及UNIQUAC四種液相活性係數模式來做關聯，並以雙成份各模式中之最佳交互作用參數來預測三成分系統的汽液平衡數據。
物理性質實驗中藉由密度(ρ)、黏度(η)、表面張力(σ)、折射率(nD)的實驗值來計算出過剩莫爾體積(VE)、黏度偏差(Δη)、表面張力偏差(Δσ)、莫爾分率折射率偏差(ΔxnD)與體積分率折射率偏差值(ΔnD)，雙成份系統的過剩莫爾體積、黏度偏差、莫爾分率折射率偏差與體積分率折射率偏差值由Redlich-Kister方程式關聯，表面張力偏差是利用另一種經驗式關聯，三成份系統的這些過剩性質是由 Jasiński 及 Malanowski、Cibulka、Singh 等人、Pintos等人、Calvo等人、Mascato等人方程式及其衍生方程式關聯。並且將三成份數據用Scatchard等人、Tsao與Smith、Toop、Kohler、Colinet、及Jacob與Fitzner 方程式來做預測，其所得的預測結果和實驗值的偏差合理地接近。

Separation of aqueous 2-propanol azeotropes is a very important operation in the biochemical and electronic industries. However, these azeotrops are complicated, nonideal mixtures that need special techniques to be separated. Among all of the separation techniques toward the above mixtures, extractive distillation behaves the most effectively. However, the selection of mass separation agents that act to increase the relative volatility of the mixture is still a handicap for the further application of the extractive distillation. Propylene glycols are widely used exicipients for developing injectable formulations for poorly water soluble drugs. Their low toxicity, low vapor pressure, and high water solubility can avoid atmospheric contamination and enable their potential use as green solvents for the extractive separation of aqueous azeotropes.
In this work, the vapor-liquid equilibria (VLE) at 101.3 kPa were conducted for the three binary systems, including 2-propanol + water, 2-propanol + 1,3-propanediol, and water + 1,3-propanediol, and the ternary system of 2-propanol + water + 1,3-propanediol. In for the physical properties of density, viscosity, surface tensions, and refractive index, at the temperatures of 298.15 K, 308.15 K, 318.15 K, and 328.15 K, the three binary systems of 2-propanol + 1,3-propanediol, 2-propanol + water, 1,3-propanediol + water, and the ternary system of 2-propanol + water + 1,3-propanediol at the temperature of 298.15 K were measured.
In the VLE experimental systems, the liquid phase activity coefficients were calculated according to the equation including the fugacity coefficients of vapor phase and the equation of the modified Raoult’s law. Calculations of the fugacity coefficients of vapor phase were made with the Soave-Redlich-Kwong (SRK) equation of state. In the binary systems, only the 2-propanol + water system appears a minimum azeotrope. Thermodynamic consistency tests were performed for the VLE data of 2-propanol + water system using the Kojima method and the direct test of Van Ness. The 2-propanol + 1,3-propanediol and 1,3-propanediol + water systems were using the direct test of Van Ness. The VLE data of the binary and ternary mixtures were correlated using the three-suffix Margules, Wilson, NRTL, and UNIQUAC activity-coefficient models. The models with their best-fitted interaction parameters of the binary systems were also used to predict the ternary vapor-liquid equilibrium.
The excess molar volumes (VE), deviations in the viscosity (Δη), deviations in the surface tension (Δσ), mole fraction deviations in the refractive index (ΔxnD), and volume-fraction deviations in the refractive index (ΔnD) for the mixtures were derived from these experimental data of densities (ρ), viscostites (η), surface tensions (σ), and refractive indexes (nD) of physical properties. The binary data of excess molar volumes, deviations in the viscosity, mole fraction deviations in the refractive index and volume-fraction deviations in the refractive index were correlated as a function of the mole fraction using the Redlich-Kister equations. The deviations in the surface tension was correlated with another form of empirical equation. The ternary excess data were correlated with the equations of Jasiński and Malanowski, Cibulka, Singh et al., Pintos et al., Calvo et al., and Mascato et al. The ternary data were also predicted using the equations of Scatchard et al., Tsao and Smith, Toop, Kohler, Colinet, and Jacob and Fitzner. The result is reasonally closed to the experimental result.

