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研究生： 泰爾迪婭
Muthiarani, Tri Eltiyah
論文名稱： 棕櫚油廠廢水（污泥棕櫚油）轉化為特殊應用的有價值化合物
The Transformation of Palm Oil Wastewater (Sludge Crude Palm Oil) into Valuable Compounds for Spesific Application
指導教授： 凌永健
Ling, Yong-Chien
口試委員: 余靖
Yu, Chin
趙奕姼
Chao, Ito
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2019
畢業學年度： 107
語文別： 英文
論文頁數： 69
中文關鍵詞： 污泥棕櫚油 、酯化反應 、脂肪酸甲酯 、油酸 、歐米茄9 、結晶
外文關鍵詞： Sludge Crude Palm Oil, Esterification reaction, Fatty acid methyl ester, Oleic acid, Omega-9, Crystallization
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    • 棕櫚油在印尼經濟的成長中扮演著著重要角色，隨著這個行業成長得越來越大，
    通過壓製提取棕櫚油後，通常利用池塘系統用於處理諸如廢水中的粗棕櫚油（CPO）污泥，處理廢水到符合排放標準，所需的土地空間，因此越來越大。為了克服這個缺點，本項由循環經濟指導的研究，開發了一種替代方法將CPO污泥處理和轉化為特定應用的有價值產品，例如脂肪酸甲酯（FAME），可以作為生質柴油。然而，FAME中仍然含有許多有價值的化合物，如油酸（Omega-9）之不飽和脂肪酸。在此，我們首先探討通過酯化反應將CPO污泥轉化為生質柴油的幾種催化劑，例如硫酸（H2SO4）、硫酰（SO2Cl2）、氫氧化鈉（NaOH）、和氫氧化四甲銨（TMAH），輔以氣相層析-質譜儀（GC-MS）分析進而確定總FAME。顯示使用15％濃度的TMAH酯化反應，可以得到最高的總FAME（98.3％）。進一步使用美國材料與試驗協會（ASTM）相關方法進行測試，以確保FAME可歸類為生物柴油。然後，使用效應曲面法（RSM）實驗設計，使用尿素和甲醇結晶FAME繼續進行油酸提取，以產生最佳的油酸提取。採用RSM結晶萃取，最佳結果為74.6％，反應條件為尿素/FAME比（2.02/1）; MEOH/尿素比（4.37/1）和24.4小時反應時間。

    Palm oil plays a significant role in the Indonesian economic growth as this industry becomes bigger and wider. After the extraction of palm oil by pressing, the wastewater containing crude palm oil (CPO) sludge is produced. In general, pond system is used to treat this CPO. Pond system needs very large land space to make the wastewater completely ready to be discharged. To overcome this drawback, this research guided by circular economy develops an alternative approach to treat and transform CPO sludge into valuable product for specific application such as fatty acid methyl ester (FAME) as a biodiesel. Nevertheless, the FAME still contains a lot of valuable compounds such as oleic acid (Omega-9) unsaturated fatty acid. Herein, we explored to transform the CPO sludge into a biodiesel with several type of catalysts such as sulfuric acid (H2SO4), sulfuryl chloride (SO2Cl2), sodium hydroxide (NaOH) and tetramethylammonium hydroxide (TMAH) by esterification reaction. The total FAME was determined by gas chromatography-mass spectrometry (GC-MS) analysis. The esterification using 15% concentration of TMAH showed the highest total FAME (98.3%). The FAME was further tested using relevant methods from American Society Testing and Materials (ASTM) to make sure that the FAME can be categorized as biodiesel. Then the experiment was continued to oleic acid extraction by crystallization FAME with urea and methanol using response surface methodology (RSM) experimental design to yield the optimal ones. The extraction by crystallization using RSM showed the optimum result of 74.6% with reaction conditions are Urea/FAME ratio (2.02/1) ; MeOH/Urea ratio ( 4.37/1) and 24.42 hours reaction time.

