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研究生:曾淑麗
研究生(外文):Shu Li Tseng
論文名稱:蒸餾固化法分離純化4-甲氧基酚+鄰苯二酚混合物
論文名稱(外文):Separation of 4-methoxyphenol + catechol mixtures by distillative freezing process
指導教授:蕭立鼎
指導教授(外文):L. D. Shiau
學位類別:碩士
校院名稱:長庚大學
系所名稱:化工與材料工程研究所
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:2008
畢業學年度:96
論文頁數:76
中文關鍵詞:蒸餾固化分離4-甲氧基酚鄰苯二酚
外文關鍵詞:distillative freezingseparation4-methoxyphenolcatechol
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蒸餾固化法(distillative freezing process)是一種新式的分離純化方法,簡稱為DF法,可應用於分離純化沸點相近的混合物。DF法結合蒸餾及固化(結晶)操作之優點,是一種低耗能、低污染且高效率的化學品分離純化法。原理上是利用三相分離的原理操作,該法中將含有揮發性不純物的液態進料帶到欲純化物質三相點以下的壓力區,使汽化與結晶操作同時進行,最後所得晶體周圍無任何液體附著,成為高純度的主成分結晶。純化過程中,液體操作在絕熱條件下,而液體結晶時所釋放出的結晶熱提供液體汽化所需之汽化熱。
本論文研究結果顯示:DF法可將鄰苯二酚(catechol),由進料組成90 %純化至99 % +,當進料組成為95 %可純化至99.8 %,實驗結果比DF模擬結果佳;在純化4-甲氧基酚(4-methoxyphenol)方面,只能由進料組成90 %純化至約91 %,而進料組成95 %只純化至95.3 %,並未達到DF模擬效果,因此利用DF法分離純化4-甲氧基酚與鄰苯二酚混合物中之鄰苯二酚是可行的。
A new separation technique, called distillative freezing (DF), is introduced in this work to separate the mixture of 4-methoxyphenol and catechol. In principle, the DF process is operated at a triple-point condition in which the liquid mixture is simultaneously vaporized and solidified due to the three-phase equilibrium. It results in the formation of pure solid and both liquid and vapor phase of mixtures. In essence, the process is continued until the liquid phase is completely eliminated and only the pure solid crystals remain in the feed.
The experimental results show that catechol can be purified from 90 % to 99 % + or from 95 % to 99.8 % in the catechol-enriched mixture. On the other hand, 4-methoxyphenol can only be purified from 90 % to 91 % or from 95 % to 95.3 % in the 4-methoxyphenol-enriched mixture.
目 錄
指導教授推薦書
論文口試委員會審定書
授權書.......................................................................................................III
誌謝...........................................................................................................IV
中文摘要....................................................................................................V
英文摘要...................................................................................................VI
目錄.........................................................................................................VII
圖目錄.......................................................................................................IX
表目錄.......................................................................................................XI
第一章 緒論...............................................................................................1
1.1 前言..............................................................................................1
1.2 研究方向......................................................................................1
第二章 文獻回顧.......................................................................................2
2.1 4-甲氧基酚和鄰苯二酚簡介........................................................2
2.2 4-甲氧基酚和鄰苯二酚來源製程................................................4
2.3 DF法純化技術.............................................................................5
第三章 蒸餾固化法...................................................................................8
3.1 蒸餾固化法原理..........................................................................8
3.2 蒸餾固化法之特點....................................................................10
3.3 相圖繪製....................................................................................13
3.4 DF系統程序分析.......................................................................26
第四章 實驗設備與方法.........................................................................30
4.1 實驗器材與藥品........................................................................30
4.2 蒸餾固化設備周邊裝置............................................................31
4.3 桌上型蒸餾固化設備................................................................32
4.4 實驗方法....................................................................................34
4.5 分析儀器....................................................................................35
第五章 結果與討論.................................................................................38
5.1 純化鄰苯二酚富相混合物........................................................38
5.2 純化4-甲氧基酚富相混合物....................................................50
第六章 結論.............................................................................................57
符號說明...................................................................................................59
參考文獻...................................................................................................61
圖目錄
Figure 2-1 The phase diagram variety of two-components at different
pressures(溫俊清, 2007)..........................................................7
Figure 3-1 Phase diagram of two-components at low pressure.................9
Figure 3-2 Separation and purification systems of hybrid(呂永方, 2001)..................................................................................................................12
Figure 3-3 The steps of drawing two-components phase diagram..........19
Figure 3-4 Solid-liquid phase diagram of 4-methoxyphenol and catechol
at 1.013×10^5 Pa(---- represents the solid-liquid equilibrium
calculated based on the ideal solution)..................................21
Figure 3-5 Vapor-liquid phase diagram of 4-methoxyphenol and catechol
at 1.013×10^5 Pa(---- represents the vapor-liquid equilibrium calculated based on the ideal solution)..................................22
Figure 3-6 Phase diagram of 4-methoxyphenol and catechol at 1.013×10^5 Pa(---- represents the solid-liquid equilibrium calculated based on the ideal solution)..................................23
Figure 3-7 Phase diagram of 4-methoxyphenol and catechol at 133 Pa
calculated in this study...........................................................24
Figure 3-8 Phase diagram of 4-methoxyphenol and catechol at 10.7 Pa
calculated in this study...........................................................25
Figure 3-9 Simulated DF operation where each stage is operated under an
adiabatic condition at a three-phase equilibrium state...........26
