臺灣博碩士論文加值系統

本研究針對以油桐樹(Vernicia fordii)籽油及將其與其他生質油品混合後，添加甲醇與氫氧化鉀進行超音波輔助轉酯化反應轉製生質柴油進行研究，並探討不同摻配及轉酯化程序對其酸價(acid value, AV)、碘價(iodine value, IV)、動黏度(kinematic viscosity, KV)、密度及其冷濾點(cold filter plugging point, CFPP)之影響。背景實驗條件為：超音波頻率(fUS) 20 kHz、輸出功率(PWUS) 270 W、桐油、芥菜油與棕櫚油之摻配比為20、50及30 wt.%、甲醇與油之莫耳數比(M/O) = 6:1、KOH觸媒劑量 (MC) 為1 wt.%、反應溫度 (TR) 20-30 °C、反應體積(VL) 390 mL、時間(tUS) 1-30 min。研究結果顯示，tUS ≥ 5 min時桐油生質柴油之轉酯率 (YF)可達87-91%；而混合油之tUS ≥ 1 min 時YF 更可達92-94%。當tUS = 10 min時桐油生質柴油之AV 為0.11 mg KOH/g、IV為159.36 g I2/100 g、KV 為9.17 mm2/s、密度為905 kg/m3、CFPP為-16 oC。而相同條件下獲得之混合油生質柴油之AV 為0.11 mg KOH/g、IV為120.35 g I2/100 g、KV為5.54 mm2/s、密度為887 kg/m3、CFPP 則為-5 oC。與ASTM-D6751標準值AV 需小於0.5 mg KOH/g、KV與密度需介於1.9-6 mm2/s及860-900 kg/m3對照，可知桐油須與其他生質油品混合後轉製生質柴油其性質方可符合生質柴油標準。若使用超音波輔助轉酯化程序其反應時間至少須達5 min以上可發揮其微混合與孔蝕加熱效益以使生質柴油轉酯化程序獲致高效能。相較於使用超音波輔助轉酯化程序反應1 min後，其KV值可自6.26 mm2/s降至5.54 mm2/s已可符合ASTM-D6751 規範之KV值 1.9-6.0 mm2/s之要求。
本研究其次以20、50及30 wt.% 比例混合之桐油、芥菜油與棕櫚油之混合油以超音波輔助轉酯化轉製生質柴油並量測成品之KV及YF，以評量生質油品轉酯化之成效。以PWUS = 270 W、TR = 25 oC、M/O = 6、MC = 1 wt.%、tUS = 5 min及tS = 10 min反應條件為對照組，探討其反應之操作參數TR、MC、tUS 及沈降時間 (settling time, tS) 對轉酯化之影響。當使用桐油為原料時，增加反應時溫度TR至60 oC時YF增加且KV下降，而增加MC至2 wt.%，YF可達最佳值98%，且KV可更進一步降低，且反應時間可低於5 min。而以混合油做為原料用油時，控制反應條件為MC = 2 wt.%、tUS = 5 min、tS = 30 min及M/O = 6時，其YF與KV於TR = 25與60 oC分別可達98.33%、4.26 mm2/s及99.68% 、4.08 mm2/s 。
因此，應用超音波輔助轉酯化製造桐油生質柴油之較適條件為TR = 60 oC、MC = 2 wt.%、M/O = 6、tUS = 5 min與tS = 30 min。然若考量節能，反應溫度可控制為25 oC，相較於TR = 60 oC，YF 略為減少約1.35％，而KV僅增加約0.18％。25 ℃轉製之混合油生質柴油之AV，IV和密度分別為0.06 mg KOH/g, 103.52 g I2/100 g 和 885 kg/m3，符合ASTM-D6751和EN14214標準。而其冷濾點-5℃，亦符合CNS15072標準之低於0 ℃需求。
本研究亦進一步比較不同預混合桐油、油菜籽油和棕櫚油濃度（CBT、CBC和CBP）之生質混合油及此三油品之原物料及分別轉酯化後之成品性質差異。藉由分析其成品之YF、AV、IV、KV、密度及CFPP以評量反應參數MC、CBT、PWUS之影響。使用桐油與棕櫚油的預混合油可大幅降低了棕櫚油的生質柴油之冷濾點，而油菜籽和棕櫚油與桐油混合所產製之生質柴油之IV和KV 較桐油生質柴油低。而MC = 2 wt.% 為最適之觸媒添加比例。控制PWUS/VL = 0.92-2.08 W/mL，CBT最佳可達60 wt.％，而CBC 僅為30 wt.％、CBC 僅10 wt.％，上述條件所生產之生質柴油其品質皆可符合標準之要求。
本研究成果獲得之資訊可提供桐油及混合油利用超音波輔助程序進行催化轉酯化轉製生質柴油之程序設計與建立相關操作參數之參考。

In this study, the effects of system parameters on the transesterification yield (YF) of biodiesel from tung (Vernicia fordii) and blended oils with CH3OH and KOH, and on key properties of biodiesel such as acid value (AV), iodine value (IV), kinematic viscosity (KV), density and cold filter plugging point (CFPP) were investigated. The background experimental conditions were as follws. The blended oil is consisted of 20, 50 and 30 wt.% of tung, canola and palm oils, respectively. The molar ratio of methanol to oil (M/O) and KOH catalyst concentration (MC) are 6:1 and 1 wt.