中文摘要 I
Abstract III
目錄 V
表目錄 VIII
圖目錄 XII
附錄目錄 XVII
符號說明 XVIII
第一章 緒論 1
1-1 前言 1
1-2 化學工業上的應用 3
1-3 香水與香料的應用性 4
1-4 相關文獻調查 5
1-5 汽液相平衡裝置介紹 8
第二章 理論概述 11
2-1 相平衡研究之重要性 11
2-2 相律 12
2-3 汽液平衡理論 13
2-4 汽液相平衡數據處理方法 16
2-4-1 狀態方程式方法(equations of state, EOS) 16
2-4-2 活性係數方法(activity coefficient method) 17
2-5 熱力學一致性測試簡介 27
2-5-1 Van Ness直接測試法 28
2-5-2 Kojima測試法 32
2-5-3 Herington面積測試法 35
2-5-4 Fredenslund逐點測試法 36
2-5-5 Wisniak熱力學一致性測試法 39
2-5-6 三成分系統之熱力學一致性測試 40
2-6 液體密度之基本原理 41
2-6-1 密度測量儀器 43
2-7 液體黏度之基本原理 48
2-7-1 黏度測量之儀器 51
2-8 液體表面張力之基本原理 61
2-8-1 液體表面張力測量儀器 62
2-9 液體折射率之基本原理 66
2-9-1 折射率測量之儀器 72
第三章 實驗設備與步驟 74
3-1 實驗藥品 74
3-2 實驗設備 80
3-2-1 汽液平衡設備 80
3-2-2 壓力控制設備 81
3-2-3 組成分析裝置 84
3-2-4 物理性質儀器 85
3-3 實驗步驟 95
3-3-1 樣品配製 96
3-3-2 建立檢量線 99
3-3-3 檢量線檢測 99
3-3-4 汽液相平衡實驗步驟 100
3-3-5 密度、折射率測量步驟 100
3-3-6 黏度測量步驟 103
3-3-7 表面張力測量步驟： 104
第四章 結果與討論 106
4-1 汽液相平衡實驗結果 106
4-2 雙成分汽液相平衡實驗結果 108
4-3 異丙醇 + 水雙成分系統共沸點的決定 109
4-4 雙成分系統熱力學一致性測試結果 109
4-5 雙成分理論模式參數迴歸計算結果 112
4-6 三成分系統的汽液相平衡實驗結果 114
4-7 三成分的預測與理論模式參數迴歸計算結果 114
4-8 異丙醇 (1) + 水 (2) + 1,3-丙二醇 (3)系統
在假設無含1,3-丙二醇之下之T-X1-Y1與Y1-X1的結果 115
4-9 異丙醇 (1) + 水 (2) + 1,3-丙二醇 (3) 系統
在假設無含1,3-丙二醇之下之相對揮發度結果 116
4-10 雙成分物理過剩性質數據計算與討論 116
4-10-1 密度與過剩莫爾體積 117
4-10-2 黏度與黏度偏差 119
4-10-3 表面張力與表面張力偏差 122
4-10-4 折射率與折射率偏差 124
4-11 三成分數據計算與討論 128
4-11-1 三成份密度與過剩摩爾體積的計算 128
4-11-2 三成份黏度與黏度偏差的計算 127
4-11-3 三成份表面張力與表面張力偏差的計算 128
4-11-4 三成份折射率與折射率偏差的計算 130
4-12 雙成分物理性質迴歸計算 131
4-12-1 密度、黏度、折射率雙成份物理性質的迴歸與討論 131
4-12-2 密度、黏度、折射率雙成份物理過剩性質的迴歸 133
4-12-3 表面張力的迴歸與過剩性質的迴歸的討論 135
4-12-4 密度、黏度、折射率雙成份物理性質合併溫度的迴歸與討論 137
4-12-5 密度、黏度、折射率雙成份過剩性質對合併溫度的迴歸與討論 138
4-12-6 表面張力及偏差對合併溫度的迴歸與討論 140
4-12-7 三成份過剩性質與偏差的迴歸 142
4-12-8 三成份過剩性質預測 144
第五章 結論 147
參考文獻 330
附錄 342

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