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研究生:林佳融
研究生(外文):Jia-Rong Lin
論文名稱:自由脂肪酸進行兩程序反應產製生質柴油之研究
論文名稱(外文):Biodiesel production from free fatty acids by a two-step process
指導教授:陳奕宏陳奕宏引用關係
口試委員:陳律言張慶源
口試日期:2013-06-01
學位類別:碩士
校院名稱:國立臺北科技大學
系所名稱:化學工程研究所
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:2013
畢業學年度:101
語文別:中文
論文頁數:96
中文關鍵詞:生質柴油自由脂肪酸甘油酯化轉酯化兩階段程序甘油純化
外文關鍵詞:Biodieselfree fatty acidsglycerolesterificationtransesterificationtwo-step processglycerin purification
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本研究探討以自由脂肪酸產製生質柴油之新穎兩階段程序,第一階段以自由脂肪酸為原料,在無添加觸媒的情況下與甘油進行高溫酯化反應,此反應可降低原料油裡的酸價,以便後續進行轉酯化反應產製生質柴油。最適酯化反應操作條件為醇酸莫耳比0.9、反應溫度250 oC、及反應時間1.5小時,可得脂肪酸轉化率為99.08%。第二階段以氫氧化鉀為觸媒,將酯化後脂肪酸與甲醇進行轉酯化反應,最適轉酯化反應條件為醇油莫耳比3、觸媒劑量1%w/w、反應溫度60 oC、及反應時間1小時,所生成脂肪酸甲基酯產率為97.0%。在本研究兩階段生質柴油產製程序中,粗甘油的回收率約為50%,已測試回收粗甘油可重複利用於酯化反應,且對反應無明顯不良影響。將本系統所產製的自由脂肪酸生質柴油進行油品性質分析,所得自由脂肪酸生質柴油的冷濾點為-15 oC、密度883 kg/m3、碘價118.66 g I2/100 g、動黏度4.93 mm2/s、及氧化穩定性0.32小時。

The objective of this study is to produce biodiesel from free fatty acids (FFAs) using a two-step process. In the first step, the FFAs are esterified with glycerol to produce glycerides. The reaction can reduce the acid value of FFAs before transesterification reaction. The conversion of FFAs was 99.08% under the optimal esterification conditions including the molar ratio of glycerol to FFAs of 9:10, reaction temperature of 250 oC, and reaction time of 1.5 h. The second step was the transesterification of the glycerides with methanol with potassium hydroxide as the catalyst. In the study, the recommended conditions for the trnsesterification of glycerides were molar ratio of methanol to oil of 3:1, catalyst loading of 1%w/w, reaction temperature of 60 oC, and reaction time of 1 h to obtain the yield of fatty acid methyl ester (FAMEs) as 97.0%. The recovery percentage of crude glycerol in the two-step process is about 50%, and the recovered crude glycerol can be reused in the esterification reaction without significant negative effects. The FFAs-based biodiesel had the cold filter plugging point of -15 oC, density of 883 kg/m3 at 15 oC, iodine value of 118.66 g I2/100 g, kinematic viscosity of 4.93 mm2/s at 40 oC, and oxidation stability of 0.32 h. 

摘 要 i
ABSTRACT ii
誌 謝 iii
目 錄 iv
表目錄 vii
圖目錄 ix
第一章 緒論 1
1.1 研究背景 1
1.2 研究動機 2
1.3 研究目的 2
第二章 文獻回顧 4
2.1 生質柴油簡介 4
2.2 生質柴油與石化柴油的比較 6
2.3 生質柴油國際標準法規 8
2.4 生質柴油的特性 12
2.4.1 十六烷值 12
2.4.2 閃火點 12
2.4.3 熱值 13
2.4.4 冷濾點 13
2.4.5 碘價 13
2.4.6 酸價 14
2.4.7 密度 14
2.4.8 動黏度 14
2.4.9 氧化穩定性 15
2.5 生質柴油之製程 18
2.5.1 油脂之前處理 19
2.5.2 轉酯化反應 20
2.5.3 分離和純化 21
2.5.4 醇類回收 21
2.5.5 甘油純化 22
2.6 原料與組成 22
2.6.1 自由脂肪酸 22
2.6.2 甘油 23
2.6.3 甘油酯 24
2.6.3.1 單酸甘油酯 24
2.6.3.2 雙酸甘油酯 25
2.6.3.3 三酸甘油酯 25
2.6.4 棕櫚脂肪酸蒸餾物(PFAD) 25
2.6.5 油酸 26
2.6.6 甘油對不同脂肪酸與甘油酯的互溶度 26
2.7 以含高自由脂肪酸原料產製生質柴油程序 28
2.8 以甘油進行脂肪酸酯化反應 29
2.9 轉酯化反應 36
第三章 儀器設備及研究方法 38
3.1 實驗樣品 38
3.2 生質柴油的製備與純化 39
3.2.1 自由脂肪酸與甘油進行酯化反應 42
3.2.2 轉酯化反應 42
3.2.3 粗製生質柴油之純化 43
3.2.4 粗甘油純化 44
3.3 分析方法及實驗儀器 46
3.3.1 酸價 46
3.3.2 脂肪酸之轉化率 46
3.3.3 甲基酯之產率 47
第四章 結果與討論 49
4.1 脂肪酸與甘油進行酯化反應 49
4.1.1 脂肪酸與甘油加熱方式對酯化反應的影響 50
4.1.2 醇酸莫耳比(nG/nFFAs)的影響 53
4.1.3 反應溫度(TR)的影響 56
4.1.4 冷凝對脂肪酸與甘油進行高溫酯化反應的影響 58
4.1.5 本研究與文獻甘油酯化反應之比較 61
4.2 酯化後脂肪酸進行轉酯化反應 65
4.2.1 醇油莫耳比(nM/nO)的影響 66
4.2.2 觸媒劑量(Wcat)的影響 69
4.2.3 反應溫度(TR)的影響 71
4.3 粗甘油的回收與再利用 73
4.3.1 脂肪酸與粗甘油進行酯化反應 73
4.3.2 粗甘油的回收率 75
4.4 自由脂肪酸生質柴油之油品性質分析 76
4.5 兩階段製程與傳統酸觸媒酯化製程之比較 77
第五章 結論與建議 81
5.1 結論 81
5.2 建議 82
參考文獻 83
附錄 A. 本研究建議反應系統示意圖 91
附錄 B. 本研究用物質性質表 92
附錄 C. 氣相層析光譜(FFAs-based biodiesel) 93
符號彙整 94


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