%, respectively. Temperature (TR), ultrasonic frequency (fUS) and ultrasonic power (PWUS) were kept at 20 to 30 oC, 20 kHz and 270 W, respectively. The sample volume (VL) was 390 mL. The ultrasonic irradiation time (tUS) was set in the range of 1-30 min. The results showed that YF reaches high value of 87-91% for tung-oil biodiesel as tUS ≥ 5 min, while of about 92-94% for blended-oil biodiesel as tUS ≥ 1 min. At tUS = 10 min, the properties of biodiesel produced from tung oil are with AV of 0.11 mg KOH/g, IV of 159.36 g I2/100 g, KV of 9.17 mm2/s, density of 905 kg/m3 and CFPP of -16 oC, while those from blended oil are with AV of 0.11 mg KOH/g, IV of 120.35 g I2/100 g, KV of 5.54 mm2/s, density of 887 kg/m3 and CFPP of -5 oC. Comparing these values with the ASTM-D6751 standards with AV < 0.5 mg KOH/g, KV = 1.9-6 mm2/s and density = 860-900 kg/m3 points out that the tung oil should be blended with other oils in order to produce biodiesel satisfying the biodiesel standards. Moreover, the results indicated that a certain enough time, say 5 min, is needed to provide sufficient cavity heating and mixing via ultrasonic wave ensuring good properties of biodiesel produced. The KV of biodiesel using blended oil decreases from 6.26 mm2/s at tUS = 1 min to 5.54 mm2/s at tUS = 5 min, thus meeting the ASTM-D6751 value of 1.9-6.0 mm2/s.
Effective performances of biodiesels produced from tung oil and blended oil consisting 20, 50 and 30 wt.% of tung, canola and palm oils employing ultrasonic irradiation also were elucidated. The YF and KV, which are essential key indices to tung-oil derived biodiesel, were measured. Appropriate conditions of TR, MC, tUS, settling time (tS) and M/O were identified. The background conditions were PWUS = 270 W, TR = 25 oC, M/O = 6, MC = 1 wt.%, tUS = 5 min and tS = 10 min. The YF increases while the KV beneficially decreases with increasing TR to 60 oC. As MC increases to 2 wt.%, the YF reaches plateau value of 98% for both tung-oil derived biodiesels without and with blending with further reduction of KV. High YF is achieved at short tUS of 5 min using MC of 2 wt.%. Steady sate is approached at tS = 30 min. At MC = 2 wt.%, tUS = 5 min, tS = 30 min and M/O = 6, the YF and KV respectively are 98.33% and 4.26 mm2/s at TR = 25 oC, while are 99.68% and 4.08 mm2/s at TR = 60 oC for the blended-oil biodiesel. Thus, the suitable conditions for the effective production of tung-oil derived biodiesels applying ultrasound irradiation are at: TR = 60 oC, MC = 2 wt.%, M/O = 6, tUS = 5 min and tS = 30 min. However, for the sake of energy-saving, the transesterification condition using TR of 25 oC may be employed, causing only slight reduction of YF of about 1.35% while increase of KV of about 0.18%. The properties of AV, IV and density of the blended-oil biodiesel produced at 25 oC are 0.06 mg KOH/g, 103.52 g I2/100 g and 885 kg/m3, respectively, satisfied with the standards of ASTM-D6751 and EN 14214. The corresponding CFPP of -5 oC, which is lower than 0 oC, also meets the standard of CNS 15072.
