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蒸餾固化法（Distillative Freezing Process,簡稱DF）是一種新式分離方法，蒸餾固化法具成本低廉、低耗能和能與傳統化工純化製程互相配合的優點。蒸餾固化法主要是應用將化學品操作在三相區間內，母液會同時的汽化與固化。母液一部分結晶為高純度的欲純化藥品，一部分則應用潛熱互換原理揮發為氣體並且去除之，蒸餾固化操作直至母液完全乾掉時停止操作，最後會得超高純度的結晶產物。
此次選擇使用蒸餾固化法純化的藥品有1-naphthol與2-naphthol混合物來純化分離1-naphthol或是2-naphthol，以及dodecanol與decanol混合物來純化分離dodecanol。naphthol方面的純化，經過四階段與五階段的蒸餾固化實驗可以將1-naphthol與2-naphthol皆從90％純化至99％以上的純度，而dodecanol方面的純化卻無法如預期的提升純度。

Distillative Freezing process (hereinafter called DF process) is a new separation technique. Basically, DF is operated at 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 liquid phase and vapor phase of mixtures. As the DF process is conducted under an adiabatic condition, the latent heat released in forming the solid crystals is mostly removed by vaporizing portions of liquid mixtures. The process is continued until the liquid phase is completely eliminated and only the pure solid crystals remain in the feed. DF is applied here to separate the 1-naphthol+2-naphthol mixture. The experiments show that four batch DF operations are required to purify 1-naphthol from 90% to >99% from the 1-naphthol-enriched mixture. On the other hand, five batch DF operations are required to purify 2-naphthol from 90% to >99% from the 2-naphthol-enriched mixture. However, it is found that DF can not be applied to separate dodecanol from the dodecanol+decanol mixture.

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授權書……………………………………………………………... Ⅲ
誌謝………………………………………………………………... Ⅳ
中文摘要…………………………………………………………... Ⅴ
英文摘要…………………………………………………………... Ⅵ
目錄………………………………………………………………... Ⅶ
圖表目錄…………………………………………………………... Ⅹ
第一章 緒論……………………………………………………... 1
第二章 文獻回顧………………………………………………... 3
2-1 naphthol簡介.………………………………………….... 3
2-2 naphthol的來源製程……………..……………………... 4
2-2-1 1-naphthol的來源製程…………………………... 4
2-2-2 2-naphthol的來源製程…………………………... 4
2-3 naphthol的純化製程………………….……………...…. 7
2-3-1 沉澱法分離純化2-naphthol……………………... 7
2-3-2 萃取結晶法分離純化2-naphthol………………... 8
2-4 脂肪醇簡介..……………………………………………. 9
2-5 脂肪醇的來源製程……………………………………... 10
2-6 dodecanol的純化製程……….…………………............. 14
2-6-1 直接接觸冷卻技術純化dodecanol……….……... 14
2-6-2 熔融結晶直接接觸冷卻技術純化dodecanol.…... 15
第三章 蒸餾固化法……………………………………………... 19
3-1 蒸餾固化法原理介紹…………………………………... 19
3-2 固汽共存區的形成……………………………………... 19
3-3 蒸餾固化法的特色和優點……………………..……..... 22
3-4 相圖的繪製……………………………………………... 25
3-5 蒸餾固化法操作條件之計算…………………………... 32
第四章 實驗設備和方法………………………………………... 36
4-1 實驗器材與藥品………………………………………... 36
4-1-1 naphthol實驗器材與藥品……………………….. 36
4-1-2 dodecanol實驗器材與藥品……………………… 37
4-2 蒸餾固化設備與周邊裝置………………………........... 38
4-2-1 naphthol蒸餾固化設備與周邊裝置……………... 38
4-2-2 dodecanol蒸餾固化設備與周邊裝置………….... 39
4-3 分析儀器………………………………………………... 53
4-3-1 naphthol分析儀器(HPLC)……………………….. 53
4-3-2 dodecanol分析儀器(GC)…………………...……. 54
4-4 實驗方法………………………………………………... 55
4-4-1 naphthol實驗方法…………………………........... 55
4-4-2 dodecanol實驗方法………………………..…...... 56
第五章 結果與討論……………………………………………... 57
5-1 naphthol實驗的結果與討論…………………………... 57
5-2 dodecanol實驗的結果與討論…………..……………... 58
第六章 結論……………………………………………………... 74
參考文獻…………………………………………………………... 76
附錄1：實驗相關分析圖譜………………………………………... 78

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