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研究生: 鄭博仁
Bo-Ren Jeng
論文名稱: 矽膠再生
Regeneration of silica gel
指導教授: 朱義旭
Yi-Hsu Ju,
口試委員: Ismadji
Suryadi Ismadji
曾文祺
Wen-Chi Tseng
學位類別: 碩士
Master
系所名稱: 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年: 2009
畢業學年度: 97
語文別: 英文
論文頁數: 66
中文關鍵詞: 矽膠再生角鯊烯植物固醇游離脂肪酸
外文關鍵詞: regeneration of silica gel, tocopherol, free fatty acid, squalene
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在大豆油除臭油(SODD)分離過程中,修正索式萃取法是一經濟可行的技術。此法經由使用溶劑回收下,可以得的高回收率的非極性脂質(NPLF)。在NPLF,以角鯊烯和固醇之脂肪酸脂(FASE)為最重要的成分。角鯊烯的回收率可達100%,FASEs的回收率可達94.32%。雖然修正索式萃取法所需成本較低,但是使用大量的矽膠當作SODD吸附劑佔了總成本的75~80%。如果可以將矽膠回收再利用,不僅可以節省多餘成本花費也可以利用在廢水處理。
在使用新鮮矽膠當作SODD吸附劑為條件下,最佳的重量比例是1:3 (SODD:矽膠)。但是,當矽膠再生後,以再生矽膠當作SODD吸附劑條件,相同的重量比例1:3(SODD:矽膠)將會使得游離脂肪酸的回收率大量提升至49.71%,遠大於使用新鮮矽膠當作吸附劑的回收率(<20%)。本研究藉由改變矽膠對SODD的重量比例,發現不同比例和不同時間下,對於角鯊烯和FASE的回收率會有不同的影響。使用新鮮的矽膠, 最佳的重量比例是1:3 (SODD:矽膠),最佳時間是12小時;使用第一次再生的矽膠,最佳的重量比例是1:5 (SODD:矽膠),最佳時間是60小時; 使用第二次再生的矽膠,最佳的重量比例是1:8 (SODD:矽膠),最佳時間是110小時;以上這些條件,可使產物回收率達到最佳化,且使FFAs回收率最小化。


Modified soxhlet extraction (MSE) is an economically viable technique in separation of bioactive compounds from SODD. The amount of solvent required in MSE is small and after extraction of non polar lipid fraction (NPLF) and polar lipid fraction (PLF), the solvent can be recovered and reused in the next extraction step. In the NPLF, squalene and FASEs are the most valuable components. The recovery of squalene and FASEs can reach 100% and 94.32%, respectively. The only hindrance in scaling up MSE is the cost of silica gel. A great deal of silica gel as adsorbent could constitute 75~80% of the total cost in MSE. If silica gel can be regenerated and reused, then the operation cost of MSE can be reduced significantly.
When fresh silica gel was used as adsorbent, the optimal mass ratio of SODD-to-silica gel is 1:3. However, when regenerated silica gel was used as the adsorbent, the same degree of separation as that of using fresh silica gel was not attainable under the same operation conditions. At a mass ratio of SODD-to-silica gel of 1:3, FFAs recovery of 49.71% was obtained which is much higher than that obtained by using fresh silica gel as the adsorbent (20% FFAs recovery). This high recovery of FFAs in NPLF would affect the quality of final product. This study investigated the effect of mass ratio of SODD-to-silica gel and extraction time on the recovery of squalene, FASEs, and FFAs. Using fresh silica gel, the optimal conditions achieved are: mass ratio of SODD to silica gel = 1:3, extraction time = 12 h. By using first regenerated silica gel, the optimal conditions achieved are mass ratio of SODD to silica gel = 1:5, extraction time = 60 h. By using second regenerated silica gel, the optimal conditions are mass ratio of SODD to silica gel = 1:8, extraction time = 110 h. Under those 3 set of optimal conditions corresponding to fresh silica gel, 1st and 2nd regenerated silica gel, the MSE can achieve approximately the same degree of separation; i.e., 100% recovery of squalende and ca. 94% recovery of FASEs in the NPLF while the FFAs recovery in NPLF can be kept to less than 20%.

CHAPTER: 1 INTRODUCTION 2 1-1 Soybean 1 1-2 Composition Of SODD 3 1-2.1 Squalene 3 1-2.2 Phytosterols 4 1-2.3 Tocopherols 6 1-3 TYPES OF PHYSICAL SEPARATION 6 1-3.1 Crystallization method 7 1-3.2 Membrane separation 8 1-3.3 Adsorption 9 1-3.4 Molecular distillation 9 1-3.5 Supercritical extraction 10 1-3.6 Soxhlet extraction 10 1-3.7 Modified soxhlet extraction 11 1-4 Objective 14 2 LITERATURE SURVEY 16 2-1 ZEOLITES 17 2-2 ACTIVATED CARBON 18 2-3 SILICA GEL 19 2-3.1 Application of silica gel 19 2-3.2 Source of silica gel 21 2-3.3 Factors affecting silica gel properties 22 3 MATERIALS AND METHODS 25 3-1 MATERIALS 25 3-2 EQUIPMENTS 25 3-3 METHODS 26 3-3.1 Activation of Fresh Silica Gel 26 3-3.2 Extraction of NPLF from SODD by using Fresh Silica Gel 26 3-3.3 Regeneration of Silica Gel 27 3-3.4 Extraction of NPLF from SODD by using Regenerated Silica Gel 29 3-3.5 TLC Analysis 30 3-3.6 HT-GC Analysis 30 3-3.7 Scanning Electron Microscopy (SEM) Analysis 30 3-3.8 Analysis by Fourier Transform - Infra Red (FT-IR) 31 3-3.9 Nitrogen Adsorption–Desorption Isotherm Analysis 31 3-3.10 Statistical Analysis 31 4 RESULTS AND DISCUSION 33 4-1 SILICA GEL CHARACTERIZATION 33 4-2 ACTIVATION OF FRESH SILICA GEL 37 4-3 EXTRACTION OF NPLF FROM SODD BY USING FRESH SILICA GEL 40 4-4 REGENERATION OF SILICA GEL 43 4-5 EXTRACTION OF NPLF FROM SODD BY USING REGENERATED SILICA GEL 45 5 CONCLUSIONS 53 REFERENCES 55 CURRICULUM VITAE COPY RIGHT

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