The beneficial use of tung oil in pre-blended oil for the production of biodiesel was further studied at various blending compositions of tung, canola and palm oils (CBT, CBC and CBP). The effects of MC, CBT, PWUS and VL on the YF and the properties of AV, IV, KV, density and CFPP were investigated. The pre-blending of tung oil with palm oil greatly decreases the CFPP of palm-oil biodiesel, whereas the presence of canola and palm oils with tung oil reduces the IV and KV of tung-oil biodiesel. An MC of 2 wt.% was found to be appropriate. For PWUS/VL = 0.92-2.08 W/mL, CBT can be as high as 60 wt.% with 30 wt.% CBC and 10 wt.% CBP to produce biodiesel with high YF and satisfactory qualities of the said properties.
The information obtained in this study is useful for the proper use of tung oil in conjunction with other edible oils for the production of biodiesel with satisfactory qualities and the rational design and operation of ultrasonically catalytic transesterification process.

Abstract (Chinese version) i
Abstract iii
Table of contents vi
List of Tables ix
List of Figures xii
Nomenclature xv
Chapter 1 Introduction 1
1.1 Backgrounds 1
1.1-1 Definition of biodiesel 3
1.1-2 General scheme of biodiesel production 4
1.1-3 History of development of biodiesel 5
1.2 The Advantages and Limitations of Biodiesel Usage as Fuel 8
1.2-1 Advantages 8
1.2-2 Limitations 10
1.2-3 Availability and renewability of biodiesel 10
1.2-4 Lower emissions from biodiesel 11
1.2-5 Biodegradability of biodiesel 14
1.2-6 Thermal degradation of fatty acids during biodiesel production 15
1.3 The Current Development of Biodiesel Production in the World 17
1.3-1 Current status of biodiesel in the United State and Canada 17
1.3-2 Current status of biodiesel in Europe 25
1.3-3 Current status of biodiesel in Asia, South America, Australia, and South Africa 28
1.4 Current Technologies in Biodiesel Production 38
1.4-1 Primary raw materials used in biodiesel production 38
1.4-2 Biodiesel production using batch processing 40
1.4-3 Biodiesel production using continuous processing 43
1.5 Biodiesel Production by Applying Ultrasound 43
1.6 Objectives of This Study 44
Chapter 2 Literature Review 46
2.1 Introduction to the Sonochemistry 46
2.1-1 Acoustic cavitation in biodiesel production 46
2.1-2 Homogeneous liquid-liquid reactions 46
2.1-3 Heterogeneous solid-liquid reactions 47
2.2 Feedstock Used for Biodiesel Production 47
2.2-1 Introduction of vegetable oils and animal fats 47
2.2-2 Properties of vegetable oil 53
2.2-3 Direct use of vegetable as fuel 53
2.3 Biodiesel 56
2.3-1 The properties of biodiesel as fuel 56
2.3-2 Biodiesel from triglycerides via transesterification 61
2.3-3 Recovery of glycerine 72
2.4 Performance of Biodiesel in Diesel Engine 76
2.4-1 Alcohol-diesel emulsions 77
2.4-2 Micro-emulsions of vegetable oil 77
2.4-3 Diesel engine fumigation 77
2.4-4 Dual injection 78
2.4-5 Injector coking 78
2.4-6 Heated surfaces 78
2.4-7 Torque tests 79
2.4-8 Spark ignition 79
2.4-9 Oxidation 79
2.5 Economy of Biodiesel Production 80
Chapter 3 Materials, Experimental Methods and Procedures 86
3.1 Materials and reagents 86
3.1-1 Chemical 86
3.1-2 Oil 86
3.1-3 Equipment 86
3.2 Transesterifiacation Procedures 86
3.2-1 Effect of PWUS on YF of tung oil 87
