以甘蔗渣水解後的殘渣製造固體酸催化劑催化油酸和甲醇之酯化反應

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研究生：	蕭以昌 Yi-Chang Xiao
論文名稱：	以甘蔗渣水解後的殘渣製造固體酸催化劑催化油酸和甲醇之酯化反應 Solid acid catalyst from post-hydrolyzed sugarcane bagasse residue for the esterification of oleic acid and methanol
指導教授：	吳耀豐 Alchris Woo Go 朱義旭 Yi-Hsu Ju
口試委員:	翁玉鑽 Artik Elisa Angkawijaya
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：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	111
中文關鍵詞：	甘蔗渣、稀酸水解、固體酸觸媒、酯化反應
外文關鍵詞：	Sugarcane bagasse, Dilute acid hydrolysis, Solid acid catalyst, Esterification
相關次數：	點閱：253 下載：0
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上一筆

本研究探索了一種全新方法製備固體酸催化劑，透過稀酸水解甘蔗渣，然後同時碳化和磺化水解後的殘渣。在稀酸水解甘蔗渣中調查了一定範圍的溶劑與固體比 (7.5, 10, 12.5 mL/g)、硫酸濃度 (2, 4, 6 wt.%) 和720分鐘內測定對糖產量、糖濃度和抑製劑濃度的影響。從稀酸水解甘蔗渣後收集的殘渣，在一定溫度（100, 125, 150 ℃）和時間（12, 24, 36 h）範圍內進行同時碳化和磺化。由稀酸水解甘蔗渣以溶劑與固體比為10 mL/g、 4 wt.%的硫酸與100 °C下進行2小時，隨後同時磺化和碳化水解後殘渣在125 ℃ 與 36小時下製備的固體酸觸媒具有強酸密度為 2.83 ± 0.03 mmol H+/g，並在催化油酸與甲醇之酯化反應中，以甲醇與油酸莫爾比5、催化劑負載為15 wt.%、200 rpm、60 °C與24小時為最佳化反應條件進行，可以達到產物中脂肪酸甲酯含量為 96.45 ± 0.09 % ，並且可以使用至少七次循環，即使在第七次循環之後仍保留其原始催化活性的38%。此研究提出了一種以甘蔗渣合成碳基固體酸觸媒與從中回收可用的糖的替代方法。

A new approach on the preparation of solid acid catalyst (SAC) from sugarcane bagasse (SCB) via a series of dilute acid hydrolysis (DAH), carbonization, and sulfonation was explored. A range of parameters; solvent to solid ratio (SSR, 7.5, 10, 12.5 mL/g), sulfuric acid concentration (2, 4, 6 wt.%), and a period of 720 minutes; were used during DAH of SCB to determine their effects on of sugar yield, sugar concentration, and inhibitor concentration. The PHSCBs collected from DAH were subsequently carbonized and sulfonated simultaneously over a range of temperature (100, 125, 150 ℃) and time (12, 24, 36 h). The SAC prepared from DAH of SCB at SSR of 10 mL/g, with 4 wt.% acid for 2 h at 100 °C and subsequent sulfonation and carbonization at 125 ℃ for 36 h (SCB-SAC-10-125-36) possess a strong acid density 2.83 ± 0.03 mmol H+/g and performed among the synthesized SAC during the esterification of oleic acid and methanol. Under favorable conditions methanol to oleic acid ratio 5, 15 wt.% catalyst loading and 200 rpm at 60 ℃ for 24 h, 96.45 ± 0.09 of FAME content in the product could be achieved. It could be used for at least seven cycles while retaining 38 % of its original catalytic activity even after the seventh cycle. This work presents an alternative approach in the synthesis of carbon-based SAC from SCB while allowing recovery of available sugars.

摘要 2
ABSTRACT 3
ACKNOWLEDGEMENT 4
TABLE OF CONTENTS 5
LIST OF FIGURES 8
LIST OF TABLES 10
LIST OF ABBREVIATIONS 11
CHAPTER 1. BACKGROUND OF STUDY 12
1. Introduction 12
2. Goal and objectives 16
3. Significance of the study 17
4 Scope and Limitations 18
CHAPTER 2. REVIEW OF RELATED LITERATURE 19
1. Sugarcane bagasse (SCB) 19
1.1. Production and availability 20
1.2. Characteristics and current use 22
2. Recovery of sugar from SCB 24
2.1. Hydrolysis with the aid of acid at high concentrations 24
2.2. Hydrolysis with the aid of enzymes 26
2.3. Hydrolysis under supercritical water conditions 27
2.4 Hydrolysis with the aid of dilute acid and/or subcritical water conditions 28
3. Carbon-based solid acid catalyst 29
3.1. Sulfonation of carbon-based or carbonaceous material 29
3.2. Carbonization of sugars and subsequent sulfonation 30
3.3. Carbonization of lignin and subsequent sulfonation 32
3.4. Carbonization of lignocellulosic biomass and subsequent sulfonation 32
3.5. Simultaneous carbonization and sulfonation 33
4 Synthesis of solid acid catalyst using SCB for application biodiesel 34
4.1. Carbonization and subsequent sulfonation    35
4.2. Hydrothermal pretreatment, carbonization and subsequent sulfonation 36
4.3. Direct sulfonation or simultaneous carbonization and sulfonation    37
5. Esterification of free fatty acids with carbon-based solid acid catalysts 37
5.1. Factor affecting the esterification process 37
5.2. Regeneration and reusability of carbon-based solid acid catalyst 39
6. Potential synthesis of SAC from SCB via DAH and subsequent direct sulfonation 42
CHAPTER 3. MATERIALS AND METHODS 43
1. Collection and storage of SCB 43
1.1. Moisture content of SCB 44
2. Determination of Structural Carbohydrates in SCB 44
3. Estimation of the total sugar content by the dinitrosalicy acid method 44
4. Estimation of the total inhibitor content by the HPLC 46
5. Diluted acid hydrolysis of sugarcane bagasse 47
5.1. Small scale 47
5.2. Large scale 49
6. Simultaneously carbonized and sulfonated PHSCB as the solid acid catalyst    50
7. Catalyst characterization of a solid acid catalyst and sugarcane bagasse    50
7.1. Particle size distribution 50
7.2. Strong acid density 51
7.3. Total acid density 52
7.4. Fourier Transform Infrared Spectrometer analysis    53
7.5. Surface Area and Pore size distribution    53
7.6. Thermogravimetric Analysis 53
7.7. FESEM-EDX analysis 55
8. Esterification activity of solid acid catalyst 55
9. Esterification of oleic acid with methanol using SCB-SAC 57
10. Reusability of sulfonated PHSCB as a catalyst during the esterification 58
CHAPTER 4. RESULTS AND DISCUSSION 60
1. Diluted acid hydrolysis of SCB 61
2. Simultaneously carbonized and sulfonated PHSCB as the solid acid catalyst 69
3. Esterification of oleic acid with SCB-SAC 79
4. Reusability of SCB-SAC 84
CHAPTER 5. CONCLUSION 89
REFERENCES 90
APPENDIX A 106
APPENDIX B 109


                                

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全文公開日期 2024/07/16 (國家圖書館：臺灣博碩士論文系統)

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