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研究生:游佳憲
研究生(外文):Jia-Xian You
論文名稱:藉由結晶製程製備高水溶性化合物: 十二烷基硫酸鈉(SDS) 以及控制其水合物
論文名稱(外文):Preparation and Hydrate Control for Highly Water Soluble Compound : Sodium Dodecyl Sulfate (SDS) by Crystallization Processes
指導教授:李度李度引用關係
指導教授(外文):Tu Lee
學位類別:碩士
校院名稱:國立中央大學
系所名稱:化學工程與材料工程學系
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:2018
畢業學年度:107
語文別:英文
論文頁數:80
中文關鍵詞:水合物共溶劑熟化
外文關鍵詞:hydrareco-solventaging
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十二烷基硫酸鈉(SDS)為高水溶性化合物,並且為常用的表面活性劑之一。在文獻報導中,十二烷基硫酸鈉具有4種水合物,分別為1/8水、半水、一水以及無水。但是製成端方面較少文獻提到如何控制SDS為何種水合物。因此本篇論文主要目的為採取工業上常用批式結晶,並結合蒸發結晶、反溶劑結晶以及冷卻結晶製造出特定SDS·1/8水合物。買來的0.5克SDS以定量的方式浸泡在由水及丙酮組成的1比17之體積比的共溶劑以製造SDS·1/8水合物。在合併結晶製程中,255毫升的丙酮作為反溶劑加入結晶槽。此合併結晶製程的產率為83%,所生產出來的SDS經由傅里葉變換紅外光譜(FTIR)、熱重分析(TGA)、差示掃描量熱法(DSC)和粉末X射線衍射(PXRD)鑑定推測為SDS·1/8水合物。最後將生產出來的SDS·1/8水合物放置25、52、75%不同濕度之環境放置5天測試穩定度。經由穩定度測試下,生產出來的SDS·1/8水合物是很穩定的水合物型式
Sodium dodecyl sulfate (SDS) was highly water soluble compound and was one of the commonly used surfactants. In previous studies, hydrate forms of SDS, 1/8 hydrate, hemihydrate, monohydrate, and anhydrous had been reported. However, there are few studies mentioned how to control the hydrate forms for SDS in the manufacturing process. Therefore, the aim of this thesis was to produce exact SDS·1/8 hydrate, through the combined process of evaporative, anti-solvent, cooling crystallization, and co-solvent system in batch system. First, purchased SDS crystals were immersed into the 1:17 volume ratio of co-solvent composed of water to acetone (v/v)) for preparation of SDS·1/8 hydrate. In combined process, 255mL of acetone was chosen as anit-solvent to introduce into crystallizer. Finally, produced SDS·1/8 hydrate was tested stability by exploring at 25, 52 and 75% relative humidity. The yield for the combined crystallization process was about 83%. The produced SDS was speculated to be SDS·1/8 hydrate, by characterization of Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and powder X-ray diffraction (PXRD). The result of stability test demonstrated that the produced SDS·1/8 hydrate was a stable form.
摘要.....................................................i
Abstract................................................ii
Acknowledgement.........................................iii
Table of Contents.......................................iv
List of Figures.........................................vii
List of Tables..........................................x
List of Schemes.........................................xi
Chapter 1 Introduction.................................1
1.1 Crystallization.................................1
1.1.1 Evaporative crystallization.....................1
1.1.2 Antisolvent Crystallization.....................2
1.1.3 Cooling Crystallization.........................3
1.2 Hydrates........................................4
1.3 Sodium Dodecyl Sulphate.........................5
1.4 Conceptual Framework............................13
1.5 References......................................14
Chapter 2 Experimental Materials and Methods...........17
2.1 Materials.......................................17
2.1.1 Chemicals.......................................17
2.1.2 Solvents........................................17
2.2 Experimental Methods............................19
2.2.1 Initial Solvent Screening.......................19
2.2.2 Combination of Composition Variation with Phase Diagram during Evaporation Process......................20
2.2.3 The End Point for Evaporation...................21
2.2.4 Preparation of SDS·1/8 Hydrate by Aging in Water /Acetone Co-solvent.....................................22
2.2.5 Crystallization Process of SDS·1/8 hydrate......23
2.2.6 Stability Test..................................27
2.3 Analytical Measurements.........................28
2.3.1 Optical Microscopy (OM).........................28
2.3.2 Fourier Transform Infrared Spectroscopy (FTIR)..28
2.3.3 Thermogravimetric Analysis (TGA)................29
2.3.4 Differential Scanning Calorimetry (DSC).........29
2.3.5 Powder X-ray Diffraction (PXRD).................30
2.3.6 References......................................31
Chapter 3 Results and Discussion.......................32
3.1 Use Test of SDS.................................32
3.2 Initial Solvent Screening of SDS................36
3.3 Composition Variations of SDS in Evaporative Crystallization Process 39
3.4 Determination of the End Point for Evaporation..42
3.5 Preparation of SDS·1/8 Hydrate by Aging in Water /Acetone Co-solvent.....................................45
3.6 Crystallization Process of SDS·1/8 Hydrate......49
3.7 Stability Test..................................57
3.8 References......................................60
Chapter 4 ........................................62
Conclusions and Future Works............................62
4.1 Conclusions.....................................62
4.2 Future Works....................................63
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