3.2-2 Effect of tUS on YF and some properties of biodiesel produced from tung and blended oils 87
3.2-3 Effect of TR 92
3.2-4 Effect of MC on tung-oil and blended-oil biodiesels 92
3.2-5 Effect of tUS at MC of 2 92
3.2-6 Effect of tS on the yield and viscosity of biodiesel 95
3.2-7 Effect of M/O on the qualities of biodiesels 95
3.2-8 Effect of mixing condition (conventional stirring and ultrasonic irradiation) 95
3.2-9 Effect of MC on specifying tung, canola, palm and blended oils 95
3.2-10 Effect of blending composition of tung oil (CBT) 96
3.2-11 Effect of PWUS on blended-oil biodiesels 96
3.2-12 Effect of reactant loading in terms of sample volume (VL) 98
3.3 Analyses 98
3.3-1 Methyl ester 98
3.3-2 AV following EN 14104 100
3.3-3 IV following EN 14111 100
3.3-4 KV following EN ISO 3104 101
3.3-5 Density following EN ISO 3675 101
3.3-6 CFPP following EN 116 101
Chapter 4 Results and Discussion 105
4.1 Biodiesel Production from Tung Oil and Blended Oil via Ultrasonic Transesterification Process 105
4.1-1 Effect of tUS on YF of ester of biodiesel produced from tung and blended oils 105
4.1-2 Effect of tUS on properties of biodiesel produced from tung and blended oils 108
4.1-2-A The acid value 108
4.1-2-B The iodine value 110
4.1-2-C The kinematic viscosity 110
4.1-2-D The density 111
4.1-2-E Properties of biodiesels produced with longer tUS 111
4.1-2-F The cold filter plugging point 114
4.1-3 Brief conclusions of section 4.1 114
4.2 Parameter Evaluation of Biodiesel Production from Unblended and Blended Tung Oils via Ultrasound-assisted Process 115
4.2-1 Effect of reaction temperature 115
4.2-2 Effect of MC on tung-oil and blended-oil biodiesels 118
4.2-3 Effect of ultrasonic irradiation time at optimal MC of 2 118
4.2-4 Effect of settling time 125
4.2-5 Effect of molar ratio of methanol to oil 128
4.2-6 Effect of mixing condition (stirring conventional and ultrasound) 129
4.2-7 Brief conclusions of section 4.2 132
4.3 Beneficial Use of Pre-blended Tung Oil for Biodiesel Production via an Ultrasonic Process 134
4.3-1 Properties of raw oils and resulted biodiesel 134
4.3-2 Effect of MC on specifying tung, canola, palm and blended oils 134
4.3-3 Effect of blending composition of tung oil (CBT) 137
4.3-4 Effect of PWUS on blended-oil biodiesels 139
4.3-5 Effect of reactant loading in terms of sample volume (VL) 139
4.3-6 Brief conclusions of section 4.3 144
Chapter 5 Conclusions and Suggestions 148
5.1 Conclusions 148
5.1-1 Biodiesel Production from Tung Oil and Blended Oil via Ultrasonic Transesterification Process 148
5.1-2 Parameter Evaluation of Biodiesel Production from Unblended and Blended Tung Oils via Ultrasound-assisted Process 149
5.1-3 Beneficial Use of Pre-blended Tung oil for Biodiesels Production via Ultrasonic Process 149
5.2 Suggestions 150
Future Works 152
References 153
Appendicies 164
Appendix A Some Specifications of Biodiesel Standards 164
Appendix B Biodiesel Production and Purification 173
Appendix C Recovery of Crude Glycerin from Glycerol Residue 177
Appendix D Melting and Solidification Behaviors of Palm and Blended Oils 179
Publications from Present Work 186
Some Activities of Study 187
Vitae 189

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