    摘要.................................................................I Abstract............................................................II Acknowledgement....................................................III List of Contents....................................................IV List of Figures...................................................VIII List of Tables......................................................IX List of Schemes......................................................X Chapter 1 Introduction...............................................1 1-1 Research Background..............................................1 1-2 Palm Oil Mill....................................................2 1-3 Crude Palm Oil (CPO).............................................3 1-3-1 CPO Sludge.....................................................5 1-4 Biodiesel........................................................5 1-5 Catalyst.........................................................7 Chapter II Literature Review.........................................9 2-1 Transesterification..............................................9 2-2 Esterification..................................................10 2-2 Crystallization of Oleic Acid...................................11 2-3 Response Surface Methodology....................................13 2-4 Central Composite Design........................................14 2-5 Gas Chromatography - Mass Spectrometry..........................15 Chapter III Experimental Section...................................17 3-1 Apparatuses and Materials......................................17 3-1-1 Experimental Apparatuses......................................17 3-1-2 Materials.....................................................17 3-2 Procedures......................................................17 3-2-1 Sample Preparation............................................17 3-2-2 The Process of Converting Fatty Acids into Esters.............18 3-2-3 The Process of Separating Fatty Acid Methyl Esters............18 3-3 The Physico-chemical Properties of FAME.........................18 3-3-1 The Viscosity and Color of Fatty Acid Methyl Esters...........18 3-3-2 Analysis of Acid Value........................................19 3-3-2-1 Standardisation of KOH......................................19 3-3-2-2 Acid Value of CPO Sludge (ASTM D-664).......................19 3-3-2-3 Acid Value of FAME..........................................19 3-3-3 Analysis of Water Content.....................................20 3-3-4 Analysis of Density (ASTM-D1217-15)..........................20 3-3-5 Analysis of Viscosity (ASTM D-445)............................21 3-4 The Optimization of Oleic Acid Extraction from FAME.............22 3-4-1 The Crystallization of FAME...................................22 3-4-2 Optimization and Variable Codes...............................22 3-4-3 Optimization of Crystallization Reaction......................25 3-4-3-1 Experiments Data Analysis order 1...........................25 3-4-3-2 Experiments Data Analysis order 2...........................26 Chapter IV Results and Discussions..................................27 4-1 Characteristics CPO Sludge......................................27 4-2 The Conversion of CPO Sludge into Fatty Acid Methyl Esters......27 4-3 The Effect of Catalyst amount on The Yield of FAME..............29 4-3-1 Sulfuric Acid.................................................29 4-3-2 Sulfuryl Chloride.............................................31 4-3-3 Sodium Hydroxide.............................................32 4-3-4 Tetramethylammonium Hydroxide.................................33 4-4 Effect of Catalysts Types on The Yield of FAME..................34 4-5 Effect of Activated Carbon and Filtration of FAME...............35 4-6 Properties of FAME..............................................37 4-6-1 Water Content.................................................37 4-6-2 Density.......................................................38 4-6-3 Viscosity.....................................................39 4-6-4 Acid Value....................................................40 4-7 Oleic Acid Extraction by Crystallisation with Urea..............41 4-7-1 The Percentage of Oleic Acid in CPO Sludge....................42 4-7-2 The Effect of Urea/FAME Ratio on Oleic Acid Percentage in CPO Sludge..............................................................43 4-7-3 The Effect of Methanol/Urea Ratio on Oleic Acid Percentage in CPO Sludge..............................................................44 4-7-4 The Effect of Reaction Time on Oleic Acid Percentage in CPO Sludge ....................................................................45 4-8 The Optimization of Extraction..................................46 4-8-1 Data Analysis of Extraction Results using Order I of Design of Experiment..........................................................46 4-8-2 Data Analysis of Extraction using order II of Design of Experiment ....................................................................48 4-8-3 Normality Test................................................50 4-9 Specific Application............................................51 4-10 Economic Analysis and Future Works.............................51 Chapter V Conclusions...............................................53 References..........................................................54

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