Figure 4-1 Schematic diagram of the experimental apparatus for the DF
operation.................................................................................33
Figure 4-2 Experimental steps.................................................................34
Figure 4-3 Calibrated curve for 4-methoxyphenol..................................36
Figure 4-4 Calibrated curve for catechol.................................................37
Figure 5-1 Decreasing of sample temperature with time during the DF
experiment for run 9...............................................................41
Figure 5-2 Comparison of experimental and simulation results for
separation of 50 g sample of catechol from the catechol
-enriched mixture (o represents feed concentration and
• represents product concentration).....................................46
Figure 5-3 Comparison of experimental and simulation results for
separation of 20 g sample of catechol from the catechol
-enriched mixture (o represents feed concentration and
• represents product concentration).....................................47
Figure 5-4 Decreasing of sample temperature with time during the DF
experiment for run 14.............................................................52
Figure 5-5 Comparison of experimental and simulation results for
separation of 4-methoxyphenol from the 4-methoxyphenol
-enriched mixture (o represents feed concentration and
• represents product concentration).....................................55
表目錄
Table 2-1 Some physical properties for 4-methoxyphenol and catechol
(NIST Standard Reference Database 11, 1985).........................3
Table 2-2 Some physical properties for hydroquinone, 2-methoxyphenol,
1,2-dimethoxybenzene and 1,4-dimethoxybenzene...................5
Table 3-1 The parameters of Wilson Eqn. for 4-methoxyphenol(A) +
catechol(B)(Hwang et al., 2000; Lin et al., 2004)...................17
Table 4-1 The method of calibrated curve for 4-methoxyphenol............36
Table 4-2 The method of calibrated curve for catechol...........................37
Table 5-1 Simulation results of DF operation for a 20 g liquid feed with
XW,A = 0.80(△T = 3.6℃).........................................................42
Table 5-2 Simulation results of DF operation for a 20 g liquid feed with
XW,A = 0.85(△T = 3.8℃).........................................................43
Table 5-3 Simulation results of DF operation for a 20 g liquid feed with
XW,A = 0.90(△T = 3.8℃).........................................................44
Table 5-4 Simulation results of DF operation for a 20 g liquid feed with
XW,A = 0.95(△T = 2.8℃).........................................................45
Table 5-5 Comparison of experimental and simulation results for
separation of catechol from the catechol-enriched mixture.....48
Table 5-6 Comparison of the final temperature and pressure for simulation
results with actual operation....................................................49
Table 5-7 Simulation results of DF operation for a 20 g liquid feed with
XW,B = 0.90(T△ = 2)℃............................................................53
Table 5-8 Simulation results of DF operation for a 20 g liquid feed with
XW,B = 0.95(△T = 2℃)............................................................54
Table 5-9 Comparison of experimental and simulation results for
separation of 4-methoxyphenol from the 4-methoxyphenol
-enriched mixture.....................................................................56
Table 5-10 Comparison of the final temperature and pressure for
simulation results with actual operation................................56
Hwang, S.M., Lee, M.J. and Lin, H.M. Isothermal vapor-liquid equilibria for mixtures of 4-methoxyphenol, catechol, and p-cresol. Fluid Phase Equilibria 172, 183-196 (2000).
Kirk, R.E. and Othmer, D.F. Encyclopedia of chemical technology. John Wiley & Sons (1985).
Lee, M.J., Chang, Y.K., Lin, H.M. and Chen, C.H. Solid-liquid equilibria for 4-methoxyphenol with catechol, ethylenediamine, or piperazine. Journal of Chemical and Engineering Data 42, 349-352 (1997).
Lee, M.J., Chang, Y.K. and Lin, H.M. Separation of close-boiling mixtures of 4-methoxyphenol/catechol with tert-butanol. Separation Science and Technology 33, 1511-1528 (1998).
Lee, M.J., Wu, F.L. and Lin, H.M. Separation of closely boiling compounds of catechol and 4-methoxyphenol with the aid of 1,4-butanediol. Industrial and Engineering Chemistry Research 40, 4596-4602 (2001).
Lin, H.M., Chou, Y.H., Wu, F.L. and Lee, M.J. Solid-liquid equilibria of closely boiling compounds of 4-methoxyphenol and catechol with p-cresol. Fluid Phase Equilibria 220, 69-74 (2004).
Moldoveanu, S.C. and Kiser, M. Gas chromatography/mass spectrometry versus liquid chromatography/fluorescence detection in the analysis of phenols in mainstream cigarette smoke. Journal of Chromatography A 1141, 90-97 (2007).
NIST Standard Reference Database 11: DIPPR data compilation of pure compound properties. Version 5.0, sponsored by The Design Institute for Physical Property Data (DIPPR) of the American Institute of Chemical Engineers, copyright by The American Institute of Chemical Engineers, 1985.
Risner, C.H. and Cash, S.L. A high-performance liquid chromatographic determination of major phenolic compounds in tobacco smoke. Journal of Chromatographic Science 28, 239-244 (1990).
Shiau, L.D., Wen, C.C. and Lin, B.S. Separation and purification of p-xylene from the mixture of m-xylene and p-xylene by distillative freezing. Industrial and Engineering Chemistry Research 44, 2258-2265 (2005).
Shiau, L.D., Wen, C.C. and Lin, B.S. Application of distillative freezing in the separation of o-xylene and p-xylene. The American Institute of Chemical Engineers 52, 1962-1967 (2006).
Shiau, L.D., Liu, K.F., Jang, S.M. and Wu, S.C. Separation of diethylbenzene isomers by distillative freezing. Journal of the Chinese Institute of Chemical Engineers 39, 59-65 (2008).
Vijayaraj, M. and Gopinath, C.S. Selective production of methoxyphenols from dihydroxybenzenes on alkali metal ion-loaded MgO. Journal of Catalysis 243, 376-388 (2006).
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